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Facile Synthesis of Sustainable Activated Biochars with Different Pore Structures as Efficient Additive-Carbon-Free Anodes for Lithium- and Sodium-Ion Batteries

  • Glaydson Simões dos Reis*
    Glaydson Simões dos Reis
    Biomass Technology Centre, Department of Forest Biomaterials and Technology, Swedish University of Agricultural Sciences, SE-901 83Umeå, Sweden
    *Email: [email protected]
    More by Glaydson Simões dos Reis
    Orcidhttps://orcid.org/0000-0001-8727-9793
  • , 
  • Chandrasekar Mayandi Subramaniyam
    Chandrasekar Mayandi Subramaniyam
    Chemistry and Biochemistry Dpto., Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanización Montepríncipe, 28668Boadilla del Monte, Madrid, Spain
    More by Chandrasekar Mayandi Subramaniyam
  • , 
  • Angélica Duarte Cárdenas
    Angélica Duarte Cárdenas
    Chemistry and Biochemistry Dpto., Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanización Montepríncipe, 28668Boadilla del Monte, Madrid, Spain
    More by Angélica Duarte Cárdenas
  • , 
  • Sylvia H. Larsson
    Sylvia H. Larsson
    Biomass Technology Centre, Department of Forest Biomaterials and Technology, Swedish University of Agricultural Sciences, SE-901 83Umeå, Sweden
    More by Sylvia H. Larsson
    Orcidhttps://orcid.org/0000-0001-5647-3630
  • , 
  • Mikael Thyrel
    Mikael Thyrel
    Biomass Technology Centre, Department of Forest Biomaterials and Technology, Swedish University of Agricultural Sciences, SE-901 83Umeå, Sweden
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  • , 
  • Ulla Lassi
    Ulla Lassi
    Research Unit of Sustainable Chemistry, University of Oulu, P.O. Box 3000, FI-90014Oulu, Finland
    Unit of Applied Chemistry, University of Jyvaskyla, Kokkola University Consortium Chydenius, Talonpojankatu 2B, FI-67100Kokkola, Finland
    More by Ulla Lassi
  • , and 
  • Flaviano García-Alvarado
    Flaviano García-Alvarado
    Chemistry and Biochemistry Dpto., Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanización Montepríncipe, 28668Boadilla del Monte, Madrid, Spain
    More by Flaviano García-Alvarado
    Orcidhttps://orcid.org/0000-0002-5698-2598
Cite this: ACS Omega 2022, 7, 46, 42570–42581
Publication Date (Web):November 8, 2022
https://doi.org/10.1021/acsomega.2c06054

Copyright © 2022 The Authors. Published by American Chemical Society. This publication is licensed under

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Abstract

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The present work elucidates facile one-pot synthesis from biomass forestry waste (Norway spruce bark) and its chemical activation yielding high specific surface area (SBET) biochars as efficient lithium- and sodium-ion storage anodes. The chemically activated biochar using ZnCl2 (Biochar-1) produced a highly mesoporous carbon containing 96.1% mesopores in its structure as compared to only 56.1% mesoporosity from KOH-activated biochars (Biochar-2). The latter exhibited a lower degree of graphitization with disordered and defective carbon structures, while the former presented more formation of ordered graphite sheets in its structure as analyzed from Raman spectra. In addition, both biochars presented a high degree of functionalities on their surfaces but Biochar-1 presented a pyridinic-nitrogen group, which helps improve its electrochemical response. When tested electrochemically, Biochar-1 showed an excellent rate capability and the longest capacity retentions of 370 mA h g–1 at 100 mA g–1 (100 cycles), 332.4 mA h g–1 at 500 mA g–1 (1000 cycles), and 319 mA h g–1 at 1000 mA g–1 after 5000 cycles, rendering as an alternative biomass anode for lithium-ion batteries (LIBs). Moreover, as a negative electrode in sodium-ion batteries, Biochar-1 delivered discharge capacities of 147.7 mA h g–1 at 50 mA g–1 (140 cycles) and 126 mA h g–1 at 100 mA g–1 after 440 cycles.

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1. Introduction

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The sharp increase in production of renewable energy not only is due to a higher awareness of fossil fuels’ climate impact but also provides social and economic benefits. (1) However, solar and wind energy are characterized by non-continuous production. Therefore, energy storage systems with high energy and power densities are required to distribute electricity in real time according to society’s needs. Lithium-ion batteries (LIBs) are today’s dominant energy storage technology for electrifying portable electronics and helping build hybrid and plug-in electric vehicles, (2) while sodium-ion batteries (NIBs) are one of the promising and viable alternatives that could potentially replace LIBs, because of the vast abundance of sodium resources, making sodium cheaper than Li. However, due to the lower electrochemical potential (+2.71 V) and higher mass of Na, NIBs deliver a low energy density and could find application where volume does not matter like in off-grid energy storage applications. (3)
Graphite, a critical anode material for battery manufacturing, is a finite fossil resource with a large CO2 footprint and is mined and processed at high costs. (4) The graphite theoretical capacity of 372 mA h g–1 corresponds to one Li+ per six C atoms and has an acceptable cycle life but suffers low rate capability as compared to the lithium storage capability of porous hard carbons. (2,4,5) Unlike in LIBs, graphite exhibits low efficiency in NIB application because Na+ hardly forms staged graphite intercalation compounds. Therefore, it is important to study new ways of replacing graphite for more sustainable approaches and better rate capability. This has trigged research on other types of carbon-based material anodes such as hard carbons from biomass precursors that, due to their larger interlayer carbon spacing, can be extremely effective in NIB application. (3)
Extensive research is conducted to develop innovative concepts where various biomass side-streams are employed as precursors for carbon-based materials as electrodes for LIBs and NIBs. (4,5) Carbon materials, such as biochars, can be made from any kind of biomass, and they have good and adaptable structural and functional properties, which make them suitable to be used as anodes for both LIBs and NIBs. (3,6−10) In addition, nowadays, battery anodes are mainly produced from fossil carbon sources or expensive materials (such as graphene and carbon nanotubes) and using biomass residues to produce efficient anodes would be both environmentally benign and economically advantageous. (2,11) Owing to its sustainable, environmentally friendly, and cost-effective characteristics, the application of biomass opens up new possibilities for the production of green, low-cost, and high-capacity battery systems.
There are many previous studies on biochars from various resources as anodes for LIBs and NIBs. Both the biomass source and biochar production determine textural and electrochemical properties. For instance, Yu et al. (12) prepared biomass electrodes using corn straw as a precursor, producing biochars with surface areas of up to 400 m2 g–1 and pore structures that provided active sites and a cross-linked structure shortening the distance between the Li ion and the electron and, thus, improving the specific capacity of LIBs. Battery tests showed cycling stability and a notable specific discharge capacity of 577 mA h g–1 after 100 cycles at 74.4 mA g–1. Guan et al. (13) used hemp stems to make nanostructured porous biochars under different pyrolysis temperatures (300–800 °C). The produced biochars displayed surface areas of up to 590 m2 g–1 (with microporous and mesoporous structures) with abundance of active sites, which facilitated the cycling insertion and extraction of lithium ions, resulting in a reversible capacity of 495 mA h g–1 for 100 cycles. For NIBs, Zhu et al. (14) synthesized carbon anodes from corn straw biomass at different temperatures (1200, 1400, and 1600 °C) for 2 h. The most efficient biochar anode was the one carbonized at 1400 °C. It delivered interesting electrochemical metrics: a reversible capacity of 310 mA h g–1 and cyclic stability at 79% capacity retention for 700 cycles.
Based on its production conditions and chemical activation method, (15) biochar can be tailored to obtain properties that provide high-performance battery anodes. (3,7−14) For instance, in the chemical activation process, zinc chloride (ZnCl2) and potassium hydroxide (KOH) are the most commonly used activation chemical agents to yield biochars with different physicochemical properties. (8−14) Shortly, ZnCl2 and KOH each act differently during the activation process; the activation mechanism of KOH is based on solid–solid or solid–liquid reactions involving hydroxide reduction and carbon oxidation yielding CO and H2 as byproducts, while the interaction mechanism with ZnCl2 is based on catalytic dehydration with ZnCl2 acting as a skeleton during carbonization, with positive effects on the pore structure and specific surface area. Therefore, ZnCl2 produces biochars with more developed mesoporosity, while KOH often yields biochars with more micropores in its structure. (12)
It is reported that the combination of micro-mesopores with a high surface area interconnected with macropores has highly desired properties for improving the efficient mass transfer pathway for Li+/Na+ diffusion in porous carbon anodes. (16,17) Furthermore, a high surface area with high mesoporosity is beneficial (1) for facilitating fast ion (Li+/Na+) diffusion through the anode to access more surface-active sites for Li+ or Na+ adsorption, which maximize both the effective intercalation area and capacitive contribution; (2) for playing a crucial role in sustaining a significant capacity even at high rates; and (3) for mitigating the volume change during cycling. Thus, basic research is required to obtain carbon materials with optimized specific surface area (SSA), porosity, and pore size distribution that are adapted to the size of electrolyte-solvated ions to therefore provide high conductivity, electrochemical response, and good physicochemical stability. (10,11)
The main goal of this work is to perform one-pot synthesis of biochars from Norway spruce bark and investigate their electrochemical properties as an alternative carbon electrode for LIBs and NIBs. The biochars were prepared using two different chemical activation, namely, using KOH and ZnCl2. The influence of chemical activation on the structural and chemical properties of the biochar materials and the role of the surface area and pore structure on mass diffusion and that of actives sites on capacitive processes in the biochars were unveiled by determining the respective contribution of the two storage mechanisms along with the diffusion coefficient for the lithium case. Thus, the chemically activated biochars exhibited enhanced lithium storage, retaining a specific capacity of 319 mA h g–1 at 1000 mA g–1 after 5000 cycles and a high reversible sodium storage capacity of 126 mA h g–1 at 100 mA g–1 for 440 cycles with 99% retention. Thus, it can be considered an above-par biomass anode material for LIB and NIB applications.

2. Materials and Methods

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2.1. Chemicals and Reagents

The Norway spruce bark was used as the carbon precursor, and it was provided by the Holmen paper and pulp industry, Sweden. The chemical agents zinc chloride (ZnCl2), potassium hydroxide (KOH), and hydrochloric acid (HCl) were purchased from Sigma-Aldrich.

2.2. Biochar Synthesis

First, the spruce bark was dried and ball milled to an average particle size of ∼500 μm using a Fritsch Pulverisette 14 ball mill. The biochars were prepared as described elsewhere: (18,19) first, 40 g of bark was mixed with activation chemicals (KOH or ZnCl2) at a ratio of 1:1 (by weight) and dispersed in 30 mL of distilled water to get a homogeneous paste. The mixtures were left for 2 h at ambient temperature and then subjected to overnight oven drying at 105 °C. The dried samples were pyrolyzed at 800 °C for 2 h at a ramp of 10 °C per min under nitrogen gas flow. After being cooled to room temperature, the samples were milled and washed with 6.0 M HCl and 1.0 M HCl for ZnCl2 and KOH biochars, respectively, and washed several times with distilled water until the pH value of the filtrate reached a neutral value. The ZnCl2-activated biochar was labeled “Biochar-1” and the KOH-activated one “Biochar-2”.

2.3. Biochar Material Characterization

The SSA (SBET) and porosity data of the biochars were evaluated via nitrogen adsorption–desorption isotherms by using a Tristar 3000 apparatus (Micrometrics Instrument Corp.). The biochars were subjected to degasification at 180 °C for 3 h, and the SBET and pore size distribution were obtained using the Brunauer–Emmett–Teller (BET) method. Mesopore surface areas were calculated using the Barrett–Joyner–Halenda (BJH) method from desorption curves, while the micropore area values were calculated using the t-plot method. The morphology of the biochars was determined using field emission scanning electron microscopy (FESEM; microscope model: Zeiss Gemini). To further investigate their structure, transmission electron microscopy (TEM) images were taken using a Talos L120C microscope (FEI, Eindhoven, the Netherlands) at acceleration voltages of 20–200 kV. TEM grids were covered with 5 mL of the diluted powder samples in deionized water. Raman spectra were collected using a Bruker Bravo spectrometer (Bruker, Ettlingen, Germany) connected to a docking measuring station. Shortly, 0.5 g of each biochar powder was placed in 2.5 mL glass vials and scanned in the 300–3200 cm–1 spectral range at a 4 cm–1 resolution for 256 scans. Min–max normalization over the 1000–2000 cm–1 region and smoothing (nine points) were done using the built-in functions of the OPUS software (version 7, Bruker Optik GmbH, Ettlingen, Germany). No baseline correction was needed. X-ray photoelectron spectroscopy (XPS) spectra of the biochars were collected using a Kratos Axis Ultra DLD electron spectrometer equipped with a monochromated Al Kα source operated at 150 W. An analyzer of 160 eV for acquiring survey spectra and another at 20 eV for individual photoelectron lines were used. The samples were gently hand-pressed using a clean Ni spatula into a powder sample holder. Due to the electrically conductive behavior of the carbonaceous material, no charge neutralization system was used. The binding energy (BE) scale was calibrated following the ASTM E 2108 and ISO 15472 standards. Processing of the spectra was accomplished with the Kratos software. A high-resolution X-ray diffractometer (model: Bruker D8) with copper Kα radiation (λ = 1.5418 Å) was employed for phase determination of biochars.

2.4. Electrochemical Measurements

The electrochemical performance of biochars were investigated using CR 2032 lithium coin cells in a half-cell configuration. An electrode slurry containing a 9:1 weight ratio of active materials to a poly(vinylidene fluoride) (PVDF) binder was well blended in N-methyl-2-pyrrolidone (NMP) solvent. The slurry was tape cast over carbon-coated copper foil using a doctor blade and then vacuum dried at 120 °C overnight. The electrodes were cut into circular discs of 12 mm diameter each and weighing about 0.8–1 mg cm–2. The half-cell-configured coin cells were assembled in an argon-filled glovebox maintained at 0.1 ppm H2O and 0.1 ppm O2. The coin cells were fabricated using biochars as the working electrodes and lithium/sodium foil as counter/reference electrodes separated by a Whatman glass microfiber separator impregnated in a few drops of 1 M lithium hexafluorophosphate in 1:1 (v/v) ethylene carbonate (EC):diethyl carbonate (DEC) for LIBs and a sodium electrolyte consisting of 1 M NaTFSI in 1:1 (v/v) EC:DEC. All cells were tested under a constant galvanostatic current density (in mA g–1) between 0.002 and 3 V for LIBs and 0.002 and 2 V for NIBs (unless mentioned) with an Arbin multichannel battery tester (Texas Instruments Inc., United States) and a Neware multichannel battery tester (China). Cyclic voltammograms (CVs) were obtained at 0.1 mV s–1, while electrochemical impedance spectra (EIS) were obtained at frequencies between 0.1 MHz and 10 mHz at a 5 mV amplitude using BioLogic VMP3 instrument (France).

3. Results and Discussion

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3.1. Physicochemical Characterization of the Biochars

The SSA (SBET) and pore structures of carbon materials are crucial properties for enhancing ion diffusivity by providing short distances, thereby improving their electrochemical rate performances. (6,7,17)Figure 1,ba shows the nitrogen adsorption–desorption at 77 K, which was used to determine the porosity features of the biochars. The N2 isotherms show that the two chemical activators’ effects on the biochars’ structural features differ, but both contain micro- and mesopores. Biochar-1 has a straight line from the initial partial pressure up to 0.4, while the isotherm of Biochar-2 displays more N2 adsorption at low partial pressure, which can be ascribed to the filling of micropores, suggesting the existence of more micropores. This observation is in accordance with the fact that no hysteresis exists in Biochar-2 unlike in Biochar-1, where a hysteresis exists between 0.4 and 0.6 relative pressures. This suggests that Biochar-1 prepared by chemical activation with ZnCl2 possesses mesopores in its structure, which is in accordance with the literature. (7,20,21)

Figure 1

Figure 1. Physiochemical properties of chemically activated Biochar-1 and Biochar-2: (a,b) nitrogen adsorption–desorption isotherms; (c,d) morphological analysis using FESEM depicting the porous structures of the biochars (at 10,000× magnification); (e,f) Raman spectra showing the structural defects and degree of graphitization in the biochars.

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The pore size distributions derived from the BJH plots of both biochar samples are displayed in Figure 1. Chemical activation seems to affect the pore structure of the biochar samples. Biochar-1 exhibits a much higher distribution of mesopores sized between 2.36 and 4.1 nm, while the higher peak in Biochar-2 is related to micropores (at 1.7 nm) and also exhibits the presence of mesopores. According to the pore distribution curves, both samples exhibit the presence of micropores and mesopores, which is in accordance with the data presented in Table 1. The difference in the pore size distribution of biochar samples can affect the ion-storing process since bigger pores can facilitate the diffusion pathways while the high presence of mesopores, instead micropores, guarantee the accessibility of the ions to the internal pore structure of the biochar, which can boost the efficiency of the materials as anode for battery application.
Table 1. Textural Properties of the Biochars
parameters (units)Biochar-1Biochar-2
SSA (m2 g–1)12941881
mesopore surface area (m2 g–1)12441055
mesopore surface area (%)96.156.1
micropore area (m2 g–1)49825
micropore area (%)3.943.9
total pore volume (cm3 g–1)0.831.06
average pore size (nm)2.652.20
yield (%)38.512.3
From the N2 isotherm adsorption/desorption curves, we could ascertain that both biochars contain micro and mesoporosity and that the activation process caused important differences in its pore structures. The numerical values for textural properties are shown in Table 1. Biochar-2 had a higher SBET value (1881 m2 g–1) than Biochar-1 (1294 m2 g–1). The mesopore surface area of Biochar-1 was 1224 m2 g–1, compared to 1055 m2 g–1 for Biochar-2. Also, in percentage, the mesopore contribution was higher for Biochar-1 (96.1%) than for Biochar-2 (56.1%). The corresponding values for the micropore surface area were as follows: Biochar-1, 49 m2 g–1 (3.9%), and Biochar-2, 825 m2 g–1 (43.9%). It was previously reported that mesopores benefit the electrochemical performance by enhancing Li+ or Na+ intercalation. (16) The large surface area and the high percentage of mesopores in Biochar-1 can effectively help the percolation of electrolyte ions into small-sized pores. That type of pore size distribution has been reported to provide a high charge storage capability even at a high current density. (17,22)
The above observations are well-supported by the morphological analysis of biochars using FESEM as shown in Figure 1c,d. The images highlight important differences related to the use of different chemical activation agents (ZnCl2 and KOH); for instance, in Figure 1d, Biochar-2 shows a more broken and irregular structure full of roughness with small holes. On the other hand, Biochar-1 (Figure 1c) shows what seems to be a much denser structure, with more elongated cavities and bigger holes of different sizes and shapes. SEM analysis also indicates that the activation method induced changes on the surface characteristics of the biochars. In addition, the images show a large quantity of macropores and ultra-macropores (especially in Biochar-1). Macropores are important because they serve as vectors for electrolyte passage until smaller pores are attained (in the interior of the biochars), which can facilitate permeation of the electrolyte along with the porous structure for the following step of charge accumulation into the cavities.
Further details of the biochars are explored through TEM images (see Figure S2). (23−25)Figure S2a (Biochar-1) shows a highly amorphous and homogeneous carbon structure. (24,25)Figure S2b (Biochar-2) shows a very heterogeneous structure. Tube-like structures can be observed in Biochar-2 (see the rectangles inside the figure) that could be attributed to excessive intercalation of mobile metallic K at high temperatures resulting in bending of the carbon sheets. (11) It also comprises some amorphous parts (see the circle inside the figure) and a certain extent of agglomeration with irregular shapes (indicated by the arrows) that can be also a reflex of the impurities observed in the X-ray diffraction (XRD) pattern (Figure S3).
The yield of the biochars is tabulated in Table 1. The yields of Biochar-1 and Biochar-2 were 38.5% and 12.3%, respectively. This result suggests that a much more violent reaction between the biomass precursor and KOH took place during the pyrolysis process. This reaction takes place via C–O–C and C–C bond breakage and maximizes the material’s volatilization, leading to a low carbon yield. (26,27) On the other hand, ZnCl2 activation results in degradation of the cellulosic material that, combined with the dehydration during carbonization, leads to charring and aromatization of the carbon matrix, which inhibits the formation of tar and reduces mass loss, providing higher yields than when using other chemical reagents. (18,27)
Raman analysis was performed to analyze the order/disorder and degrees of graphitization in the biochars.7,29–31Figure 1e,f shows that both samples exhibit a disorder-induced D band (around 1340 cm–1) and in-plane vibrational G band (around 1585 cm–1), corresponding to the disordered and imperfect structures of carbon materials and the vibrations of carbon atoms with an sp2 electronic configuration in graphite structures. Comparing the spectra of the two samples, Biochar-1 has a bigger G peak than Biochar-2, which has a bigger D peak. These results suggest that Biochar-1 has a more ordered and higher graphitic structure, while Biochar-2 has more defects. The ID/IG ratio of Biochar-1 goes below 1 (0.98), indicating the formation of sufficiently ordered graphite sheets, while Biochar-2 has an ID/IG ratio of 2.0. It is well known that graphite has a high conductivity degree and behaves as an efficient material when used as an anode for battery application. A low ID/IG value suggests that the material has more perfect and orderly graphite structures with a high graphitization degree; a high ID/IG indicates that the material has more defects in its structure. (7,31,32)
The differences in the graphitization degrees could be related to the different activation methods. It is well-known that KOH activation enhances the expansion of carbon lattices, resulting in the increase of defects, which is reflected in the abundant pores on the carbon. (33) This is in accordance with our textural properties highlighted in Table 1. Also, ZnCl2 showed a less defective structure with a more cohesive morphology/structure (as observed in SEM images). The abundance in defects can result in a less graphitic structure. In addition, Song et al. (34) reported that activation with KOH generated biochars with less graphitized structures due to the high oxygen content. This statement is consistent with our results that displayed Biochar-2 (KOH) with a much higher oxygen content compared to Biochar-1.
XPS analysis was carried out to evaluate the effect of the chemical activation methods (KOH and ZnCl2) on the biochars’ surface element composition, chemical state, and functional groups. Figure 2 shows the XPS spectra for the carbon, oxygen, and nitrogen elements of Biochar-1 (Figure 2a) and Biochar-2 (Figure 2b). The carbon spectra (C 1s) were deconvoluted into four peaks centered at 284.1–284.4 eV, which are related to C–C and C═C bonds; at 285.4–285.5 eV, which is attributed to C–N; at 286.3 and 286.5 eV (C–O–C); and at 287.2 and 287.5 eV, which are related to C═O. (7,28,29) For the oxygen spectra (O 1s), some differences are observed in relation to the chemical activation process. The O 1s spectra of Biochar-1 were deconvoluted into four oxygen chemical states with binding energies at around 531.4, 532.8, 535.3, and 537.2 eV, while those of Biochar-2 were deconvoluted into three peaks, 530.8, 532.5, and 535.6 eV. (7,28,29) The peaks at 531.2 and 530.8 eV are attributed to oxygen double-bonded with carbon in carbonyl and quinone-like structures; those at 532.5 and 532.8 eV are related to oxygen singly bonded to carbon in aromatic rings, phenols, and ethers, and those at 535.1 and 535.6 eV are related to hydroxyl groups. A different peak at 537.2 eV is found only in Biochar-1, which is related to the adsorbed H2O–OH sub-monolayer in which −OH and H2O are hydrogen-bonded to each other. Nitrogen spectra (N 1s) are also shown in Figure 2. A solo peak is observed in Biochar-2, which is related to pyrrolic nitrogen, (7,28,30) while for Biochar-1, two peaks are exhibited, one at 397.8 eV, which is related to pyridinic species, and one at 400.3 eV (pyrrolic nitrogen). (29,31) The presence of pyridinic species in Biochar-1 can give it better electrochemical performances. N species act as the electron donor, which facilitates and improves the charge transfer. (30) In addition, Hou et al. (30) reported that pyridinic-N boosts the electrochemical performances of electrodes, which can be considered an important advantage for Biochar-1.

Figure 2

Figure 2. Carbon (C 1s), oxygen (O 1s), and nitrogen (N 1s) XPS spectra of (a) Biochar-1 and (b) Biochar-2.

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The presence of pyridinic-N could be related to the aromatization process of the biochars, which is maximized under ZnCl2 activation and not under KOH activation. (35) ZnCl2 is an efficient dehydrating agent, and the dehydration process could result in the enhancement of the charring process and aromatization of the carbon skeleton. (36) Peiris et al. (35) prepared biochars from tea wastes and reported that the presence of aromatic rings derived from the nitration reaction allowed the fixation of nitrogen species in the biochars during thermochemical reactions. Moreover, its distinctive oxygen functionality and low aromatization degree (36,37) could explain the fact why Biochar-1 (ZnCl2) exhibits a pyridinic-N specie on its surface that promotes electronic conductivity.
Table 2 presents the main compositions of the two biochars based on XPS and EDS elemental analyses.
Table 2. XPS Elemental Composition (at. %) and Elemental Analysis (%) of the Biochars
 XPS (at. %)elemental analysis (%)
sample IDC 1sO 1sN 1sC/OCNHOash
Biochar-194.74.90.719.394.50.51.02.81.2
Biochar-289.78.40.810.784.90.71.18.64.7
Biochar-1 presents higher carbon and lower oxygen contents compared to Biochar-2. The higher presence of oxygen can be related to the presence of large amounts of functionalities on the biochar surface. For instance, C/O ratios are presented, which indicates the formation and presence of hydroxyl groups on the biochars’ surfaces. (38) The Biochar-2 sample had a lower C/O value (10.7) compared to Biochar-1 (19.3); this suggests that Biochar-2 is richer in oxygen functionalities compared to Biochar-1. During KOH activation, reactions between KOH, O-containing species in the biomass, and carbon fragments can form an abundance of vacancies in the biochar. (38) The OH– from KOH rapidly enters these vacancies, forming a large amount of new O-containing groups (i.e., C–O, −OH, C–O, O–C–O, and −COOH groups), which in turn increases the amount of oxygen in Biochar-2. (38)
Biochar-1 presented lower ash contents compared to Biochar-2. Biochar-2 has more than three times ash content compared to Biochar-1. The ash contents are mostly related to calcite and quartz (electronic inert components). (39−41) It is well known that high carbon and low ash contents positively affect the specific capacity of the electrode material. On the other hand, a high amount of ash can contribute to low Coulombic efficiency and cyclability of the electrode, especially if the ashes are electronically inert.
One possible reason why Biochar-2 has a higher ash content than Biochar-1 could be related to the leaching-out process. (8,19) It is well known that the inorganic compounds formed during pyrolysis are leaching out during the washing procedure with HCl solution. The washing step was performed with HCl solutions at concentrations of 6.0 and 1.0 M for Biochar-1 and Biochar-2, respectively. It could be possible that 1.0 M HCl was not efficient enough to remove all inorganic and crystalline phases in the biochar while 6.0 M is strong enough to remove all inorganics. (8,18,19,21)
The above analysis is verified by XRD of biochars as shown in Figure S3. The biochar activated with ZnCl2 (Biochar-1) presents an amorphous structure with broad and weak signals of a typical highly disordered carbon structure, which is expected for porous carbon, while the KOH activation (Biochar-2) presented some distinct peaks pertaining to a crystalline impurity coexisting with the carbon amorphous phase. The presence of amorphous material is recommended for carbon electrodes due to its network pores and vacancies. (28) The XRD pattern of Biochar-2 displays peaks that are related to a high concentration of calcite (42) and some quartz while in Biochar-1 none of these peaks is observed. Once both biochars were prepared with the same precursor and pyrolysis conditions, a possible aspect that can contribute for higher crystallites in Biochar-2 could be related to the leaching-out process as earlier discussed in XPS discussion.

3.2. Electrochemical Characterization

3.2.1. Biochar/Li+ Half-Cells

The effects of chemical treatment on the electrochemical performance of additive-carbon-free biochars were studied in a CR 2032 type coin cell in a half-cell configuration against Li metal cycled between 0.002 and 3 V. Figure 3a shows various charge–discharge plots of Biochar-1. In the first discharge cycle, the long sloping plateau below 1 V corresponds to the sum of different processes: the intercalation of Li ions into graphitic carbon, adsorption of lithium in the mesoporous carbon structures, chemical interactions of functional groups on the biochars’ surface, and formation of a solid–electrolyte interface (SEI) layer delivering the first discharge capacity of 1402.4 mA h g–1. Upon charging, a capacity of 461.2 mA h g–1 was delivered inasmuch as the two latter processes are not reversible. In the subsequent cycles, Biochar-1 delivered a reversible capacity pertaining to a Coulombic efficiency of 89.7% for the next four cycles and then improved to 99.1% for long cycles. Figure 3b shows the capacity retention capability of the active materials at different current densities to meet the demand of electric vehicles. The specific capacity of Biochar-1 decreased from 441 mA h g–1 at 50 mA g–1 to 220.2 mA h g–1 at 2000 mA g–1 and reverted to 387 mA h g–1 at 100 mA g–1 even after 100 cycles, which exhibits its excellent capacity reversibility at various current densities. In the long run, the biochars were cycled at 100 mA g–1 for 100 cycles followed by an increased rate of 500 mA g–1 for the next 1000 cycles and, finally, at 1000 mA g–1 for 5000 cycles (Figure 4c). Biochar-1 delivered an excellent reversible capacity of 320 mA h g–1 at 1000 mA g–1 at 99.6% Coulombic efficiency even after 5000 cycles while KOH-activated Biochar-2 could manage to deliver only 172.2 mA h g–1. The enhanced long cycle stability and the excellent capacity retention at a high rate of Biochar-1 could be attributed to the high conductivity due to the pyridinic-N group and the high percentage of mesopores in its carbon structures, which helps ease the transport of ions.

Figure 3

Figure 3. (a) Charge–discharge of Biochar-1 at various cycles, (b) rate test, and (c) long cycle stability of biochars at various current densities.

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Figure 4

Figure 4. (a) Electrochemical impedance spectroscopy (EIS) of fresh cells (inset: equivalent electrical circuit); (b) cyclic voltammetry (CV) of biochars; (c) CV at different scan rates of Biochar-1; (d) CV with mapping of the diffusion-controlled mechanism and capacitive effect; (e) contribution of Faradic and capacitive effect in Biochar-1 as a function of scan rates; (f) slope b as a function of each potential during the charge–discharge process. From the plot, we can conclude that as the slope b value is greater than 0.5, the electrochemical kinetics of biochar is limited by the non-diffusive surface capacitive mechanism.

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These characteristic features are determined by the Nyquist plot of the EIS of fresh cells (at OCV) as shown in Figure 4a. Both biochars exhibited a complete semi-circle and an incomplete depressed semi-circle followed by an inclined line pertaining to the Warburg semi-infinite diffusion characteristic pattern at high-, intermediate-, and low-frequency regions. This is represented in terms of an equivalent circuit (Figure 4a, inset) consisting of the solution resistance (Rs) and the electrical double-layer capacitance (Cdl) in parallel to the resistance to charge transfer (Rct) followed by a constant-phase element (Q1) and the resistance associated with the metal-ion diffusion (Wd). (43) The measured solution resistance (Rs) for Biochar-1 is 4.6 Ω, while it is four-fold higher for Biochar-2. Considering the total resistance of the cells, the Rs values are insignificant and are expected to have little influence on the cell polarization difference. However, the different values of Rs can be explained as being due to the different textural properties of the biochars. At high frequencies, the intercept corresponds to the combined effects of the internal Ohmic resistances of the electrolyte and cell components such as current collectors and metallic electrical contacts. (44) As ascertained from the cycling performance, Biochar-1 exhibited the lowest Rct value of 57.2 Ω as compared to 97.3 Ω by Biochar-2. However, the total resistance after 5000 cycles is increased, possibly due to the contribution of the SEI resistance (Figure S4). (45) The lithium diffusion coefficient (DLi+ in cm2 s–1) could be determined from the Warburg component of EIS at a low frequency using Fick’s law of diffusion as stated below:
DLi+=0.5(VmFSσ)2(dEdx)2
where Vm is the molar volume of carbon (cm3 mol–1), F is the Faraday constant (C mol–1), S is the electrode surface area (cm2), (dE/dx) is the first derivative of the discharge cycle, and σ is the Warburg coefficient (Ω s–1/2), calculated from the slope of the linear fitting Z′ vs ω–0.5 (Figure S5). The calculated diffusion coefficient of Biochar-2 at the end of the first discharge cycle is 3.1 × 10–17 cm2 s–1, which is 1.5 times lower than the Biochar-1 value of 4.6 × 10–17 cm2 s–1. This may be due to the high percentage of mesoporous structures in the carbon layers, which helps ease mass transfer and hence is reflected in their excellent electrochemical performance at different current densities.
Figure 4b depicts the CV curves for five cycles at a 0.1 mV s–1 scan rate. Both samples display a typical CV curve of amorphous carbon. In the first discharge cycle, the sloping curve between 1.0 and 0.45 V pertains to the irreversible formation of an SEI layer and a reduction peak (0.45–0.16 V) corresponds to intercalation of Li ions into the carbon layers to form a reversible LixC6 (xLi+ + 6C + xe– ↔ LixC6) phase or surface storage in their mesoporous structures. The corresponding oxidation peak at 0.2–0.5 is observed upon reversing the polarity corresponding to the Li+ deintercalation process and releasing the storage electrons to the external circuit. The SEI layer is composed of decomposed electrolyte products that traps Li+ and is the reason behind the huge drop in the capacity from 1402.4 to 461.2 mA h g–1 resulting in the low first cycle Coulombic efficiency. For the subsequent cycles, the CV curves almost overlap with each other, which suggests that the intercalation and de-intercalation and surface storage of Li ions exhibited good reversibility and excellent electrochemical stability.
An elaborate kinetic investigation was carried out to elucidate possible modes of charge storage in Biochar-1. For this purpose, a half-cell was subjected to CV measurements between 0.01 and 3 V for three cycles at each scan rate starting from high (1.0 mV s–1) to low rates (0.01 mV s–1) (Figure 4c and Figure S6). The CV curve shows similar peak positions as discussed above with broadened and compressed peaks at high and low scan rates, respectively. The total area under the CV curve corresponds to the total stored charge/capacitance, which is the sum of Faradic diffusion-controlled and non-diffusive capacitive contribution mechanisms. The latter is predominant in high surface area carbonaceous materials due to charge storage by interaction with functional groups at the surface level. These contributions could be determined from CV plots at various scan rates using a power law, i = avb, where i is the measured current (mA); v is the scan rate (mV s–1); and a and b are the variable parameters, where b is determined from the slope of the plot of log i vs log v wherein, if b = 0.5 and b = 1, then the kinetics of the electrochemical reaction is limited by diffusion-controlled intercalation and non-diffusive capacitive mechanisms, respectively, with either ions electrochemically adsorbed or just adsorbed ions at the surface. (46,47) Therefore, the measured current at each potential is the sum of these two contributions represented as I = a1v + a2v0.5, where a1v is the current from the capacitive effect and a2v0.5 is the current from the diffusion-controlled effect. The constants a1 and a2 could be determined from the slope and intercept of I/v0.5 vs v0.5 plots. Figure 4d represents the contributions of capacitive (red-shaded region) and Li+ diffusive intercalation mechanisms. The latter redox reactions are due to diffusion-controlled electrochemical kinetics and therefore take place near the redox peak positions of CV while the remaining areas are the non-diffusion capacitive effect due to surface charge storage and double-layer effects. At high scan rates, the major contribution is due to the non-diffusion capacitive effect but transcends to diffusion-limited electrochemical kinetics at low scan rates (Figure 4e). For instance, from 0.075 to 0.01 mV s–1 scan rates, the charge storage component from Li+ diffusion kinetics increased from 48 to 68% (Figure 4e), but still, the major charge storage contribution is from capacitive effects. This observation is in accordance with slope b as shown in Figure 4f. This is mainly due to the requirement of more time for Li+ diffusion as the majority interacts with surface functional groups contributing to the surface-limited rate-controlling mechanism in Biochar-1.
The electrochemical performances of our Biochar-1 LIB anodes are above par compared with many reported ones in the literature. (10,47−54) We emphasize that our facile chemically activated biochar outclassed in terms of high surface area (1294 and 1881 m2 g–1), delivering a high initial discharge of 1402.4 mA h g–1, rate capability, and long cycle stability/retention of 5000 cycles even at a high current density of 1000 mA g–1, as a yardstick against other state-of-the-art electrode biomass LIB anodes. A more detailed comparison is tabulated in the Supporting Information (Table S1).

3.2.2. Biochar/Na Half-Cells

As stated earlier, the electrochemical potential of sodium (+2.71 V) is lower than that of lithium (+3.04 V) and owing to its higher atomic mass, it is anticipated that the energy density of an NIB tends to be lower than that of an LIB for the same materials of interest. However, our biochar possesses a high percentage of mesoporosity with interconnected channels for fast electron and ion transport, which could help alleviate the volume changes due to intercalation/de-intercalation of bigger Na ions and, therefore, an above-par excellent reversible cyclability is expected when this biochar is used as a sodium storing anode. In the CV plot for the first cycle, two reduction peaks at 0.53 and 0.98 V were observed. These peaks can be attributed to the decomposition of the electrolyte and formation of an irreversible SEI layer. (48) However, these peaks disappeared in the subsequent cycles (Figure 5a), indicating that the SEI was mainly formed in the first charge/discharge. (49,50) The CV curves from the second to the fifth cycle almost overlapped, which indicates a good reversibility for the charge storage mechanisms. The cycles overlapping after the first cycle may suggest electrolyte exposure to more active sites during sodiation/desodiation, for instance, the opening of the pores because of the material’s highly porous surface. (50) The absence of voltage peaks in the CV profiles indicates more surface-controlled reactions during the sodiation/desodiation process. (55)

Figure 5

Figure 5. (a) Cyclic voltammetry (CV) of Biochar-1, (b) rate tests at different current densities, (c) long cycle stability of biochars at various current densities, and (d) Nyquist electrochemical impedance spectroscopy (EIS) plot of fresh cells and cells after cycling (inset: enlarged at high frequencies).

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The dynamic electrochemical characteristics of Biochar-1 were evaluated by measuring the rate performance at current densities from 25 to 1000 mA g–1 (see Figure 5b). Biochar-1 exhibited reversible capacities of 231, 197, 167, 136, 105, and 47 mA h g–1 at current rates of 25, 50, 100, 200, 500, and 1000 mA g–1 and delivers a reversible capacity upon lowering of the current density to 50 mA g−1 at the end of the 45th cycle, demonstrating an excellent rate capability performance under different current densities. To further evaluate the cycling stability of Biochar-1 as a sodium anode, current densities of 25, 50, and 100 mA g–1 were applied to evaluate longer cycle stabilities. As can be seen in Figure 5c, the Biochar-1 anode delivered a first discharge capacity of 566.2 at 50 mA g–1 and 147.7 mA h g–1 after 140 cycles and a high reversible capacity of 126 mA h g–1 at 100 mA g–1 for 440 cycles, retaining the capacity at 99%, exhibiting excellent cycle stability. This could be attributed to the low Rct of 94.42 Ω (from the EIS Nyquist plot, Figure 5d) maintained and the high percentage of mesoporosity that helps fast ion transport and buffer volume change during the Na+-intercalation and de-intercalation process. Compared with previous reports (Table S2), Biochar-1 exhibited superior Na+ storage performance, a higher reversible specific capacity, and better capacity retention than reported values; however, for long-term cyclability, it needs further studies. Moreover, the Biochar-1 anode showing a high Coulombic efficiency of ∼99% after 440 cycles indicates highly reversible and stable electrochemical charge storage mechanisms in our biochar anode. Although there is mainly capacity as deduced from the I–V profile (Figure 5a), a mass diffusion-controlled mechanism seems to be also present as deduced from the spike developed at a low frequency in the EIS experiment (Figure 5d).

4. Conclusions

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In summary, we successfully synthesized chemically activated nanoporous biochar using low-cost and sustainable Norway spruce bark as a precursor to fabricate carbon electrodes with superior Li+ and Na+ storage capability. The ZnCl2-activated Biochar-1 possesses excellent physicochemical properties such as a high percentage of mesopores with ordered structures as compared to the disordered KOH-activated Biochar-2 sample. Biochar-1 exhibited a superior electrochemical performance of 319 mA h g–1 at 1000 mA g–1 for 5000 cycles with 99.1% Coulombic efficiency when tested in lithium half-cells. A postmortem of the electrode’s morphology after 5000 cycles shows that there is no appreciable change in the morphology of the active materials as compared to that of the fresh electrode (Figure S7a,b). Biochar-1 delivered a reversible capacity of 126 mA h g–1 at 100 mA g–1 for 440 cycles, keeping the capacity at 99% in sodium half-cells.
Due to its facile, cheap, and environmentally benign nature, the single-step biochar preparation could be extended to large-scale production of efficient biochar electrodes with improved electrochemical properties for future advanced battery applications. However, the use of biomass-based carbon materials in full cells (Figure S7c,d) remains challenging due to the large irreversible first cycle loss associated with the formation of a thick SEI layer, which is an intrinsic property of high surface area carbonaceous materials.

Supporting Information

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The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acsomega.2c06054.

  • Figure S1, pore size distributions of Biochar-1 and Biochar-2. Figure S2, TEM images of Biochar-1 (a) and Biochar-2 (b). Figure S3, XRD patterns of Biochar-1 and Biochar-2. Figure S4, impedance spectra of a Biochar-1//Li cell after 5000 cycles (inset: simulated equivalent electrical circuit). Figure S5, determination of the Warburg constant from the slopes of the plots of Z′ vs ω–1/2 of (a) Biochar-1 and (b) Biochar-2. Figure S6, CV with mapping of lithium diffusion-controlled mechanism and capacitive effect in Biochar-1 at various scan rates. Table S1, comparative electrochemical performances of Biochar-1 and biomass carbonaceous materials as LIB anodes. Table S2, comparative electrochemical performances of Biochar-1 and biomass carbonaceous materials as NIB anodes. Figure S7, morphology of the Biochar-1 electrode at 3000× magnification: (a) fresh electrode and (b) after 5000 cycles. The fresh electrode composition consisted of Biochar-1 and a PVDF binder at a 9:1 weight ratio. Electrochemical performance of full cell using Biochar-1 as the anode and LiFePO4 as the cathode; (c) charge–discharge plot and (d) long cycling stability at various current densities (PDF)

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Author Information

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  • Corresponding Author
  • Authors
    • Chandrasekar Mayandi Subramaniyam - Chemistry and Biochemistry Dpto., Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanización Montepríncipe, 28668Boadilla del Monte, Madrid, Spain
    • Angélica Duarte Cárdenas - Chemistry and Biochemistry Dpto., Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanización Montepríncipe, 28668Boadilla del Monte, Madrid, Spain
    • Sylvia H. Larsson - Biomass Technology Centre, Department of Forest Biomaterials and Technology, Swedish University of Agricultural Sciences, SE-901 83Umeå, Sweden;  Orcidhttps://orcid.org/0000-0001-5647-3630
    • Mikael Thyrel - Biomass Technology Centre, Department of Forest Biomaterials and Technology, Swedish University of Agricultural Sciences, SE-901 83Umeå, Sweden
    • Ulla Lassi - Research Unit of Sustainable Chemistry, University of Oulu, P.O. Box 3000, FI-90014Oulu, Finland;  Unit of Applied Chemistry, University of Jyvaskyla, Kokkola University Consortium Chydenius, Talonpojankatu 2B, FI-67100Kokkola, Finland
    • Flaviano García-Alvarado - Chemistry and Biochemistry Dpto., Facultad de Farmacia, Universidad San Pablo-CEU, CEU Universities, Urbanización Montepríncipe, 28668Boadilla del Monte, Madrid, Spain;  Orcidhttps://orcid.org/0000-0002-5698-2598
  • Author Contributions

    G.S.d.R. and C.M.S. contributed equally to this work.

  • Notes
    The authors declare no competing financial interest.

Acknowledgments

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This research was funded by Bio4Energy, a Strategic Research Environment appointed by the Swedish government, and the Swedish University of Agricultural Sciences. The Raman measurement was performed at the Vibrational Spectroscopy Core Facility (ViSp), Chemical Biological Centre (KBC), Umeå University. The Umeå Core Facility for Electron Microscopy (UCEM-NMI node) at the Chemical Biological Centre (KBC), Umeå University, is gratefully acknowledged. Electrochemical characterization at Universidad San Pablo CEU was carried out with the financial support of MCIN/AEI/10.13039/501100011033 (Project PID2019-106662RB-C41).

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    Hernández-Rentero, C.; Marangon, V.; Olivares-Marín, M.; Gómez-Serrano, V.; Caballero, Á.; Morales, J.; Hassoun, J. Alternative lithium-ion battery using biomass-derived carbons as environmentally sustainable anode. J. Colloid Interface Sci. 2020, 573, 396– 408,  DOI: 10.1016/j.jcis.2020.03.092
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    10
    Alternative lithium-ion battery using biomass-derived carbons as environmentally sustainable anode
    Hernandez-Rentero, Celia; Marangon, Vittorio; Olivares-Marin, Mara; Gomez-Serrano, Vicente; Caballero, Alvaro; Morales, Julian; Hassoun, Jusef
    Journal of Colloid and Interface Science (2020), 573 (), 396-408CODEN: JCISA5; ISSN:0021-9797. (Elsevier B.V.)
    Disordered carbons derived from biomass are herein efficiently used as an alternative anode in lithium-ion battery. Carbon precursor obtained from cherry pit is activated by using either KOH or H3PO4, to increase the sp. surface area and enable porosity. Structure, morphol. and chem. characteristics of the activated carbons are investigated by X-ray diffraction (XRD), transmission electron microscopy (TEM), SEM (SEM), thermogravimetry (TG), Raman spectroscopy, nitrogen and mercury porosimetry. The electrodes are studied in lithium half-cell by galvanostatic cycling, cyclic voltammetry, and electrochem. impedance spectroscopy (EIS). The study evidences substantial effect of chem. activation on the carbon morphol., electrode resistance, and electrochem. performance. The materials reveal the typical profile of disordered carbon with initial irreversibility vanishing during cycles. Carbons activated by H3PO4 show higher capacity at the lower C-rates, while those activated by KOH reveal improved reversible capacity at the high currents, with efficiency approaching 100% upon initial cycles, and reversible capacity exceeding 175 mAh g-1. Therefore, the carbons and LiFePO4 cathode are combined in lithium-ion cells delivering 160 mAh g-1 at 2.8 V, with a retention exceeding 95% upon 200 cycles at C/3 rate. Hence, the carbons are suggested as environmentally sustainable anode for Li-ion battery.
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  11. 11
    Dehkhoda, A. M.; Gyenge, E.; Ellis, N. A novel method to tailor the porous structure of KOH-activated biochar and its application in capacitive deionization and energy storage. Biomass Bioenergy 2016, 87, 107– 121,  DOI: 10.1016/j.biombioe.2016.02.023
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    11
    A novel method to tailor the porous structure of KOH-activated biochar and its application in capacitive deionization and energy storage
    Dehkhoda, Amir Mehdi; Gyenge, Elod; Ellis, Naoko
    Biomass and Bioenergy (2016), 87 (), 107-121CODEN: BMSBEO; ISSN:0961-9534. (Elsevier Ltd.)
    This study reveals a novel method to tailor the micro- and meso-porous structures of activated biochar by exploiting the interaction between pre-carbonization drying conditions and carbonization temp. in KOH activation. Biochar samples were mixed with concd. KOH and then dried under air or nitrogen for various periods of time (0-280 h) followed by carbonization at 475, 675 or 875 °C. It is confirmed that by manipulating drying conditions and carbonization temps., the KOH activated biochar can have a predominantly microporous, mesoporous or a combined (micro/meso) porous structure. The surface area, micropore and mesopore vols. tailored between: 488-2670 m2 g-1, 0.04-0.72 cm3 g-1, and 0.05-1.70 cm3 g-1, resp. The mechanism of porosity development was investigated by FTIR anal. suggesting conversion of KOH to K2CO3 due to different drying conditions as a major role in tailoring the structure. The application of activated biochar with tailored porosity was investigated for Elec. Double Layer adsorption of NaCl/NaOH to be employed in water treatment (capacitive deionization) or energy storage (supercapacitor) processes. The majorly microporous activated biochar (N2-dried activated at 675 °C) showed promising capacitances between 220 and 245 F g-1. Addn. of mesoporous structure resulted in capacitances between 182 and 240 F g-1 with significantly reduced electrode resistance and improved capacitive behavior as evidenced by Impedance Spectroscopy and Galvanostatic Charge/Discharge tests.
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  12. 12
    Yu, K.; Wang, J.; Song, K.; Wang, X.; Liang, C.; Dou, Y. Hydrothermal synthesis of cellulose-derived carbon nanospheres from corn straw as anode materials for lithium-ion batteries. Nanomaterials 2019, 9, 93,  DOI: 10.3390/nano9010093
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    12
    Hydrothermal synthesis of cellulose-derived carbon nanospheres from corn straw as anode materials for lithium ion batteries
    Yu, Kaifeng; Wang, Jingjing; Song, Kexian; Wang, Xiaofeng; Liang, Ce; Dou, Yanli
    Nanomaterials (2019), 9 (1), 93/1-93/13CODEN: NANOKO; ISSN:2079-4991. (MDPI AG)
    As a most attractive renewable resource, biomass has the advantages of low pollution, wide distribution and abundant resources, promoting its applications in lithium ion batteries (LIBs). Herein, cellulose-derived carbon nanospheres (CCS) were successfully synthesized by hydrothermal carbonization (HTC) from corn straw for use as an anode in LIBs. The uniform distribution and cross-linked structure of carbon nanospheres were obtained by carefully controlling reaction time, which could not only decrease the transport pathway of lithium ions, but also reduce the structural damage caused by the intercalation of lithium ions. Esp., obtained after hydrothermal carbonization for 36 h, those typical characteristics make it deliver excellent cycling stability as well as the notable specific capacity of 577 mA h g-1 after 100 cycles at 0.2C. Hence, this efficient and environment-friendly method for the fabrication of CCS from corn straw could realize the secondary utilization of biomass waste, as well as serve as a new choice for LIBs anode materials.
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  13. 13
    Guan, Z.; Guan, Z.; Li, Z.; Liu, J.; Yu, K. Characterization and preparation of nano-porous carbon derived from hemp stems as anode for lithium-ion batteries. Nanoscale Res. Lett. 2019, 14, 338,  DOI: 10.1186/s11671-019-3161-1
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    13
    Characterization and Preparation of Nano-porous Carbon Derived from Hemp Stems as Anode for Lithium-Ion Batteries
    Guan Zhongxiang; Guan Zhiping; Li Zhigang; Liu Junhui; Yu Kaifeng; Guan Zhiping; Li Zhigang; Yu Kaifeng
    Nanoscale research letters (2019), 14 (1), 338 ISSN:1931-7573.
    As a biomass waste, hemp stems have the advantages of low cost and abundance, and it is regarded as a promising anode material with a high specific capacity. In this paper, activated carbon derived from hemp stems is prepared by low-temperature carbonization and high-temperature activation. The results of characterizations show the activated carbon has more pores due to the advantages of natural porous structure of hemp stem. The aperture size is mainly microporous, and there are mesopores and macropores in the porous carbon. The porous carbon has an excellent reversible capacity of 495 mAh/g after 100 cycles at 0.2 °C as the anode of lithium-ion battery. Compared with the graphite electrode, the electrochemical property of activated carbon is significantly improved due to the reasonable distribution of pore size. The preparation of the activated carbon provides a new idea for low cost and rapid preparation of anode materials for high capacity lithium-ion batteries.
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    Zhu, Y.-E.; Gu, H.; Chen, Y.-N.; Yang, D.; Wei, J.; Zhou, Z. Hard carbon derived from corn straw piths as anode materials for sodium ion batteries. Ionics (Kiel) 2018, 24, 1075– 1081,  DOI: 10.1007/s11581-017-2260-1
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    Tyagi, A.; Banerjee, S.; Singh, S.; Kar, K. K. Biowaste derived activated carbon electrocatalyst for oxygen reduction reaction: Effect of chemical activation. Int. J. Hydrogen Energy 2020, 45, 16930– 16943,  DOI: 10.1016/j.ijhydene.2019.06.195
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    15
    Biowaste derived activated carbon electrocatalyst for oxygen reduction reaction: Effect of chemical activation
    Tyagi, Alekha; Banerjee, Soma; Singh, Shashank; Kar, Kamal K.
    International Journal of Hydrogen Energy (2020), 45 (34), 16930-16943CODEN: IJHEDX; ISSN:0360-3199. (Elsevier Ltd.)
    Conversion of bio-wastes to useful doped carbon materials for various energy applications is emerging as a cost-effective strategy. A novel activated carbon electrocatalyst derived from chicken feather rachis (RCF), a poultry industry bio-waste is explored for oxygen redn. reaction (ORR) catalysis. The rachis is the central stem from which the fibrous ramus is completely removed and it is more cryst. compared to feather ramus. Nitrogen doped activated carbon (CNAx) electrocatalyst is prepd. by chem. activation coupled pyrolysis. The chem. activators used include potassium hydroxide (KOH), phosphoric acid (H3PO4) and zinc chloride (ZnCl2) followed by pyrolysis at 500, 700 and 900°C. Electrochem. performance has been evaluated using cyclic voltammetry (CV) and linear sweep voltammetry (LSV) using a rotating disk electrode (RDE). KOH activated electrocatalyst exhibits remarkable improvement in surface area favoring improved onset potential (-0.02 V vs Ag/AgCl). This increased activity is due to increase in no. of well-exposed ORR active sites on activation. The effect of chem. activators on the structure and morphol. of the activated carbons are discussed using Raman spectroscopy, adsorption-desorption isotherm study, electron microscopic techniques, at. force microscopy (AFM), and XPS studies. KOH activated CNAx-900 exhibits best combination of properties and confirms its feasibility to be a suitable electrocatalyst for PEMFC. Hence, RCF derived electrocatalysts are propitious alternates for ORR catalysis.
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    Zhang, Y.; Chen, L.; Meng, Y.; Xie, J.; Guo, Y.; Xiao, D. Lithium and sodium storage in highly ordered mesoporous nitrogen-doped carbons derived from honey. J. Power Sources 2016, 335, 20– 30,  DOI: 10.1016/j.jpowsour.2016.08.096
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    16
    Lithium and sodium storage in highly ordered mesoporous nitrogen-doped carbons derived from honey
    Zhang, Yongzhi; Chen, Li; Meng, Yan; Xie, Jun; Guo, Yong; Xiao, Dan
    Journal of Power Sources (2016), 335 (), 20-30CODEN: JPSODZ; ISSN:0378-7753. (Elsevier B.V.)
    Honey, a widely existent biomass, consists mainly of carbohydrate and other N-contg. substances such as proteins, enzymes and org. acids. It can be mixed homogeneously with mesoporous SiO2 template for its excellent H2O-soly. and moderate viscosity. Honey was employed as a N-contg. C precursor to prep. N-doped ordered mesoporous carbons (OMCs). The obtained honey derived mesoporous N-doped carbons (HMNCs) with dilated interlayer spacings of 0.387-0.395 nm, narrow pore size distributions centering at ∼4 nm and satisfactory N contents of 1.38-4.32% offer superb dual functionality for Li-ion battery (LIB) and Na-ion battery (NIB) anodes. Tested against Li, the optimized HMNC-700 delivers a superior reversible capacity of 1359 mA h g-1 after 10 cycles at 100 mA g-1 and excellent rate capability and cycling stability of 722 mA h g-1 after 200 cycles at 1 A g-1. For NIB applications, HMNC-700 offers a high initial reversible capacity of 427 mA h g-1 and stable reversible capacity of 394 mA h g-1 at 100 mA g-1.
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  17. 17
    Léonard, A. F.; Castro-Muñiz, A.; Suárez-García, F.; Job, N.; Paredes, J. I. Understanding the effect of the mesopore volume of ordered mesoporous carbons on their electrochemical behavior as Li-ion battery anodes. Microporous Mesoporous Mater. 2020, 306, 110417,  DOI: 10.1016/j.micromeso.2020.110417
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    17
    Understanding the effect of the mesopore volume of ordered mesoporous carbons on their electrochemical behavior as Li-ion battery anodes
    Leonard, Alexandre F.; Castro-Muniz, Alberto; Suarez-Garcia, Fabian; Job, Nathalie; Paredes, Juan I.
    Microporous and Mesoporous Materials (2020), 306 (), 110417CODEN: MIMMFJ; ISSN:1387-1811. (Elsevier B.V.)
    This work aims at understanding the effect of the mesopore vol. of ordered mesoporous carbons (OMCs) on their behavior as anodes for Li-ion batteries. To that purpose, the hard-templating method was used as an enabling tool, with the controlled partial etching of the silica template to prep. a series of OMCs with a wide range of mesopore vols. The formed carbon-silica hybrids were processed into electrodes using a water-based ink prepn. route in the presence of xanthan gum as a binder, which retained access to the pores after formation of the electrodes. The pore texture of the latter was compared to that of the starting powders. A very good linear relationship could be evidenced between the mesopore vol. of the electrodes and the first insertion capacity of Li-ions. The lithium de-insertion also followed a linear trend, but its behavior was dependent on the final applied potential. Indeed, the higher the mesopore vol., the higher the contribution of de-insertion at elevated voltages. This study further points out the importance of the textural characterization of electrodes (instead of just the starting material) as well as the conditions at which the electrochem. measurements are carried out, esp. the max. applied de-insertion voltage.
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  18. 18
    dos Reis, G. S.; Larsson, S. H.; Thyrel, M.; Pham, T. N.; Claudio Lima, E.; de Oliveira, H. P.; Dotto, G. L. Preparation and Application of Efficient Biobased Carbon Adsorbents Prepared from Spruce Bark Residues for Efficient Removal of Reactive Dyes and Colors from Synthetic Effluents. Coatings 2021, 11, 772,  DOI: 10.3390/coatings11070772
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    18
    Preparation and Application of Efficient Biobased Carbon Adsorbents Prepared from Spruce Bark Residues for Efficient Removal of Reactive Dyes and Colors from Synthetic Effluents
    dos Reis, Glaydson Simoes; Larsson, Sylvia H.; Thyrel, Mikael; Pham, Tung Ngoc; Claudio Lima, Eder; de Oliveira, Helinando Pequeno; Dotto, Guilherme L.
    Coatings (2021), 11 (7), 772CODEN: COATED; ISSN:2079-6412. (MDPI AG)
    Biobased carbon materials (BBC) obtained from Norway spruce (Picea abies Karst.) bark was produced by single-step chem. activation with ZnCl2 or KOH, and pyrolysis at 800°C for one hour. The chem. activation reagent had a significant impact on the properties of the BBCs. KOH-biobased carbon material (KOH-BBC) had a higher sp. surface area (SBET), equal to 1067 m2 g-1, larger pore vol. (0.558 cm3 g-1), more mesopores, and a more hydrophilic surface than ZnCl2-BBC. However, the carbon yield for KOH-BBC was 63‰ lower than for ZnCl2-BBC. Batch adsorption expts. were performed to evaluate the ability of the two BBCs to remove two dyes, reactive orange 16 (RO-16) and reactive blue 4 (RB-4), and treat synthetic effluents. The general order model was most suitable for modeling the adsorption kinetics of both dyes and BBCs. The equil. parameters at 22°C were calcd. using the Liu model. Upon adsorption of RO-16, Qmax was 90.1 mg g-1 for ZnCl2-BBC and 354.8 mg g-1 for KOH-BBC. With RB-4, Qmax was 332.9 mg g-1 for ZnCl2-BBC and 582.5 mg g-1 for KOH-BBC. Based on characterization and exptl. data, it was suggested that electrostatic interactions and hydrogen bonds between BBCs and RO-16 and RB-4 dyes played the most crucial role in the adsorption process. The biobased carbon materials showed high efficiency for removing RO-16 and RB-4, comparable to the best examples from the literature. Addnl., both the KOH- and ZnCl2-BBC showed a high ability to purify two synthetic effluents, but the KOH-BBC was superior.
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  19. 19
    Lima, D. R.; Lima, E. C.; Thue, P. S.; Dias, S. L. P.; Machado, F. M.; Seliem, M. K.; Sherf, F.; dos Reis, G. S.; Saeb, M. R.; Rinklebe, J. Comparison of acidic leaching using a conventional and ultrasound-assisted method for preparation of magnetic-activated biochar. J. Environ. Chem. Eng. 2021, 9, 105865,  DOI: 10.1016/j.jece.2021.105865
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    19
    Comparison of acidic leaching using a conventional and ultrasound-assisted method for preparation of magnetic-activated biochar
    Lima, Diana R.; Lima, Eder C.; Thue, Pascal S.; Dias, Silvio L. P.; Machado, Fernando M.; Seliem, Moaaz K.; Sher, Farooq; dos Reis, Glaydson S.; Saeb, Mohammad Reza; Rinklebe, Jorg
    Journal of Environmental Chemical Engineering (2021), 9 (5), 105865CODEN: JECEBG; ISSN:2213-3437. (Elsevier Ltd.)
    Four magnetic biochars (MBs) were prepd. from two mixts. of Sappeli sawdust with NiCl2 soln. or Sappeli sawdust with NiCl2 plus ZnCl2 solns. These mixts. formed two pastes that were dried and further pyrolyzed at 700 °C under nitrogen flow. The pyrolyzed material was leached out with 0.1 M HCl under conventional reflux (AL- 80 °C, 2 h) or assisted by ultrasound-leaching (US- 15 min, 600 W), obtaining four biochars: SNiAL, SNiUS, SNiZnAL, SNiZnUS. The biochars were characterized by VSM, XRD, FTIR, isotherms of adsorption and desorption of nitrogen, pHpzc, hydrophobically characteristics (HI), TGA, elemental anal. (CHN/O). The data show that using the leaching process assisted by ultrasound can obtain biochars that present good magnetization satn., with a lower leaching time than conventional leaching. The four biochar were tested as adsorbents to remove ten emerging contaminants and four dyes of aq. effluents. It was obsd. that the impregnation of zinc chloride in the samples led to an increase in the surface areas of the magnetic biochars, which influenced the most of sorption capacities of the adsorbents for the different sorbing species. Making a ratio of sorption capacities of SNiAL/SNiZnAL and SNiUS/SNiZnUS, it was obtained the values, resp., of 0.9761, and 0.9710 (Acid Red 1), 2.057, and 3.030 (Reactive Blue 4), 4.192, and 1.971 (Basic Violet 3), 3.359, and 1.129 (Basic Green 1), 1.673, and 1.835 (Paracetamol), 3.612, and 3.779 (Propranolol), 5.871, and 5.171 (Sodium Diclofenac), 1.457, and 1.607 (Nicotinamide), 1.094 and 1.093 (Caffeine), 1.167, and 2.398 (4-chloroaniline), 1.009 and 0.9965 (2-nitrophenol), 1.156 and 1.341 (Resorcinol), 1.299 and 1.331 (Hydroquinone), 0.9975 and 1.019 (4-bromophenol).
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    Moralı, U.; Demiral, H.; Şensöz, S. Optimization of activated carbon production from sunflower seed extracted meal: Taguchi design of experiment approach and analysis of variance. J. Cleaner Prod. 2018, 189, 602– 611,  DOI: 10.1016/j.jclepro.2018.04.084
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    20
    Optimization of activated carbon production from sunflower seed extracted meal: Taguchi design of experiment approach and analysis of variance
    Morali, Ugur; Demiral, Hakan; Sensoz, Sevgi
    Journal of Cleaner Production (2018), 189 (), 602-611CODEN: JCROE8; ISSN:0959-6526. (Elsevier Ltd.)
    Taguchi method has been applied to design optimal activation conditions in the prodn. of activated carbon with high sp. surface area using sunflower seed extd. meal through chem. activation using either zinc chloride or phosphoric acid. The activation temp. and the impregnation ratio were selected as the factors of the activation process to be optimized. The activated carbons were prepd. according to the L9 orthogonal array. Brunauer-Emmett-Teller surface area of the activated carbons was calcd. by using nitrogen adsorption data obtained at -196° C. The optimum level of the activation temp. for prepg. the activated carbon with a high surface area was 600° C for both chem. agents. The optimal levels of the impregnation ratio for a high sp. surface area were detd. as 3:1 and 2:1 for zinc chloride and phosphoric acid, resp. The results of this study showed that the activation temp. is the most significant factor to get activated carbons with higher sp. surface area. Taguchi method also allows a more detailed and accurate assessment to prep. the activated carbon in a cleaner way.
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  21. 21
    Thue, P. S.; Umpierres, C. S.; Lima, E. C.; Lima, D. R.; Machado, F. M.; dos Reis, G. S.; da Silva, R. S.; Pavan, F. A.; Tran, H. N. Single-step pyrolysis for producing magnetic activated carbon from tucumã (Astrocaryum aculeatum) seed and nickel(II) chloride and zinc(II) chloride. Application for removal of Nicotinamide and Propanolol. J. Hazard. Mater. 2020, 398, 122903,  DOI: 10.1016/j.jhazmat.2020.122903
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    21
    Single-step pyrolysis producing magnetic activated carbon from tucuma~ (Astrocaryum aculeatum) seed and nickel(II) chloride and zinc(II) chloride for removal of nicotinamide and propanolol
    Thue, Pascal S.; Umpierres, Cibele S.; Lima, Eder C.; Lima, Diana R.; Machado, Fernando M.; dos Reis, Glaydson S.; da Silva, Raphaelle S.; Pavan, Flavio A.; Tran, Hai Nguyen
    Journal of Hazardous Materials (2020), 398 (), 122903CODEN: JHMAD9; ISSN:0304-3894. (Elsevier B.V.)
    The present research describes the synthesis of new nanomagnetic activated carbon material with high magnetization, and high surface area prepd. in a single pyrolysis step that is used for the carbonization, activation, and magnetization of the produced material. The pyrolysis step of tucuma~ seed was carried out in a conventional tubular oven at 600°C under N2-flow. It was prepd. three magnetic carbons MT-1.5, MT-2.0, MT-2.5, that corresponds to the proportion of biomass: ZnCl2 always 1:1 and varying the proportion of NiCl2 of 1.5, 2.0, and 2.5, resp. These magnetic nanocomposites were characterized by Vibrating Sample Magnetometer (VSM), X-ray diffraction, SEM, thermogravimetric anal., hydrophobic/hydrophilic balance, CHN/O elemental anal., modified Boehm titrn., N2 adsorption-desorption isotherms; and pHpzc. All the materials obtained presented Ni particles with an av. crystallite size of less than 33 nm. The MT-2.0 was employed for the removal of nicotinamide and propranolol from aq. solns. Based on Liu isotherm, the Qmax was 199.3 and 335.4 mg g-1 for nicotinamide and propranolol, resp. MT-2.0 was used to treat simulated pharmaceutical industry effluents attaining removal of all org. compds. attaining up to 99.1% of removal.
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    Liu, Z.; Yuan, X.; Zhang, S.; Wang, J.; Huang, Q.; Yu, N.; Zhu, Y.; Fu, L.; Wang, F.; Chen, Y.; Wu, Y. Three-dimensional ordered porous electrode materials for electrochemical energy storage. NPG Asia Mater. 2019, 11, 12,  DOI: 10.1038/s41427-019-0112-3
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    Three-dimensional ordered porous electrode materials for electrochemical energy storage
    Liu, Zaichun; Yuan, Xinhai; Zhang, Shuaishuai; Wang, Jing; Huang, Qinghong; Yu, Nengfei; Zhu, Yusong; Fu, Lijun; Wang, Faxing; Chen, Yuhui; Wu, Yuping
    NPG Asia Materials (2019), 11 (1), 12CODEN: NAMPCE; ISSN:1884-4057. (Nature Research)
    A review. The past decade has witnessed substantial advances in the synthesis of various electrode materials with three-dimensional (3D) ordered macroporous or mesoporous structures (the so-called "inverse opals") for applications in electrochem. energy storage devices. This review summarizes recent advancements in 3D ordered porous (3DOP) electrode materials and their unusual electrochem. properties endowed by their intrinsic and geometric structures. The 3DOP electrode materials discussed here mainly include carbon materials, transition metal oxides (such as TiO2, SnO2, Co3O4, NiO, Fe2O3, V2O5, Cu2O, MnO2, and GeO2), transition metal dichalcogenides (such as MoS2 and WS2), elementary substances (such as Si, Ge, and Au), intercalation compds. (such as Li4Ti5O12, LiCoO2, LiMn2O4, LiFePO4), and conductive polymers (polypyrrole and polyaniline). Representative applications of these materials in Li ion batteries, aq. rechargeable lithium batteries, Li-S batteries, Li-O2 batteries, and supercapacitors are presented. Addnl., we discuss research opportunities as well as the current challenges to facilitate further contributions to this emerging research frontier.
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    Chu, K.; Zhang, X.; Yang, Y.; Li, Z.; Wei, L.; Yao, G.; Zheng, F.; Chen, Q. Edge-nitrogen enriched carbon nanosheets for potassium-ion battery anodes with an ultrastable cycling stability. Carbon 2021, 184, 277– 286,  DOI: 10.1016/j.carbon.2021.08.015
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    Edge-nitrogen enriched carbon nanosheets for potassium-ion battery anodes with an ultrastable cycling stability
    Chu, Kainian; Zhang, Xiaojuan; Yang, Yang; Li, Zhiqiang; Wei, Lingzhi; Yao, Ge; Zheng, Fangcai; Chen, Qianwang
    Carbon (2021), 184 (), 277-286CODEN: CRBNAH; ISSN:0008-6223. (Elsevier Ltd.)
    Edge-nitrogen (pyridinic/pyrrolic nitrogen) doped carbon materials have been considered as promising anodes for potassium ion batteries (KIBs), which can provide a high surface-induced capacitive capacity beyond the K+-intercalated mechanism. However, achieving a high-level edge-nitrogen doping is still a great challenge owning to inevitable introduction of graphitic nitrogen into carbon materials via conventional pyrolysis process. Herein, we design porous carbon nanosheets with bundant defects and edge sites to graft nitrogen atoms to achieve a high-level edge-nitrogen doping (88.36%). The optimized edge-nitrogen doped carbon nanosheets (ENCNs-600) exhibits a high reversible capacity of 443 mAh g-1 at 0.1 A g-1 after 200 cycles, excellent rate performance (175 mAh g-1 at 20 A g-1), and ultrastable cycling stability (246 mAh g-1 at 5 A g-1 over 10,000 cycles). D. functional theory calcns. and kinetic studies confirm that both edge-nitrogen doping and explanded interlayer distance are greatly conducive for the adsorption and diffusion of K+, thereby ensuring enhanced potassium-storage performance with a synergistic adsorption-intercalation mechanism.
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  24. 24
    Xu, Y.; Sun, X.; Li, Z.; Wei, L.; Yao, G.; Niu, H.; Yang, Y.; Zheng, F.; Chen, Q. Boosting the K+ −adsorption capacity in edgenitrogen doped hierarchically porous carbon spheres for ultrastable potassium ion battery anodes. Nanoscale 2021, 13, 19634– 19641,  DOI: 10.1039/D1NR06665J
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    24
    Boosting the K+-adsorption capacity in edge-nitrogen doped hierarchically porous carbon spheres for ultrastable potassium ion battery anodes
    Xu, Yang; Sun, Xinpeng; Li, Zhiqiang; Wei, Lingzhi; Yao, Ge; Niu, Heling; Yang, Yang; Zheng, Fangcai; Chen, Qianwang
    Nanoscale (2021), 13 (46), 19634-19641CODEN: NANOHL; ISSN:2040-3372. (Royal Society of Chemistry)
    Although carbon materials have great potential for potassium ion battery (KIB) anodes due to their structural stability and abundant carbon-contg. resources, the limited K+-intercalated capacity impedes their extensive applications in energy storage devices. Current research studies focus on improving the surface-induced capacitive behavior to boost the potassium storage capacity of carbon materials. Herein, we designed edge-nitrogen (pyridinic-N and pyrrolic-N) doped carbon spheres with a hierarchically porous structure to achieve high potassium storage properties. The electrochem. tests confirmed that the edge-nitrogen induced active sites were conducive for the adsorption of K+, and the hierarchical porous structure promoted the generation of stable solid electrolyte interphase (SEI) films, both of which endow the resulting materials with a high reversible capacity of 381.7 mA h g-1 at 0.1 A g-1 over 200 cycles and an excellent rate capability of 178.2 mA h g-1 at 5 A g-1. Even at 5 A g-1, the long-term cycling stability of 5000 cycles was achieved with a reversible capacity of 190.1 mA h g-1. This work contributes to deeply understand the role of the synergistic effect of edge-nitrogen induced active sites and the hierarchical porous structure in the potassium storage performances of carbon materials.
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  25. 25
    Niu, P.; Yang, Y.; Li, Z.; Ding, G.; Wei, L.; Yao, G.; Niu, H.; Min, Y.; Zheng, F.; Chen, Q. Rational design of a hollow porous structure for enhancing diffusion kinetics of K ions in edge-nitrogen doped carbon nanorods. Nano Res. 2022, 15, 8109– 8117,  DOI: 10.1007/s12274-022-4496-y
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    25
    Rational design of a hollow porous structure for enhancing diffusion kinetics of K ions in edge-nitrogen doped carbon nanorods
    Niu, Ping; Yang, Yang; Li, Zhiqiang; Ding, Gaohui; Wei, Lingzhi; Yao, Ge; Niu, Helin; Min, Yulin; Zheng, Fangcai; Chen, Qianwang
    Nano Research (2022), 15 (9), 8109-8117CODEN: NRAEB5; ISSN:1998-0000. (Springer GmbH)
    The high elec. cond. makes it possible for one-dimensional (1D) carbon materials to be used as the promising anodes for potassium ion batteries (PIBs), however, the sluggish diffusion kinetics caused by large-sized potassium ions (K+) limits their practical applications in energy storage systems. In this work, hollow carbon nanorods were rationally designed as a case to verify the superiority of 1D hollow structure to improve the diffusion kinetics of K+. Simultaneously, edge-N (pyridinic-N and pyrrolic-N) atoms were also introduced into 1D hollow carbon structure, which can provide ample active sites and defects in graphitic lattices to adsorb K+, providing extra capacitive storage capacity. As expected, the optimized edge-N doped hollow carbon nanorods (ENHCRs) exhibits a high reversible capacity of 544 mAh·g-1v at 0.1 A·g-1 after 200 cycles. Even at 5 A·g-1, it displays a long-term cycling stability with 255 mAh·g-1 over 10,000 cycles. The electrochem. measurements confirm that the hollow structure is favorable to improve the transfer kinetics of K+ during cycling. And the theor. calcns. demonstrate that edge-N doping can enhance the local electronegativity of graphitic lattices to adsorb much more K+, where edge-N doping synergizes with 1D hollow structure to achieve enhanced K+-storage performances.
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  26. 26
    dos Reis, G. S.; Guy, M.; Mathieu, M.; Jebrane, M.; Lima, E. C.; Thyrel, M.; Dotto, G. L.; Larsson, S. H. A comparative study of chemical treatment by MgCl2, ZnSO4, ZnCl2, and KOH on physicochemical properties and acetaminophen adsorption performance of biobased porous materials from tree bark residues. Colloids Surf., A 2022, 642, 128626,  DOI: 10.1016/j.colsurfa.2022.128626
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    26
    A comparative study of chemical treatment by MgCl2, ZnSO4, ZnCl2, and KOH on physicochemical properties and acetaminophen adsorption performance of biobased porous materials from tree bark residues
    dos Reis, Glaydson S.; Guy, Marine; Mathieu, Manon; Jebrane, Mohamed; Lima, Eder C.; Thyrel, Mikael; Dotto, Guilherme L.; Larsson, Sylvia H.
    Colloids and Surfaces, A: Physicochemical and Engineering Aspects (2022), 642 (), 128626CODEN: CPEAEH; ISSN:0927-7757. (Elsevier B.V.)
    Prepg. sustainable and highly efficient biomass-based carbon materials (BBPM) as adsorbents remains a challenge for org. pollutant management. In this work, novel biobased carbon material has been synthesized via facile, sustainable, and different single-step pyrolysis chem. methods (KOH, ZnCl2, ZnSO4, and MgCl2) using a Norway spruce bark as suitable and efficient carbon precursor. The effects of each chem. activator on the physicochem. structure of synthesized were thoroughly investigated as well as its performance on the acetaminophen adsorption. The results showed that the use of different chem. activation provoked remarkable differences in the BBPM physicochem. characteristics. The KOH activation generated material with the highest sp. surface area (2209 m2 g-1), followed by ZnCl2 (1019 m2 g-1), ZnSO4 (446 m2 g-1), and MgCl2 (98 m2 g-1). The chem. characterization of the carbon materials indicated that the activation of MgCl2 yielded a material around three times more hydrophobic when compared with the other activation methods. The acetaminophen removal showed to be ultrafast, not only due to the BBPM's microstructure but also to the abundant active sites provided by the different chem. activation methods. The adsorption equil. times were reached at 1 min for BBPM-KOH and BBPM-MgCl2 and 15 min for BBPM-ZnSO4 and BBPM-ZnCl2. The adsorption process suggests that the pore-filling mechanism mainly dominates the acetaminophen removal but also some phys.-chem. interactions such as hydrogen bonding between the amide group of acetaminophen and oxygenated or nitrogenated groups of biochar, π-π interactions between the arom. ring of the pharmaceutical and the aroms. of biochar, n-π interaction, van der Waals interactions. The BBPM regeneration studies showed very good cyclability; in the 3rd cycle, the removal was approx. 70% for all four samples. The samples were also used to treat two synthetic effluents, which attained a removal percentage up to 91.9%.
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  27. 27
    Guy, M.; Mathieu, M.; Anastopoulos, I. P.; Martínez, M. G.; Rousseau, F.; Dotto, G. L.; de Oliveira, H. P.; Lima, E. C.; Thyrel, M.; Larsson, S. H.; dos Reis, G. S. Process Parameters Optimization, Characterization, and Application of KOH-Activated Norway Spruce Bark Graphitic Biochars for Efficient Azo Dye Adsorption. Molecules 2022, 27, 456,  DOI: 10.3390/molecules27020456
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    27
    Process Parameters Optimization, Characterization, and Application of KOH-Activated Norway Spruce Bark Graphitic Biochars for Efficient Azo Dye Adsorption
    Guy, Marine; Mathieu, Manon; Anastopoulos, Ioannis P.; Martinez, Maria G.; Rousseau, Frederic; Dotto, Guilherme L.; de Oliveira, Helinando P.; Lima, Eder C.; Thyrel, Mikael; Larsson, Sylvia H.; dos Reis, Glaydson S.
    Molecules (2022), 27 (2), 456CODEN: MOLEFW; ISSN:1420-3049. (MDPI AG)
    In this work, Norway spruce bark was used as a precursor to prep. activated biochars (BCs) via chem. activation with potassium hydroxide (KOH) as a chem. activator. A Box-Behnken design (BBD) was conducted to evaluate and identify the optimal conditions to reach high sp. surface area and high mass yield of BC samples. The studied BC prepn. parameters and their levels were as follows: pyrolysis temp. (700, 800, and 900°C), holding time (1, 2, and 3 h), and ratio of the biomass: chem. activator of 1: 1, 1.5, and 2. The planned BBD yielded BC with extremely high SSA values, up to 2209 m2·g-1. In addn., the BCs were physiochem. characterized, and the results indicated that the BCs exhibited disordered carbon structures and presented a high quantity of O-bearing functional groups on their surfaces, which might improve their adsorption performance towards org. pollutant removal. The BC with the highest SSA value was then employed as an adsorbent to remove Evans blue dye (EB) and colorful effluents. The kinetic study followed a general-order (GO) model, as the most suitable model to describe the exptl. data, while the Redlich-Peterson model fitted the equil. data better. The EB adsorption capacity was 396.1 mg·g-1. The employment of the BC in the treatment of synthetic effluents, with several dyes and other org. and inorg. compds., returned a high percentage of removal degree up to 87.7%. Desorption and cyclability tests showed that the biochar can be efficiently regenerated, maintaining an adsorption capacity of 75% after 4 adsorption-desorption cycles. The results of this work pointed out that Norway spruce bark indeed is a promising precursor for producing biochars with very promising properties.
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  28. 28
    Li, Y.; Li, S.; Wang, Y.; Wang, J.; Liu, H.; Liu, X.; Wang, L.; Liu, X.; Xue, W.; Ma, N. Electrochemical synthesis of phosphorus-doped graphene quantum dots for free radical scavenging. Phys. Chem. Chem. Phys. 2017, 19, 11631,  DOI: 10.1039/C6CP06377B
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    Electrochemical synthesis of phosphorus-doped graphene quantum dots for free radical scavenging
    Li, Yan; Li, Sen; Wang, Yingmin; Wang, Jun; Liu, Hui; Liu, Xinqian; Wang, Lifeng; Liu, Xiaoguang; Xue, Wendong; Ma, Ning
    Physical Chemistry Chemical Physics (2017), 19 (18), 11631-11638CODEN: PPCPFQ; ISSN:1463-9076. (Royal Society of Chemistry)
    P-doped graphene quantum dots (P-GQDs) with a high P doping content (>7 at.%) are synthesized via an electrochem. approach. Na phytate (C6H6Na12O24P6), a green food antioxidant additive, is used as the electrolyte for providing both a P source and an electrolysis environment. The obtained P-GQDs exhibit excellent scavenging activity of free radicals, such as hydroxyl radicals (̇ OH) and 2,2-diphenyl-1-picrylhydrazyl (DPPH). Combined with Raman, FTIR, and XPS spectral analyses, the reason for high P content and the mechanism of free radical scavenging of P-GQDs are studied.
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  29. 29
    Yuan, C.; Chen, M.; Zhu, K.; Ni, J.; Wang, S.; Cao, B.; Zhong, S.; Zhou, J.; Wang, S. Facile synthesis of nitrogen-doped interconnected porous carbons derived from reed and chlorella for high-performance supercapacitors. Fuel Process. Technol. 2022, 238, 107466,  DOI: 10.1016/j.fuproc.2022.107466
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    Facile synthesis of nitrogen-doped interconnected porous carbons derived from reed and chlorella for high-performance supercapacitors
    Yuan, Chuan; Chen, Mao; Zhu, Kai; Ni, Jun; Wang, Shuang; Cao, Bin; Zhong, Shan; Zhou, Jingsong; Wang, Shurong
    Fuel Processing Technology (2022), 238 (), 107466CODEN: FPTEDY; ISSN:0378-3820. (Elsevier Ltd.)
    Three-dimensionally (3D) nitrogen (N)-doped interconnected porous carbons (IPC) derived from cost-effective biomasses were facilely prepd. by one-step method and utilized as electrochem. double layer capacitor (EDLC) electrodes. The reed and chlorella derived interconnected porous carbons (denoted as IPC-R and IPC-C) through carbonization with chem. activation both exhibited typical capacitive behaviors; importantly, by introducing N-rich chlorella into N-free reed by interactive-carbonization, the resultant N-doped interconnected porous carbons (IPC-RC) pos. demonstrated a high N content, a large sp. surface area and pore vol. as well as a high graphitization, which are crucial for fast ion diffusion and thus enhancing the electrochem. properties of supercapacitor. In the three-electrode system, the IPC-RC1.2 showed a superb specific capacitance of 340.4 F/g at a c.d. of 1 A/g, one of the highest capacitances for biomass derived-carbon electrodes reported so far. Even at 20 A/g, the capacitance could achieve 265.5 F/g, revealing the superb rate capability. In the sym. two-electrode system, the max. power d. and energy d. reached up to 23.6 Wh/kg and 15,000 W/kg, resp. Besides, an outstanding cycling stability was obsd. after 10,000 cycles.
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  30. 30
    Hou, S.; Cai, X.; Wu, H.; Yu, X.; Peng, M.; Yan, K.; Zou, D. Nitrogen-doped graphene for dye-sensitized solar cells and the role of nitrogen states in triiodide reduction. Energy Environ. Sci. 2013, 6, 3356– 3362,  DOI: 10.1039/c3ee42516a
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    Nitrogen-doped graphene for dye-sensitized solar cells and the role of nitrogen states in triiodide reduction
    Hou, Shaocong; Cai, Xin; Wu, Hongwei; Yu, Xiao; Peng, Ming; Yan, Kai; Zou, Dechun
    Energy & Environmental Science (2013), 6 (11), 3356-3362CODEN: EESNBY; ISSN:1754-5706. (Royal Society of Chemistry)
    Nitrogen-doped graphene was demonstrated as an efficient and alternative metal-free electrocatalyst for dye-sensitized solar cells. Electrochem. measurements showed that the nitrogen-doping process can remarkably improve the catalytic activity of graphene toward triiodide redn., lower the charge transfer resistance, and thus enhance the corresponding photovoltaic performance. Furthermore, the nitrogen doping levels ranging from 3.5 at% to 18 at%, as well as the nitrogen states (including pyrrolic, pyridinic and quaternary configurations) in graphene, were controlled to interpret the roles of graphene structure in catalytic activity and device performance. The results suggested that the nitrogen states, rather than the total N content, have a significant effect on the catalytic activity. Both pyridinic and quaternary nitrogen states can provide active sites for promoting triiodide redn. reaction, probably due to the shift in redox potential and the lowered adsorption energy.
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  31. 31
    Wei, M.; Marrakchi, F.; Yuan, C.; Cheng, X.; Jiang, D.; Zafar, F. F.; Fu, Y.; Wang, S. Adsorption modeling, thermodynamics, and DFT simulation of tetracycline onto mesoporous and high-surface-area NaOH-activated macroalgae carbon. J. Hazard. Mater. 2022, 425, 127887,  DOI: 10.1016/j.jhazmat.2021.127887
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    Adsorption modeling, thermodynamics, and DFT simulation of tetracycline onto mesoporous and high-surface-area NaOH-activated macroalgae carbon
    Wei, Manman; Marrakchi, Fatma; Yuan, Chuan; Cheng, Xiaoxue; Jiang, Ding; Zafar, Fatemeh Fazeli; Fu, Yanxia; Wang, Shuang
    Journal of Hazardous Materials (2022), 425 (), 127887CODEN: JHMAD9; ISSN:0304-3894. (Elsevier B.V.)
    Activated carbon (ENAC) was prepd. by NaOH activation, using macroalgae (Enteromorpha clathrate) as raw material. The prepd. activated carbon has a large surface area (1238.491 m2 g-1) and its total pore vol. and av. pore size are 0.6823 cm3g-1 and 2.2038 nm, resp. The ENAC was characterized by SEM, FTIR, BET and XPS. The effects of contact time (0-960 min), initial tetracycline (TC) concn. (50-500 mg L-1), temp. (30-50°C) and initial pH (2-11) on TC adsorption were evaluated. The adsorption isotherm and adsorption kinetics were discussed. Results showed that the adsorption isotherm was the Langmuir model, and the adsorption process can be described by the pseudo-second-order model. The N2 adsorption-desorption isotherm was type IV, indicating that the activated carbon had mesoporous structure. Thermodn. anal. showed that the adsorption process was endothermic and spontaneous. The max. adsorption capacity of TC was 381.584 mg g-1. D. functional theory (DFT) was used to simulate and analyze the adsorption process, and the influence of different types of N on the adsorption was expounded. The results showed that there are electrostatic interactions, π-π interactions and hydrogen bonding between the adsorbent and TC. These results indicated that the prepd. ENAC had a great application prospect in the removal of antibiotics from aq. soln.
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    Sun, L.; Tian, C.; Li, M.; Meng, X.; Wang, L.; Wang, R.; Yin, J.; Fu, H. From coconut shell to porous graphene-like nanosheets for high-power supercapacitors. J. Mater. Chem. A 2013, 1, 6462– 6470,  DOI: 10.1039/c3ta10897j
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    From coconut shell to porous graphene-like nanosheets for high-power supercapacitors
    Sun, Li; Tian, Chungui; Li, Meitong; Meng, Xiangying; Wang, Lei; Wang, Ruihong; Yin, Jie; Fu, Honggang
    Journal of Materials Chemistry A: Materials for Energy and Sustainability (2013), 1 (21), 6462-6470CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
    Sheet-like graphitic carbon with a porous structure can provide low-resistant pathways and short ion-diffusion channels for energy storage, and thus is expected to be an excellent material for high-power supercapacitors. Herein, porous graphene-like nanosheets (PGNSs) with a large surface area were synthesized for the first time via an easy and cost-effective SAG (simultaneous activation-graphitization) route from renewable biomass waste coconut shell. In the synthesis, the graphitic catalyst precursor (FeCl3) and activating agent (ZnCl2) were introduced simultaneously into the skeleton of the coconut shell through coordination of the metal precursor with the functional groups in the coconut shell, thus making simultaneous realization of activation and graphitization of the carbon source under heat treatment. Notably, the iron catalyst in the framework of the coconut shell can generate a carburized phase which plays a key role in the formation of a graphene-like structure during the pyrolytic process. The results indicated that PGNSs possess good elec. cond. due to the high graphitic degree, exceptionally high Brunauer-Emmett-Teller surface area (SBET = 1874 m2 g-1) and large pore vol. (1.21 cm3 g-1). While being used as a supercapacitor electrode without the use of any conductive additives, PGNSs exhibit a high specific capacitance of 268 F g-1, much higher than that of activated carbon (210 F g-1) fabricated by only activation and graphitic carbon (117 F g-1) by only graphitization at 1 A g-1. Also, PGNSs show superior cycle durability and Coulombic efficiency over 99.5% after 5000 cycles in KOH. Remarkably, in an org. electrolyte, PGNSs also display an outstanding capacitance of 196 F g-1 at 1 A g-1. An energy d. of up to 54.7 W h kg-1 could be achieved at a high power d. of 10 kW kg-1. The SAG strategy developed here would provide a novel route for low-cost and large-scale prodn. of PGNS electrode materials for high-power supercapacitors.
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    Chen, W.; Wang, X.; Feizbakhshan, M.; Liu, C.; Hong, S.; Yang, P.; Zhou, X. Preparation of lignin-based porous carbon with hierarchical oxygen enriched structure for high-performance supercapacitors. J. Colloid Interface Sci. 2019, 540, 524– 534,  DOI: 10.1016/j.jcis.2019.01.058
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    Preparation of lignin-based porous carbon with hierarchical oxygen-enriched structure for high-performance supercapacitors
    Chen, Weimin; Wang, Xin; Feizbakhshan, Mohammad; Liu, Chaozheng; Hong, Shu; Yang, Pei; Zhou, Xiaoyan
    Journal of Colloid and Interface Science (2019), 540 (), 524-534CODEN: JCISA5; ISSN:0021-9797. (Elsevier B.V.)
    The biomass-based porous carbon produced by the conventional two-step method (carbonization followed by chem. activation) has a high prodn. cost and an undeveloped mesopore/macropore structure. In this study, lignin was successfully converted into porous carbon (LPC) in one step by microwave heating combined with the use of humidified nitrogen. The obtained LPC had abundant micropores (0.70 cm-3·g-1), hierarchical pore distribution (mesopore ratio: 65.8%), and an oxygen-enriched chem. structure (surface oxygen content: 16.5%). These characteristics provided a high energy d. (23.0 kW·kg-1 at 10 A·g-1) and excellent rate capability of the prepd. supercapacitor in a gel electrolyte (polyvinyl alc./LiCl), leading to a high specific capacitance of 173 F·g-1 at 0.5 A·g-1, and 71.1% at 10 A·g-1 remains. The prepd. supercapacitor could deliver a high power d. of 1.1 kW·kg-1 at the max. energy d. The obtained results demonstrate the feasibility of the proposed energy-saving cost-effective prepn. approach to obtain a high-performance supercapacitor with a low prodn. cost.
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    Song, M.; Zhou, Y.; Ren, X.; Wan, J.; Du, Y.; Wu, G.; Ma, F. Biowaste-based porous carbon for supercapacitor: The influence of preparation processes on structure and performance. J. Colloid Interface Sci. 2019, 535, 276– 286,  DOI: 10.1016/j.jcis.2018.09.055
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    34
    Biowaste-based porous carbon for supercapacitor: The influence of preparation processes on structure and performance
    Song, Mingyuan; Zhou, Yuhao; Ren, Xue; Wan, Jiafeng; Du, Yueyao; Wu, Guang; Ma, Fangwei
    Journal of Colloid and Interface Science (2019), 535 (), 276-286CODEN: JCISA5; ISSN:0021-9797. (Elsevier B.V.)
    Here, a series of porous carbon based supercapacitor electrode materials have been synthesized by means of pyrolysis and hydrothermal methods combining with KOH activation using the biomass wastes mung bean husks as resources. The influence of synthesis process on the morphol., structure and supercapacitor performance of mung bean husks derived porous carbons has been investigated systematically. Esp., it is found that these oxygen-contg. groups on the biochar play a crucial role in fabricating the three-dimensional (3D) hierarchical porous structure carbon. The original bio-structured porous carbon (PC3-600), the 3D architecture porous carbon (HPC2-700) and the porous carbon block (HPPC2-700) have a high sp. surface area, and the former mainly contains micropores and the latter two possess multistage pores. The specific capacitance of PC3-600, HPC2-700 and HPPC2-700 is resp. up to 390 F g-1, 353 F g-1, 304 F g-1 at 1 A g-1, and still maintains as high as 287 F g-1, 270 F g-1 and 235 F g-1 with corresponding retention ratio of 73.5%, 76.48%, 77.3% even at a high c.d. of 50 A g-1. HPC2-700//HPC2-700 sym. supercapacitor achieves a high energy d. of 20.4 Wh kg-1 at 872 W kg-1 in 1 M Na2SO4 electrolyte.
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    Peiris, C.; Nayanathara, O.; Navarathna, C.-M.; Jayawardhana, Y.; Nawalage, S.; Burk, G.; Karunanayake, A. G.; Madduri, S. B.; Vithanage, M.; Kaumal, M. N.; Mlsna, T. E.; Hassan, E. B.; Abeysundara, S.; Ferezi, F.; Gunatilake, S. R. The influence of three acid modifications on the physicochemical characteristics of tea-waste biochar pyrolyzed at different temperatures: a comparative study. RSC Adv. 2019, 9, 17612– 17622,  DOI: 10.1039/C9RA02729G
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    The influence of three acid modifications on the physicochemical characteristics of tea-waste biochar pyrolyzed at different temperatures: a comparative study
    Peiris, Chathuri; Nayanathara, Oshani; Navarathna, Chanaka M.; Jayawardhana, Yohan; Nawalage, Samadhi; Burk, Griffin; Karunanayake, Akila G.; Madduri, Sunith B.; Vithanage, Meththika; Kaumal, M. N.; Mlsna, Todd E.; Hassan, El Barbary; Abeysundara, Sachith; Ferez, Felio; Gunatilake, Sameera R.
    RSC Advances (2019), 9 (31), 17612-17622CODEN: RSCACL; ISSN:2046-2069. (Royal Society of Chemistry)
    Tea-waste is an abundant feedstock for producing biochar (BC) which is considered to be a cost effective carbonaceous adsorbent useful for water remediation and soil amendment purposes. In the present study, tea-waste BC (TWBC) produced at three different temps. were subjected to nitric, sulfuric and hydrochloric acid modifications (abbreviated as NM, SM and HM resp.). Characteristics of the raw and modified BC such as ultimate and proximate analyses, surface morphol., surface acidity and functionality, point of zero charge, cation exchange capacity (CEC) and thermal stability were compared to evaluate the influence of pyrolysis temp. and of modifications incorporated. The amt. of carboxylic and phenolic surface functionalities on TWBC was seen to decrease by 93.44% and 81.06% resp. when the pyrolysis temp. was increased from 300 to 700°. Addnl., the yield of BC was seen to decrease by 46% upon the latter temp. increment. The elemental anal. results provided justification for high-temp. BC being more hydrophobic as was obsd. by the 61% increase in H/C ratio which is an indication of augmented aromatization. The CEC was the highest for the low-temp. BC and was seen to further increase by NM which is attributed to the 81.89% increase in carboxylic functionalities. The surface area was seen to significantly increase for BC700 upon NM (∼27 times). The SM led to pore wall destruction which was obsd. in SEM images. Findings would enable the rational use of these particular modifications in relevant remediation and soil amendment applications.
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    Thithai, V.; Jin, X.; Ajaz Ahmed, M.; Choi, J.-W. Physicochemical Properties of Activated Carbons Produced from Coffee Waste and Empty Fruit Bunch by Chemical Activation Method. Energies 2021, 14, 3002,  DOI: 10.3390/en14113002
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    Physicochemical properties of activated carbons produced from coffee waste and empty fruit bunch by chemical activation method
    Thithai, Vilaysit; Jin, Xuanjun; Ahmed, Muhammed Ajaz; Choi, Joon-Weon
    Energies (Basel, Switzerland) (2021), 14 (11), 3002CODEN: ENERGA; ISSN:1996-1073. (MDPI AG)
    In this study, coffee waste (CW) and empty fruit bunches (EFB) were employed as pre-cursors for the prodn. of activated carbons by a chem. activation method. KOH, ZnCl2, and H3PO4 were used as activating agents along with their three mixing ratios of 1:0, 1:1, 1:3, wt./wt., and carbonization temps. of 600°C, 700°C, and 800°C were used to prep. these activated carbons. The highest yields of produced activated carbons were obsd. at 600°C with a value of 45.20% for coffee waste and 48.20% for empty fruit bunch, with a 1:3 wt./wt. (H3PO4) ratio. However, the max. sp. surface area was 3068 m2 g-1, and 2147 m2 g-1 obtained at 800°C for coffee waste and empty fruit bunch activated carbons, resp. The surface features of these products exhibited acute morphol. changes, as were clearly noticed via SEM studies. Moreover, in the Van Krevelen diagram, it was also obsd. that both the H/C and O/C ratios were dramatically decreased to 0.0019 and 0.0759, and 0.0066 and 0.1659 for coffee waste and empty fruit bunch at 800°C with a (1:3) potassium hydroxide and zinc chloride ratio, resp., and this similar phenomenon was also supported by a thermal gravimetric anal. All these results, together with the specific characteristics of the products, suggest that this scheme can be an effective strategy for the activated carbon prodn. from such residues.
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    Chatir, E. M.; El Hadrami, A.; Ojala, S.; Brahmi, R. Production of activated carbon with tunable porosity and surface chemistry via chemical activation of hydrochar with phosphoric acid under oxidizing atmosphere. Surf. Interfaces 2022, 30, 101849,  DOI: 10.1016/j.surfin.2022.101849
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    Production of activated carbon with tunable porosity and surface chemistry via chemical activation of hydrochar with phosphoric acid under oxidizing atmosphere
    Chatir, El Mehdi; El Hadrami, Abdelouahab; Ojala, Satu; Brahmi, Rachid
    Surfaces and Interfaces (2022), 30 (), 101849CODEN: SIUNCN; ISSN:2468-0230. (Elsevier B.V.)
    This work highlights the chem. activation of hydrothermally carbonized biomass with phosphoric acid under static air as activating atm. Argan nut shells were hydrothermally carbonized, and then chem. activated with phosphoric acid under oxidizing atm. The activated carbons displayed excellent sp. surface areas (from 1200 m2g-1 to 1880 m2g-1) and the material yield were in acceptable level (between 27 and 50%). The varied activation conditions provided a distinctive possibility for creating and controlling the mesoporosity of the activated carbons. At 500°C, a mesoporosity around of 93% could be reached by an H3PO4 impregnation ratio of 4. The activating temp. 500°C and the impregnation ratio of 3 were obsd. as optimum for achieving the best textural properties. The optimized material HC-500-3 exhibited a specific area of 1880 m2g-1, pore vol. and av. pore diam. of 1.36 cm3g-1 and 2.9 nm, as well as good amt. of oxygen functional groups (2.25 mmolg-1) including carboxyl, phenol, and lactone groups. The adsorption performance of optimized material was evaluated using Bisphenol A as a target mol. The adsorption process could be described by Weber Morris and Langmuir isotherm models. At a temp. of 25°C, Langmuir monolayer adsorption capacity was obsd. to be 420 mgg-1 which is comparable or higher than those reported previously. The estd. thermodn. parameters indicate spontaneous and exothermic adsorption process (ΔH° = -19.39 kJmol-1; -5.58 kJmol-1 ≤ ΔG° ≤ -4.65 kJmol-1). The mesoporous activated carbon prepd. by chem. activation of biomass-derived hydrochar under atm. air proved to be very potential adsorbent for Bisphenol A removal.
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    Chen, W.; Gong, M.; Li, K.; Xia, M.; Chen, Z.; Xiao, H.; Fang, Y.; Chen, Y.; Yang, H.; Chen, H. Insight into KOH activation mechanism during biomass pyrolysis: Chemical reactions between O-containing groups and KOH. Appl. Energy 2020, 278, 115730,  DOI: 10.1016/j.apenergy.2020.115730
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    Insight into KOH activation mechanism during biomass pyrolysis: Chemical reactions between O-containing groups and KOH
    Chen, Wei; Gong, Meng; Li, Kaixu; Xia, Mingwei; Chen, Zhiqun; Xiao, Haoyu; Fang, Yang; Chen, Yingquan; Yang, Haiping; Chen, Hanping
    Applied Energy (2020), 278 (), 115730CODEN: APENDX; ISSN:0306-2619. (Elsevier Ltd.)
    In this study, the effects of KOH/biomass ratios (1:8 to 1:1) and temps. (400-800°C) on biomass pyrolysis were investigated. The KOH chem. activation mechanism was explored by revealing the evolution mechanisms of the gaseous product, bio-oil, biochar, and KOH, based on expts. and quantum calcns. Results showed that KOH can react with active O-contg. species in biomass, which was the main reaction at lower ratios (1:8-1:2) or lower temps. (400-600°C). Here, KOH was completely transformed to K2CO3, leading to the formation of large amts. of gaseous products and phenols (reaching 75%). The reaction between KOH and more stable carbon fragments, however, was enhanced at higher ratios (>1:2) or higher temps. (700-800°C), such that it became the main reaction. With a significant decrease in the phenols and O-species, the hydrocarbons became the dominant species (reaching a content of 57.43%). For biochar, the reactions among KOH, O-contg. species, and carbon fragments generated an abundance of vacancies in the biochar. The OH- from KOH rapidly entered these vacancies, forming a large amt. of new O-contg. groups (i.e., C=O, -OH, C-O, O-C=O, and -COOH groups). This also caused an increase in oxygen content (reaching 23.68 wt%) in biochar. At higher temps., the reactions between KOH and biomass were significantly enhanced, along with a sharp increase in the sp. surface area (reaching 1351.13 m2/g).
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    Guo, S.; Chen, Y.; Shi, L.; Dong, Y.; Ma, J.; Chen, X.; Song, H. Nitrogen-doped biomass-based ultra-thin carbon nanosheets with interconnected framework for High-Performance Lithium-Ion Batteries. Appl. Surf. Sci. 2018, 437, 136– 143,  DOI: 10.1016/j.apsusc.2017.12.144
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    Nitrogen-doped biomass-based ultra-thin carbon nanosheets with interconnected framework for High-Performance Lithium-Ion Batteries
    Guo, Shasha; Chen, Yaxin; Shi, Liluo; Dong, Yue; Ma, Jing; Chen, Xiaohong; Song, Huaihe
    Applied Surface Science (2018), 437 (), 136-143CODEN: ASUSEE; ISSN:0169-4332. (Elsevier B.V.)
    In this paper, a low-cost and environmental friendly synthesis strategy is proposed to fabricate nitrogen-doped biomass-based ultra-thin carbon nanosheets (N-CNS) with interconnected framework by using soybean milk as the carbon precursor and sodium chloride as the template. The interconnected porous nanosheet structure is beneficial for lithium ion transportation, and the defects introduced by pyridine nitrogen doping are favorable for lithium storage. When used as the anodes for lithium-ion batteries, the N-CNS electrode shows a high initial reversible specific capacity of 1334 mAh g-1 at 50 mA g-1, excellent rate performance (1212, 555 and 336 mAh g-1 at 0.05, 0.5 and 2 A g-1, resp.) and good cycling stability (355 mAh g-1 at 1 A g-1 after 1000 cycles). Furthermore, this study demonstrates the prospects of biomass and soybean milk, as the potential anode for the application of electrochem. energy storage devices.
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    Bello, A.; Fashedemi, O. O.; Barzegar, F.; Madito, M. J.; Momodu, D. Y.; Masikhwa, T. M.; Dangbegnon, J. K.; Manyala, N. Microwave synthesis: Characterization and electrochemical properties of amorphous activated carbon-MnO2 nanocomposite electrodes. J. Alloys Compd. 2016, 681, 293– 300,  DOI: 10.1016/j.jallcom.2016.04.227
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    Microwave synthesis: Characterization and electrochemical properties of amorphous activated carbon-MnO2 nanocomposite electrodes
    Bello, A.; Fashedemi, O. O.; Barzegar, F.; Madito, M. J.; Momodu, D. Y.; Masikhwa, T. M.; Dangbegnon, J. K.; Manyala, N.
    Journal of Alloys and Compounds (2016), 681 (), 293-300CODEN: JALCEU; ISSN:0925-8388. (Elsevier B.V.)
    The green chem. route (microwave) was used to produce nanocomposite materials based on activated carbon (AC) and manganese (Mn) oxide nanostructures. XRD anal. revealed that amorphous and cryst. oxide structures were synthesized. SEM studies revealed rod-like α-MnO2 for the pristine sample, while cubic Mn3O4 and irregularly shaped MnO2 structures anchored on the AC substrate, with the nanostructures being uniformly distributed on the AC. The electrochem. tests of the composites as electrodes showed that the amorphous AC-MnO2 had a specific capacitance of 180 F g-1, nearly four times higher than that of the cryst. AC-Mn3O4 composite electrode (55 F g-1). The coulombic efficiency for the AC-MnO2 cell was 98% after 5000 cycles, indicating only a small loss of capacitance. The green route technique and good electrochem. properties indicate that the amorphous AC-MnO2 nanocomposite could be a good material for high-capacity, low-cost, and environmentally friendly electrodes for electrochem. capacitors.
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    Neiva, D. M.; Araújo, S.; Gominho, J.; Carneiro, A. d. C.; Pereira, H. An integrated characterization of Picea abies industrial bark regarding chemical composition, thermal properties and polar extracts activity. PLoS One 2018, 13, e0208270  DOI: 10.1371/journal.pone.0208270
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    An integrated characterization of Picea abies industrial bark regarding chemical composition, thermal properties and polar extracts activity
    Neiva, Duarte M.; Araujo, Solange; Gominho, Jorge; Carneiro, Angelica de Cassia; Pereira, Helena
    PLoS One (2018), 13 (11), e0208270/1-e0208270/14CODEN: POLNCL; ISSN:1932-6203. (Public Library of Science)
    Present work dets. chem. and thermal characteristics as well as phytochem. and antioxidant potential of polar extractives of the Picea abies bark from industrial mill, their wood and bark components and also different bark fractions obtained by mech fractionization. Aim is to increase knowledge on Picea abies bark to better det. possible uses other than burning for energy prodn. and to test initial size redn. process to achieve fractions with different characteristics. Compared to wood, bark presented similar lignin higher mineral and extractives and lower polysaccharides contents. Regarding bark fractions the fines showed higher ash , extractives and lignin than the coarse fraction. Phytochem. profile of ethanol and water exts. presented higher contents for bark than wood of total phenols (2x higher), flavonoids (3x higher) and tannins (4-10× higher) with an increasing tendency with particle size. Bark antioxidant activity was higher than that of wood for ferric-reducing antioxidant power and free radical scavenging activity methods. Bark thermal properties showed a much lower volatiles to fixed carbon ratio (V/FC) than wood (3.1 vs 5.2) although the same higher heating value. Bark presented chem. features that point to their possible upgrade, whether by taking advantage of the high extractives with bioactive compds. or the prodn. potential for hemicellulose-derived oligomers with possible use in nutraceutical and pharmaceutical industries.
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    Thyrel, M.; Backman, R.; Boström, D.; Skyllberg, U.; Lestander, T. A. Phase transitions involving Ca – The most abundant ash forming element – In thermal treatment of lignocellulosic biomass. Fuel 2021, 285, 119054,  DOI: 10.1016/j.fuel.2020.119054
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    Phase transitions involving Ca - The most abundant ash forming element - In thermal treatment of lignocellulosic biomass
    Thyrel, Mikael; Backman, Rainer; Bostroem, Dan; Skyllberg, Ulf; Lestander, Torbjoern A.
    Fuel (2021), 285 (), 119054CODEN: FUELAC; ISSN:0016-2361. (Elsevier Ltd.)
    Torrefaction, pyrolysis and gasification are of interest to convert lignocellulosic biomass into fuels and chems. These techniques involve thermal treatment at low partial pressures of oxygen. However, little is known about the transformation of ash elements during these processes. The phase transition of the major ash element calcium (Ca) was therefore studied with powder from pine as biomass model treated at temps. 300-800° under atmospheres of 100% N2, 3% O2 and 6% O2 and thermodn. equil. modeling. For evaluation, x-ray powder diffraction and synchrotron Ca K-edge x-ray absorption near edge structure (XANES) spectroscopy in combination with linear combination fitting and ref. compds. was used. The most abundant Ca-contg. species in the untreated material was thermally unstable Ca oxalate (CaC2O4) primarily decompg. into Ca phases dominated by carbonates at temps. up to 600°. Double carbonates of calcium and potassium were obsd. in the form of fairchildiite/butscheliite (K2Ca(CO3)2), and these phases were stable over the low temp. range studied. Hydroxyapatite (Ca5(PO4)3OH) was expected to be present and thermally stable over the entire temp. interval and was found in untreated material. At temps. above 600° calcium oxide (CaO) was formed. The amt. of oxygen had little effect on the phase transitions. The results of thermodn. modeling were in agreement with XANES showing that this is a versatile technique that can be applied to systems as complex as Ca phase transitions in thermally treated lignocellulosic biomass at low partial pressures of oxygen.
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    Zhu, C.; Chen, J.; Liu, S.; Cheng, B.; Xu, Y.; Zhang, P.; Zhang, Q.; Li, Y.; Zhong, S. Improved electrochemical performance of bagasse and starch-modified LiNi0.5Mn0.3Co0.2O2 materials for lithium-ion batteries. J. Mater. Sci. 2018, 53, 5242– 5254,  DOI: 10.1007/s10853-017-1926-4
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    Improved electrochemical performance of bagasse and starch-modified LiNi0.5Mn0.3Co0.2O2 materials for lithium-ion batteries
    Zhu, Caijian; Chen, Jun; Liu, Shanshan; Cheng, Boming; Xu, Yong; Zhang, Pengwei; Zhang, Qian; Li, Yutao; Zhong, Shengwen
    Journal of Materials Science (2018), 53 (7), 5242-5254CODEN: JMTSAS; ISSN:0022-2461. (Springer)
    Org. C-coated LiNi0.5Mn0.3Co0.2O2 materials are prepd. by mixing 2 or 5% starch or bagasse evenly with the synthesized LiNi0.5Mn0.3Co0.2O2 material and calcining for 10 h at 750°. The microstructures and electrochem. performance are studied by x-ray diffraction, SEM, C/S anal., TEM and electrochem. testing. The org. C coated on the surface of LiNi0.5Mn0.3Co0.2O2 material does not change the surface morphol. and crystal structure, but greatly improves the cond., rate and cycle performance of the LiNi0.5Mn0.3Co0.2O2 cathode in a Li-ion battery. The initial discharge capacity of the synthesized LiNi0.5Mn0.3Co0.2O2 material is 147.8 mAh g-1, which increases to 152.4 and 153.3 mAh g-1 for 2% starch and bagasse, resp. After 100 cycles, the capacity retention rates are 70.7% (uncoated), 83.3% (coated with 2% starch), 90.1% (coated with 2% bagasse), 83.1% (coated with 5% starch) and 91.1% (coated with 5% bagasse). The influence of the percentage of coated C and its dispersion uniformity on the performance of the battery is analyzed. A small coating capacity and uniform C film can achieve better performance. Rational org. C coating technol. is an effective way to improve the electrochem. performance of LiNi1-x-yMnxCoyO2-based material.
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    Meddings, N.; Heinrich, M.; Overney, F.; Lee, J.-S.; Ruiz, V.; Napolitano, E.; Seitz, S.; Hinds, G.; Raccichini, R.; Gaberšček, M.; Park, J. J. Power Sources 2020, 480, 228742,  DOI: 10.1016/j.jpowsour.2020.228742
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    Application of electrochemical impedance spectroscopy to commercial Li-ion cells: A review
    Meddings, Nina; Heinrich, Marco; Overney, Frederic; Lee, Jong-Sook; Ruiz, Vanesa; Napolitano, Emilio; Seitz, Steffen; Hinds, Gareth; Raccichini, Rinaldo; Gaberscek, Miran; Park, Juyeon
    Journal of Power Sources (2020), 480 (), 228742CODEN: JPSODZ; ISSN:0378-7753. (Elsevier B.V.)
    A review. Electrochem. impedance spectroscopy (EIS) is a widely applied non-destructive method of characterization of Li-ion batteries. Despite its ease of application, there are inherent challenges in ensuring the quality and reproducibility of the measurement, as well as reliable interpretation and validation of impedance data. Here, we present a focus review summarizing best metrol. practice in the application of EIS to com. Li-ion cells. State-of-the-art methods of EIS interpretation and validation are also reported and examd. to highlight the benefits and drawbacks of the technique.
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    Subramaniyam, C. M.; Srinivasan, N. R.; Tai, Z.; Liu, H. K.; Goodenough, J. B.; Dou, S. X. Self-assembled porous carbon microparticles derived from halloysite clay as a lithium battery anode. J. Mater. Chem. A 2017, 5, 7345– 7354,  DOI: 10.1039/C7TA00940B
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    Self-assembled porous carbon microparticles derived from halloysite clay as a lithium battery anode
    Subramaniyam, Chandrasekar M.; Srinivasan, N. R.; Tai, Zhixin; Liu, Hua Kun; Goodenough, John B.; Dou, Shi Xue
    Journal of Materials Chemistry A: Materials for Energy and Sustainability (2017), 5 (16), 7345-7354CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
    A naturally available clay mineral, halloysite, is used as a templating agent for the prepn. of porous C microparticles (PCMs); these PCMs were studied as a candidate for Li-ion battery (LIB) anodes. The PCMs are obtained with furfuryl alc. as the C precursor; we also propose a possible mechanism for their self-assembled structure. This structure exhibits a Brunauer-Emmett-Teller surface area of 329 m2/g, which is higher than that of halloysite (50 m2/g). Even after 300 cycles, the PCMs exhibited a stable reversible discharge capacity of 600 mAh/g when tested at 100 mA/g. The presence of porous structure in PCM electrode provides surface controlled reaction, contributing pseudocapacitance (58.5%) to the total charge storage capacity.
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    Choi, C.; Ashby, D. S.; Butts, D. M.; DeBlock, R. H.; Wei, Q.; Lau, J.; Dunn, B. Achieving high energy density and high power density with pseudocapacitive materials. Nature Rev. Mater. 2019, 5, 5– 19,  DOI: 10.1038/s41578-019-0142-z
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    Augustyn, V.; Simon, P.; Dunn, B. Pseudocapacitive oxide materials for high-rate electrochemical energy storage. Energy Environ. Sci. 2014, 7, 1597– 1614,  DOI: 10.1039/c3ee44164d
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    Pseudocapacitive oxide materials for high-rate electrochemical energy storage
    Augustyn, Veronica; Simon, Patrice; Dunn, Bruce
    Energy & Environmental Science (2014), 7 (5), 1597-1614CODEN: EESNBY; ISSN:1754-5706. (Royal Society of Chemistry)
    Electrochem. energy storage technol. is based on devices capable of exhibiting high energy d. (batteries) or high power d. (electrochem. capacitors). There is a growing need, for current and near-future applications, where both high energy and high power densities are required in the same material. Pseudocapacitance, a faradaic process involving surface or near surface redox reactions, offers a means of achieving high energy d. at high charge-discharge rates. Here, we focus on the pseudocapacitive properties of transition metal oxides. First, we introduce pseudocapacitance and describe its electrochem. features. Then, we review the most relevant pseudocapacitive materials in aq. and non-aq. electrolytes. The major challenges for pseudocapacitive materials along with a future outlook are detailed at the end.
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    Surace, Y.; Leanza, D.; Mirolo, M.; Kondracki, Ł.; Vaz, C. A. F.; El Kazzi, M.; Novák, P.; Trabesinger, S. Evidence for stepwise formation of solid electrolyte interphase in a Li-ion battery. Energy Storage Mater. 2022, 44, 156– 167,  DOI: 10.1016/j.ensm.2021.10.013
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    Hong, K.-L.; Qie, L.; Zeng, R.; Yi, Z.-Q.; Zhang, W.; Wang, D.; Yin, W.; Wu, C.; Fan, Q. J.; Zhang, W.-X.; Huang, Y.-H. Biomass derived hard carbon used as a high performance anode material for sodium ion batteries. J. Mater. Chem. A 2014, 2, 12733,  DOI: 10.1039/C4TA02068E
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    Biomass derived hard carbon used as a high performance anode material for sodium ion batteries
    Hong, Kun-lei; Long, Qie; Zeng, Rui; Yi, Zi-qi; Zhang, Wei; Wang, Duo; Yin, Wei; Wu, Chao; Fan, Qing-jie; Zhang, Wu-xing; Huang, Yun-hui
    Journal of Materials Chemistry A: Materials for Energy and Sustainability (2014), 2 (32), 12733-12738CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
    A porous hard carbon material was synthesized by the simple pyrolysis of H3PO4-treated biomass, i.e., pomelo peels, at 700 °C in N2. The as-obtained hard carbon had a 3D connected porous structure and a large sp. surface area of 1272 m2 g-1. XPS anal. showed that the carbon material was functionalized by O-contg. and P-contg. groups. The porous hard carbon was used as an anode for sodium ion batteries and exhibited good cycling stability and rate capability, delivering a capacity of 181 mA h g-1 at 200 mA g-1 after 220 cycles and retaining a capacity of 71 mA h g-1 at 5 A g-1. The sodium storage mechanisms of the porous hard carbon can be explained by Na+ intercalation into the disordered graphene layers, redox reaction of the surface O-contg. functional groups and Na+ storage in the nanoscale pores. However, the porous hard carbon demonstrated a low coulombic efficiency of 27%, resulting from the formation of a solid electrolyte interphase film and the side reactions of surface phosphorus groups.
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    Ghani, U.; Iqbal, N.; Aboalhassan, A. A.; Liu, B.; Aftab, T.; Zada, I.; Ullah, F.; Gu, J.; Li, Y.; Zhu, S.; Liu, Q. One-step sonochemical fabrication of biomass-derived porous hard carbons; towards tuned-surface anodes of sodium-ion batteries. J. Colloid Interface Sci. 2022, 611, 578– 587,  DOI: 10.1016/j.jcis.2021.12.104
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  1. Palanivel Molaiyan, Glaydson Simões Dos Reis, Diwakar Karuppiah, Chandrasekar M. Subramaniyam, Flaviano García-Alvarado, Ulla Lassi. Recent Progress in Biomass-Derived Carbon Materials for Li-Ion and Na-Ion Batteries—A Review. Batteries 2023, 9 (2) , 116. https://doi.org/10.3390/batteries9020116
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  • Abstract

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    Figure 1

    Figure 1. Physiochemical properties of chemically activated Biochar-1 and Biochar-2: (a,b) nitrogen adsorption–desorption isotherms; (c,d) morphological analysis using FESEM depicting the porous structures of the biochars (at 10,000× magnification); (e,f) Raman spectra showing the structural defects and degree of graphitization in the biochars.

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    Figure 2

    Figure 2. Carbon (C 1s), oxygen (O 1s), and nitrogen (N 1s) XPS spectra of (a) Biochar-1 and (b) Biochar-2.

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    Figure 3

    Figure 3. (a) Charge–discharge of Biochar-1 at various cycles, (b) rate test, and (c) long cycle stability of biochars at various current densities.

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    Figure 4

    Figure 4. (a) Electrochemical impedance spectroscopy (EIS) of fresh cells (inset: equivalent electrical circuit); (b) cyclic voltammetry (CV) of biochars; (c) CV at different scan rates of Biochar-1; (d) CV with mapping of the diffusion-controlled mechanism and capacitive effect; (e) contribution of Faradic and capacitive effect in Biochar-1 as a function of scan rates; (f) slope b as a function of each potential during the charge–discharge process. From the plot, we can conclude that as the slope b value is greater than 0.5, the electrochemical kinetics of biochar is limited by the non-diffusive surface capacitive mechanism.

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    Figure 5. (a) Cyclic voltammetry (CV) of Biochar-1, (b) rate tests at different current densities, (c) long cycle stability of biochars at various current densities, and (d) Nyquist electrochemical impedance spectroscopy (EIS) plot of fresh cells and cells after cycling (inset: enlarged at high frequencies).

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      Dehkhoda, Amir Mehdi; Gyenge, Elod; Ellis, Naoko
      Biomass and Bioenergy (2016), 87 (), 107-121CODEN: BMSBEO; ISSN:0961-9534. (Elsevier Ltd.)
      This study reveals a novel method to tailor the micro- and meso-porous structures of activated biochar by exploiting the interaction between pre-carbonization drying conditions and carbonization temp. in KOH activation. Biochar samples were mixed with concd. KOH and then dried under air or nitrogen for various periods of time (0-280 h) followed by carbonization at 475, 675 or 875 °C. It is confirmed that by manipulating drying conditions and carbonization temps., the KOH activated biochar can have a predominantly microporous, mesoporous or a combined (micro/meso) porous structure. The surface area, micropore and mesopore vols. tailored between: 488-2670 m2 g-1, 0.04-0.72 cm3 g-1, and 0.05-1.70 cm3 g-1, resp. The mechanism of porosity development was investigated by FTIR anal. suggesting conversion of KOH to K2CO3 due to different drying conditions as a major role in tailoring the structure. The application of activated biochar with tailored porosity was investigated for Elec. Double Layer adsorption of NaCl/NaOH to be employed in water treatment (capacitive deionization) or energy storage (supercapacitor) processes. The majorly microporous activated biochar (N2-dried activated at 675 °C) showed promising capacitances between 220 and 245 F g-1. Addn. of mesoporous structure resulted in capacitances between 182 and 240 F g-1 with significantly reduced electrode resistance and improved capacitive behavior as evidenced by Impedance Spectroscopy and Galvanostatic Charge/Discharge tests.
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    12. 12
      Yu, K.; Wang, J.; Song, K.; Wang, X.; Liang, C.; Dou, Y. Hydrothermal synthesis of cellulose-derived carbon nanospheres from corn straw as anode materials for lithium-ion batteries. Nanomaterials 2019, 9, 93,  DOI: 10.3390/nano9010093
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      12
      Hydrothermal synthesis of cellulose-derived carbon nanospheres from corn straw as anode materials for lithium ion batteries
      Yu, Kaifeng; Wang, Jingjing; Song, Kexian; Wang, Xiaofeng; Liang, Ce; Dou, Yanli
      Nanomaterials (2019), 9 (1), 93/1-93/13CODEN: NANOKO; ISSN:2079-4991. (MDPI AG)
      As a most attractive renewable resource, biomass has the advantages of low pollution, wide distribution and abundant resources, promoting its applications in lithium ion batteries (LIBs). Herein, cellulose-derived carbon nanospheres (CCS) were successfully synthesized by hydrothermal carbonization (HTC) from corn straw for use as an anode in LIBs. The uniform distribution and cross-linked structure of carbon nanospheres were obtained by carefully controlling reaction time, which could not only decrease the transport pathway of lithium ions, but also reduce the structural damage caused by the intercalation of lithium ions. Esp., obtained after hydrothermal carbonization for 36 h, those typical characteristics make it deliver excellent cycling stability as well as the notable specific capacity of 577 mA h g-1 after 100 cycles at 0.2C. Hence, this efficient and environment-friendly method for the fabrication of CCS from corn straw could realize the secondary utilization of biomass waste, as well as serve as a new choice for LIBs anode materials.
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    13. 13
      Guan, Z.; Guan, Z.; Li, Z.; Liu, J.; Yu, K. Characterization and preparation of nano-porous carbon derived from hemp stems as anode for lithium-ion batteries. Nanoscale Res. Lett. 2019, 14, 338,  DOI: 10.1186/s11671-019-3161-1
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      13
      Characterization and Preparation of Nano-porous Carbon Derived from Hemp Stems as Anode for Lithium-Ion Batteries
      Guan Zhongxiang; Guan Zhiping; Li Zhigang; Liu Junhui; Yu Kaifeng; Guan Zhiping; Li Zhigang; Yu Kaifeng
      Nanoscale research letters (2019), 14 (1), 338 ISSN:1931-7573.
      As a biomass waste, hemp stems have the advantages of low cost and abundance, and it is regarded as a promising anode material with a high specific capacity. In this paper, activated carbon derived from hemp stems is prepared by low-temperature carbonization and high-temperature activation. The results of characterizations show the activated carbon has more pores due to the advantages of natural porous structure of hemp stem. The aperture size is mainly microporous, and there are mesopores and macropores in the porous carbon. The porous carbon has an excellent reversible capacity of 495 mAh/g after 100 cycles at 0.2 °C as the anode of lithium-ion battery. Compared with the graphite electrode, the electrochemical property of activated carbon is significantly improved due to the reasonable distribution of pore size. The preparation of the activated carbon provides a new idea for low cost and rapid preparation of anode materials for high capacity lithium-ion batteries.
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    14. 14
      Zhu, Y.-E.; Gu, H.; Chen, Y.-N.; Yang, D.; Wei, J.; Zhou, Z. Hard carbon derived from corn straw piths as anode materials for sodium ion batteries. Ionics (Kiel) 2018, 24, 1075– 1081,  DOI: 10.1007/s11581-017-2260-1
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      Tyagi, A.; Banerjee, S.; Singh, S.; Kar, K. K. Biowaste derived activated carbon electrocatalyst for oxygen reduction reaction: Effect of chemical activation. Int. J. Hydrogen Energy 2020, 45, 16930– 16943,  DOI: 10.1016/j.ijhydene.2019.06.195
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      15
      Biowaste derived activated carbon electrocatalyst for oxygen reduction reaction: Effect of chemical activation
      Tyagi, Alekha; Banerjee, Soma; Singh, Shashank; Kar, Kamal K.
      International Journal of Hydrogen Energy (2020), 45 (34), 16930-16943CODEN: IJHEDX; ISSN:0360-3199. (Elsevier Ltd.)
      Conversion of bio-wastes to useful doped carbon materials for various energy applications is emerging as a cost-effective strategy. A novel activated carbon electrocatalyst derived from chicken feather rachis (RCF), a poultry industry bio-waste is explored for oxygen redn. reaction (ORR) catalysis. The rachis is the central stem from which the fibrous ramus is completely removed and it is more cryst. compared to feather ramus. Nitrogen doped activated carbon (CNAx) electrocatalyst is prepd. by chem. activation coupled pyrolysis. The chem. activators used include potassium hydroxide (KOH), phosphoric acid (H3PO4) and zinc chloride (ZnCl2) followed by pyrolysis at 500, 700 and 900°C. Electrochem. performance has been evaluated using cyclic voltammetry (CV) and linear sweep voltammetry (LSV) using a rotating disk electrode (RDE). KOH activated electrocatalyst exhibits remarkable improvement in surface area favoring improved onset potential (-0.02 V vs Ag/AgCl). This increased activity is due to increase in no. of well-exposed ORR active sites on activation. The effect of chem. activators on the structure and morphol. of the activated carbons are discussed using Raman spectroscopy, adsorption-desorption isotherm study, electron microscopic techniques, at. force microscopy (AFM), and XPS studies. KOH activated CNAx-900 exhibits best combination of properties and confirms its feasibility to be a suitable electrocatalyst for PEMFC. Hence, RCF derived electrocatalysts are propitious alternates for ORR catalysis.
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    16. 16
      Zhang, Y.; Chen, L.; Meng, Y.; Xie, J.; Guo, Y.; Xiao, D. Lithium and sodium storage in highly ordered mesoporous nitrogen-doped carbons derived from honey. J. Power Sources 2016, 335, 20– 30,  DOI: 10.1016/j.jpowsour.2016.08.096
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      16
      Lithium and sodium storage in highly ordered mesoporous nitrogen-doped carbons derived from honey
      Zhang, Yongzhi; Chen, Li; Meng, Yan; Xie, Jun; Guo, Yong; Xiao, Dan
      Journal of Power Sources (2016), 335 (), 20-30CODEN: JPSODZ; ISSN:0378-7753. (Elsevier B.V.)
      Honey, a widely existent biomass, consists mainly of carbohydrate and other N-contg. substances such as proteins, enzymes and org. acids. It can be mixed homogeneously with mesoporous SiO2 template for its excellent H2O-soly. and moderate viscosity. Honey was employed as a N-contg. C precursor to prep. N-doped ordered mesoporous carbons (OMCs). The obtained honey derived mesoporous N-doped carbons (HMNCs) with dilated interlayer spacings of 0.387-0.395 nm, narrow pore size distributions centering at ∼4 nm and satisfactory N contents of 1.38-4.32% offer superb dual functionality for Li-ion battery (LIB) and Na-ion battery (NIB) anodes. Tested against Li, the optimized HMNC-700 delivers a superior reversible capacity of 1359 mA h g-1 after 10 cycles at 100 mA g-1 and excellent rate capability and cycling stability of 722 mA h g-1 after 200 cycles at 1 A g-1. For NIB applications, HMNC-700 offers a high initial reversible capacity of 427 mA h g-1 and stable reversible capacity of 394 mA h g-1 at 100 mA g-1.
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    17. 17
      Léonard, A. F.; Castro-Muñiz, A.; Suárez-García, F.; Job, N.; Paredes, J. I. Understanding the effect of the mesopore volume of ordered mesoporous carbons on their electrochemical behavior as Li-ion battery anodes. Microporous Mesoporous Mater. 2020, 306, 110417,  DOI: 10.1016/j.micromeso.2020.110417
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      17
      Understanding the effect of the mesopore volume of ordered mesoporous carbons on their electrochemical behavior as Li-ion battery anodes
      Leonard, Alexandre F.; Castro-Muniz, Alberto; Suarez-Garcia, Fabian; Job, Nathalie; Paredes, Juan I.
      Microporous and Mesoporous Materials (2020), 306 (), 110417CODEN: MIMMFJ; ISSN:1387-1811. (Elsevier B.V.)
      This work aims at understanding the effect of the mesopore vol. of ordered mesoporous carbons (OMCs) on their behavior as anodes for Li-ion batteries. To that purpose, the hard-templating method was used as an enabling tool, with the controlled partial etching of the silica template to prep. a series of OMCs with a wide range of mesopore vols. The formed carbon-silica hybrids were processed into electrodes using a water-based ink prepn. route in the presence of xanthan gum as a binder, which retained access to the pores after formation of the electrodes. The pore texture of the latter was compared to that of the starting powders. A very good linear relationship could be evidenced between the mesopore vol. of the electrodes and the first insertion capacity of Li-ions. The lithium de-insertion also followed a linear trend, but its behavior was dependent on the final applied potential. Indeed, the higher the mesopore vol., the higher the contribution of de-insertion at elevated voltages. This study further points out the importance of the textural characterization of electrodes (instead of just the starting material) as well as the conditions at which the electrochem. measurements are carried out, esp. the max. applied de-insertion voltage.
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    18. 18
      dos Reis, G. S.; Larsson, S. H.; Thyrel, M.; Pham, T. N.; Claudio Lima, E.; de Oliveira, H. P.; Dotto, G. L. Preparation and Application of Efficient Biobased Carbon Adsorbents Prepared from Spruce Bark Residues for Efficient Removal of Reactive Dyes and Colors from Synthetic Effluents. Coatings 2021, 11, 772,  DOI: 10.3390/coatings11070772
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      18
      Preparation and Application of Efficient Biobased Carbon Adsorbents Prepared from Spruce Bark Residues for Efficient Removal of Reactive Dyes and Colors from Synthetic Effluents
      dos Reis, Glaydson Simoes; Larsson, Sylvia H.; Thyrel, Mikael; Pham, Tung Ngoc; Claudio Lima, Eder; de Oliveira, Helinando Pequeno; Dotto, Guilherme L.
      Coatings (2021), 11 (7), 772CODEN: COATED; ISSN:2079-6412. (MDPI AG)
      Biobased carbon materials (BBC) obtained from Norway spruce (Picea abies Karst.) bark was produced by single-step chem. activation with ZnCl2 or KOH, and pyrolysis at 800°C for one hour. The chem. activation reagent had a significant impact on the properties of the BBCs. KOH-biobased carbon material (KOH-BBC) had a higher sp. surface area (SBET), equal to 1067 m2 g-1, larger pore vol. (0.558 cm3 g-1), more mesopores, and a more hydrophilic surface than ZnCl2-BBC. However, the carbon yield for KOH-BBC was 63‰ lower than for ZnCl2-BBC. Batch adsorption expts. were performed to evaluate the ability of the two BBCs to remove two dyes, reactive orange 16 (RO-16) and reactive blue 4 (RB-4), and treat synthetic effluents. The general order model was most suitable for modeling the adsorption kinetics of both dyes and BBCs. The equil. parameters at 22°C were calcd. using the Liu model. Upon adsorption of RO-16, Qmax was 90.1 mg g-1 for ZnCl2-BBC and 354.8 mg g-1 for KOH-BBC. With RB-4, Qmax was 332.9 mg g-1 for ZnCl2-BBC and 582.5 mg g-1 for KOH-BBC. Based on characterization and exptl. data, it was suggested that electrostatic interactions and hydrogen bonds between BBCs and RO-16 and RB-4 dyes played the most crucial role in the adsorption process. The biobased carbon materials showed high efficiency for removing RO-16 and RB-4, comparable to the best examples from the literature. Addnl., both the KOH- and ZnCl2-BBC showed a high ability to purify two synthetic effluents, but the KOH-BBC was superior.
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    19. 19
      Lima, D. R.; Lima, E. C.; Thue, P. S.; Dias, S. L. P.; Machado, F. M.; Seliem, M. K.; Sherf, F.; dos Reis, G. S.; Saeb, M. R.; Rinklebe, J. Comparison of acidic leaching using a conventional and ultrasound-assisted method for preparation of magnetic-activated biochar. J. Environ. Chem. Eng. 2021, 9, 105865,  DOI: 10.1016/j.jece.2021.105865
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      19
      Comparison of acidic leaching using a conventional and ultrasound-assisted method for preparation of magnetic-activated biochar
      Lima, Diana R.; Lima, Eder C.; Thue, Pascal S.; Dias, Silvio L. P.; Machado, Fernando M.; Seliem, Moaaz K.; Sher, Farooq; dos Reis, Glaydson S.; Saeb, Mohammad Reza; Rinklebe, Jorg
      Journal of Environmental Chemical Engineering (2021), 9 (5), 105865CODEN: JECEBG; ISSN:2213-3437. (Elsevier Ltd.)
      Four magnetic biochars (MBs) were prepd. from two mixts. of Sappeli sawdust with NiCl2 soln. or Sappeli sawdust with NiCl2 plus ZnCl2 solns. These mixts. formed two pastes that were dried and further pyrolyzed at 700 °C under nitrogen flow. The pyrolyzed material was leached out with 0.1 M HCl under conventional reflux (AL- 80 °C, 2 h) or assisted by ultrasound-leaching (US- 15 min, 600 W), obtaining four biochars: SNiAL, SNiUS, SNiZnAL, SNiZnUS. The biochars were characterized by VSM, XRD, FTIR, isotherms of adsorption and desorption of nitrogen, pHpzc, hydrophobically characteristics (HI), TGA, elemental anal. (CHN/O). The data show that using the leaching process assisted by ultrasound can obtain biochars that present good magnetization satn., with a lower leaching time than conventional leaching. The four biochar were tested as adsorbents to remove ten emerging contaminants and four dyes of aq. effluents. It was obsd. that the impregnation of zinc chloride in the samples led to an increase in the surface areas of the magnetic biochars, which influenced the most of sorption capacities of the adsorbents for the different sorbing species. Making a ratio of sorption capacities of SNiAL/SNiZnAL and SNiUS/SNiZnUS, it was obtained the values, resp., of 0.9761, and 0.9710 (Acid Red 1), 2.057, and 3.030 (Reactive Blue 4), 4.192, and 1.971 (Basic Violet 3), 3.359, and 1.129 (Basic Green 1), 1.673, and 1.835 (Paracetamol), 3.612, and 3.779 (Propranolol), 5.871, and 5.171 (Sodium Diclofenac), 1.457, and 1.607 (Nicotinamide), 1.094 and 1.093 (Caffeine), 1.167, and 2.398 (4-chloroaniline), 1.009 and 0.9965 (2-nitrophenol), 1.156 and 1.341 (Resorcinol), 1.299 and 1.331 (Hydroquinone), 0.9975 and 1.019 (4-bromophenol).
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    20. 20
      Moralı, U.; Demiral, H.; Şensöz, S. Optimization of activated carbon production from sunflower seed extracted meal: Taguchi design of experiment approach and analysis of variance. J. Cleaner Prod. 2018, 189, 602– 611,  DOI: 10.1016/j.jclepro.2018.04.084
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      20
      Optimization of activated carbon production from sunflower seed extracted meal: Taguchi design of experiment approach and analysis of variance
      Morali, Ugur; Demiral, Hakan; Sensoz, Sevgi
      Journal of Cleaner Production (2018), 189 (), 602-611CODEN: JCROE8; ISSN:0959-6526. (Elsevier Ltd.)
      Taguchi method has been applied to design optimal activation conditions in the prodn. of activated carbon with high sp. surface area using sunflower seed extd. meal through chem. activation using either zinc chloride or phosphoric acid. The activation temp. and the impregnation ratio were selected as the factors of the activation process to be optimized. The activated carbons were prepd. according to the L9 orthogonal array. Brunauer-Emmett-Teller surface area of the activated carbons was calcd. by using nitrogen adsorption data obtained at -196° C. The optimum level of the activation temp. for prepg. the activated carbon with a high surface area was 600° C for both chem. agents. The optimal levels of the impregnation ratio for a high sp. surface area were detd. as 3:1 and 2:1 for zinc chloride and phosphoric acid, resp. The results of this study showed that the activation temp. is the most significant factor to get activated carbons with higher sp. surface area. Taguchi method also allows a more detailed and accurate assessment to prep. the activated carbon in a cleaner way.
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    21. 21
      Thue, P. S.; Umpierres, C. S.; Lima, E. C.; Lima, D. R.; Machado, F. M.; dos Reis, G. S.; da Silva, R. S.; Pavan, F. A.; Tran, H. N. Single-step pyrolysis for producing magnetic activated carbon from tucumã (Astrocaryum aculeatum) seed and nickel(II) chloride and zinc(II) chloride. Application for removal of Nicotinamide and Propanolol. J. Hazard. Mater. 2020, 398, 122903,  DOI: 10.1016/j.jhazmat.2020.122903
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      21
      Single-step pyrolysis producing magnetic activated carbon from tucuma~ (Astrocaryum aculeatum) seed and nickel(II) chloride and zinc(II) chloride for removal of nicotinamide and propanolol
      Thue, Pascal S.; Umpierres, Cibele S.; Lima, Eder C.; Lima, Diana R.; Machado, Fernando M.; dos Reis, Glaydson S.; da Silva, Raphaelle S.; Pavan, Flavio A.; Tran, Hai Nguyen
      Journal of Hazardous Materials (2020), 398 (), 122903CODEN: JHMAD9; ISSN:0304-3894. (Elsevier B.V.)
      The present research describes the synthesis of new nanomagnetic activated carbon material with high magnetization, and high surface area prepd. in a single pyrolysis step that is used for the carbonization, activation, and magnetization of the produced material. The pyrolysis step of tucuma~ seed was carried out in a conventional tubular oven at 600°C under N2-flow. It was prepd. three magnetic carbons MT-1.5, MT-2.0, MT-2.5, that corresponds to the proportion of biomass: ZnCl2 always 1:1 and varying the proportion of NiCl2 of 1.5, 2.0, and 2.5, resp. These magnetic nanocomposites were characterized by Vibrating Sample Magnetometer (VSM), X-ray diffraction, SEM, thermogravimetric anal., hydrophobic/hydrophilic balance, CHN/O elemental anal., modified Boehm titrn., N2 adsorption-desorption isotherms; and pHpzc. All the materials obtained presented Ni particles with an av. crystallite size of less than 33 nm. The MT-2.0 was employed for the removal of nicotinamide and propranolol from aq. solns. Based on Liu isotherm, the Qmax was 199.3 and 335.4 mg g-1 for nicotinamide and propranolol, resp. MT-2.0 was used to treat simulated pharmaceutical industry effluents attaining removal of all org. compds. attaining up to 99.1% of removal.
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    22. 22
      Liu, Z.; Yuan, X.; Zhang, S.; Wang, J.; Huang, Q.; Yu, N.; Zhu, Y.; Fu, L.; Wang, F.; Chen, Y.; Wu, Y. Three-dimensional ordered porous electrode materials for electrochemical energy storage. NPG Asia Mater. 2019, 11, 12,  DOI: 10.1038/s41427-019-0112-3
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      Three-dimensional ordered porous electrode materials for electrochemical energy storage
      Liu, Zaichun; Yuan, Xinhai; Zhang, Shuaishuai; Wang, Jing; Huang, Qinghong; Yu, Nengfei; Zhu, Yusong; Fu, Lijun; Wang, Faxing; Chen, Yuhui; Wu, Yuping
      NPG Asia Materials (2019), 11 (1), 12CODEN: NAMPCE; ISSN:1884-4057. (Nature Research)
      A review. The past decade has witnessed substantial advances in the synthesis of various electrode materials with three-dimensional (3D) ordered macroporous or mesoporous structures (the so-called "inverse opals") for applications in electrochem. energy storage devices. This review summarizes recent advancements in 3D ordered porous (3DOP) electrode materials and their unusual electrochem. properties endowed by their intrinsic and geometric structures. The 3DOP electrode materials discussed here mainly include carbon materials, transition metal oxides (such as TiO2, SnO2, Co3O4, NiO, Fe2O3, V2O5, Cu2O, MnO2, and GeO2), transition metal dichalcogenides (such as MoS2 and WS2), elementary substances (such as Si, Ge, and Au), intercalation compds. (such as Li4Ti5O12, LiCoO2, LiMn2O4, LiFePO4), and conductive polymers (polypyrrole and polyaniline). Representative applications of these materials in Li ion batteries, aq. rechargeable lithium batteries, Li-S batteries, Li-O2 batteries, and supercapacitors are presented. Addnl., we discuss research opportunities as well as the current challenges to facilitate further contributions to this emerging research frontier.
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    23. 23
      Chu, K.; Zhang, X.; Yang, Y.; Li, Z.; Wei, L.; Yao, G.; Zheng, F.; Chen, Q. Edge-nitrogen enriched carbon nanosheets for potassium-ion battery anodes with an ultrastable cycling stability. Carbon 2021, 184, 277– 286,  DOI: 10.1016/j.carbon.2021.08.015
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      23
      Edge-nitrogen enriched carbon nanosheets for potassium-ion battery anodes with an ultrastable cycling stability
      Chu, Kainian; Zhang, Xiaojuan; Yang, Yang; Li, Zhiqiang; Wei, Lingzhi; Yao, Ge; Zheng, Fangcai; Chen, Qianwang
      Carbon (2021), 184 (), 277-286CODEN: CRBNAH; ISSN:0008-6223. (Elsevier Ltd.)
      Edge-nitrogen (pyridinic/pyrrolic nitrogen) doped carbon materials have been considered as promising anodes for potassium ion batteries (KIBs), which can provide a high surface-induced capacitive capacity beyond the K+-intercalated mechanism. However, achieving a high-level edge-nitrogen doping is still a great challenge owning to inevitable introduction of graphitic nitrogen into carbon materials via conventional pyrolysis process. Herein, we design porous carbon nanosheets with bundant defects and edge sites to graft nitrogen atoms to achieve a high-level edge-nitrogen doping (88.36%). The optimized edge-nitrogen doped carbon nanosheets (ENCNs-600) exhibits a high reversible capacity of 443 mAh g-1 at 0.1 A g-1 after 200 cycles, excellent rate performance (175 mAh g-1 at 20 A g-1), and ultrastable cycling stability (246 mAh g-1 at 5 A g-1 over 10,000 cycles). D. functional theory calcns. and kinetic studies confirm that both edge-nitrogen doping and explanded interlayer distance are greatly conducive for the adsorption and diffusion of K+, thereby ensuring enhanced potassium-storage performance with a synergistic adsorption-intercalation mechanism.
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    24. 24
      Xu, Y.; Sun, X.; Li, Z.; Wei, L.; Yao, G.; Niu, H.; Yang, Y.; Zheng, F.; Chen, Q. Boosting the K+ −adsorption capacity in edgenitrogen doped hierarchically porous carbon spheres for ultrastable potassium ion battery anodes. Nanoscale 2021, 13, 19634– 19641,  DOI: 10.1039/D1NR06665J
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      24
      Boosting the K+-adsorption capacity in edge-nitrogen doped hierarchically porous carbon spheres for ultrastable potassium ion battery anodes
      Xu, Yang; Sun, Xinpeng; Li, Zhiqiang; Wei, Lingzhi; Yao, Ge; Niu, Heling; Yang, Yang; Zheng, Fangcai; Chen, Qianwang
      Nanoscale (2021), 13 (46), 19634-19641CODEN: NANOHL; ISSN:2040-3372. (Royal Society of Chemistry)
      Although carbon materials have great potential for potassium ion battery (KIB) anodes due to their structural stability and abundant carbon-contg. resources, the limited K+-intercalated capacity impedes their extensive applications in energy storage devices. Current research studies focus on improving the surface-induced capacitive behavior to boost the potassium storage capacity of carbon materials. Herein, we designed edge-nitrogen (pyridinic-N and pyrrolic-N) doped carbon spheres with a hierarchically porous structure to achieve high potassium storage properties. The electrochem. tests confirmed that the edge-nitrogen induced active sites were conducive for the adsorption of K+, and the hierarchical porous structure promoted the generation of stable solid electrolyte interphase (SEI) films, both of which endow the resulting materials with a high reversible capacity of 381.7 mA h g-1 at 0.1 A g-1 over 200 cycles and an excellent rate capability of 178.2 mA h g-1 at 5 A g-1. Even at 5 A g-1, the long-term cycling stability of 5000 cycles was achieved with a reversible capacity of 190.1 mA h g-1. This work contributes to deeply understand the role of the synergistic effect of edge-nitrogen induced active sites and the hierarchical porous structure in the potassium storage performances of carbon materials.
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    25. 25
      Niu, P.; Yang, Y.; Li, Z.; Ding, G.; Wei, L.; Yao, G.; Niu, H.; Min, Y.; Zheng, F.; Chen, Q. Rational design of a hollow porous structure for enhancing diffusion kinetics of K ions in edge-nitrogen doped carbon nanorods. Nano Res. 2022, 15, 8109– 8117,  DOI: 10.1007/s12274-022-4496-y
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      25
      Rational design of a hollow porous structure for enhancing diffusion kinetics of K ions in edge-nitrogen doped carbon nanorods
      Niu, Ping; Yang, Yang; Li, Zhiqiang; Ding, Gaohui; Wei, Lingzhi; Yao, Ge; Niu, Helin; Min, Yulin; Zheng, Fangcai; Chen, Qianwang
      Nano Research (2022), 15 (9), 8109-8117CODEN: NRAEB5; ISSN:1998-0000. (Springer GmbH)
      The high elec. cond. makes it possible for one-dimensional (1D) carbon materials to be used as the promising anodes for potassium ion batteries (PIBs), however, the sluggish diffusion kinetics caused by large-sized potassium ions (K+) limits their practical applications in energy storage systems. In this work, hollow carbon nanorods were rationally designed as a case to verify the superiority of 1D hollow structure to improve the diffusion kinetics of K+. Simultaneously, edge-N (pyridinic-N and pyrrolic-N) atoms were also introduced into 1D hollow carbon structure, which can provide ample active sites and defects in graphitic lattices to adsorb K+, providing extra capacitive storage capacity. As expected, the optimized edge-N doped hollow carbon nanorods (ENHCRs) exhibits a high reversible capacity of 544 mAh·g-1v at 0.1 A·g-1 after 200 cycles. Even at 5 A·g-1, it displays a long-term cycling stability with 255 mAh·g-1 over 10,000 cycles. The electrochem. measurements confirm that the hollow structure is favorable to improve the transfer kinetics of K+ during cycling. And the theor. calcns. demonstrate that edge-N doping can enhance the local electronegativity of graphitic lattices to adsorb much more K+, where edge-N doping synergizes with 1D hollow structure to achieve enhanced K+-storage performances.
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    26. 26
      dos Reis, G. S.; Guy, M.; Mathieu, M.; Jebrane, M.; Lima, E. C.; Thyrel, M.; Dotto, G. L.; Larsson, S. H. A comparative study of chemical treatment by MgCl2, ZnSO4, ZnCl2, and KOH on physicochemical properties and acetaminophen adsorption performance of biobased porous materials from tree bark residues. Colloids Surf., A 2022, 642, 128626,  DOI: 10.1016/j.colsurfa.2022.128626
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      26
      A comparative study of chemical treatment by MgCl2, ZnSO4, ZnCl2, and KOH on physicochemical properties and acetaminophen adsorption performance of biobased porous materials from tree bark residues
      dos Reis, Glaydson S.; Guy, Marine; Mathieu, Manon; Jebrane, Mohamed; Lima, Eder C.; Thyrel, Mikael; Dotto, Guilherme L.; Larsson, Sylvia H.
      Colloids and Surfaces, A: Physicochemical and Engineering Aspects (2022), 642 (), 128626CODEN: CPEAEH; ISSN:0927-7757. (Elsevier B.V.)
      Prepg. sustainable and highly efficient biomass-based carbon materials (BBPM) as adsorbents remains a challenge for org. pollutant management. In this work, novel biobased carbon material has been synthesized via facile, sustainable, and different single-step pyrolysis chem. methods (KOH, ZnCl2, ZnSO4, and MgCl2) using a Norway spruce bark as suitable and efficient carbon precursor. The effects of each chem. activator on the physicochem. structure of synthesized were thoroughly investigated as well as its performance on the acetaminophen adsorption. The results showed that the use of different chem. activation provoked remarkable differences in the BBPM physicochem. characteristics. The KOH activation generated material with the highest sp. surface area (2209 m2 g-1), followed by ZnCl2 (1019 m2 g-1), ZnSO4 (446 m2 g-1), and MgCl2 (98 m2 g-1). The chem. characterization of the carbon materials indicated that the activation of MgCl2 yielded a material around three times more hydrophobic when compared with the other activation methods. The acetaminophen removal showed to be ultrafast, not only due to the BBPM's microstructure but also to the abundant active sites provided by the different chem. activation methods. The adsorption equil. times were reached at 1 min for BBPM-KOH and BBPM-MgCl2 and 15 min for BBPM-ZnSO4 and BBPM-ZnCl2. The adsorption process suggests that the pore-filling mechanism mainly dominates the acetaminophen removal but also some phys.-chem. interactions such as hydrogen bonding between the amide group of acetaminophen and oxygenated or nitrogenated groups of biochar, π-π interactions between the arom. ring of the pharmaceutical and the aroms. of biochar, n-π interaction, van der Waals interactions. The BBPM regeneration studies showed very good cyclability; in the 3rd cycle, the removal was approx. 70% for all four samples. The samples were also used to treat two synthetic effluents, which attained a removal percentage up to 91.9%.
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    27. 27
      Guy, M.; Mathieu, M.; Anastopoulos, I. P.; Martínez, M. G.; Rousseau, F.; Dotto, G. L.; de Oliveira, H. P.; Lima, E. C.; Thyrel, M.; Larsson, S. H.; dos Reis, G. S. Process Parameters Optimization, Characterization, and Application of KOH-Activated Norway Spruce Bark Graphitic Biochars for Efficient Azo Dye Adsorption. Molecules 2022, 27, 456,  DOI: 10.3390/molecules27020456
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      27
      Process Parameters Optimization, Characterization, and Application of KOH-Activated Norway Spruce Bark Graphitic Biochars for Efficient Azo Dye Adsorption
      Guy, Marine; Mathieu, Manon; Anastopoulos, Ioannis P.; Martinez, Maria G.; Rousseau, Frederic; Dotto, Guilherme L.; de Oliveira, Helinando P.; Lima, Eder C.; Thyrel, Mikael; Larsson, Sylvia H.; dos Reis, Glaydson S.
      Molecules (2022), 27 (2), 456CODEN: MOLEFW; ISSN:1420-3049. (MDPI AG)
      In this work, Norway spruce bark was used as a precursor to prep. activated biochars (BCs) via chem. activation with potassium hydroxide (KOH) as a chem. activator. A Box-Behnken design (BBD) was conducted to evaluate and identify the optimal conditions to reach high sp. surface area and high mass yield of BC samples. The studied BC prepn. parameters and their levels were as follows: pyrolysis temp. (700, 800, and 900°C), holding time (1, 2, and 3 h), and ratio of the biomass: chem. activator of 1: 1, 1.5, and 2. The planned BBD yielded BC with extremely high SSA values, up to 2209 m2·g-1. In addn., the BCs were physiochem. characterized, and the results indicated that the BCs exhibited disordered carbon structures and presented a high quantity of O-bearing functional groups on their surfaces, which might improve their adsorption performance towards org. pollutant removal. The BC with the highest SSA value was then employed as an adsorbent to remove Evans blue dye (EB) and colorful effluents. The kinetic study followed a general-order (GO) model, as the most suitable model to describe the exptl. data, while the Redlich-Peterson model fitted the equil. data better. The EB adsorption capacity was 396.1 mg·g-1. The employment of the BC in the treatment of synthetic effluents, with several dyes and other org. and inorg. compds., returned a high percentage of removal degree up to 87.7%. Desorption and cyclability tests showed that the biochar can be efficiently regenerated, maintaining an adsorption capacity of 75% after 4 adsorption-desorption cycles. The results of this work pointed out that Norway spruce bark indeed is a promising precursor for producing biochars with very promising properties.
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    28. 28
      Li, Y.; Li, S.; Wang, Y.; Wang, J.; Liu, H.; Liu, X.; Wang, L.; Liu, X.; Xue, W.; Ma, N. Electrochemical synthesis of phosphorus-doped graphene quantum dots for free radical scavenging. Phys. Chem. Chem. Phys. 2017, 19, 11631,  DOI: 10.1039/C6CP06377B
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      28
      Electrochemical synthesis of phosphorus-doped graphene quantum dots for free radical scavenging
      Li, Yan; Li, Sen; Wang, Yingmin; Wang, Jun; Liu, Hui; Liu, Xinqian; Wang, Lifeng; Liu, Xiaoguang; Xue, Wendong; Ma, Ning
      Physical Chemistry Chemical Physics (2017), 19 (18), 11631-11638CODEN: PPCPFQ; ISSN:1463-9076. (Royal Society of Chemistry)
      P-doped graphene quantum dots (P-GQDs) with a high P doping content (>7 at.%) are synthesized via an electrochem. approach. Na phytate (C6H6Na12O24P6), a green food antioxidant additive, is used as the electrolyte for providing both a P source and an electrolysis environment. The obtained P-GQDs exhibit excellent scavenging activity of free radicals, such as hydroxyl radicals (̇ OH) and 2,2-diphenyl-1-picrylhydrazyl (DPPH). Combined with Raman, FTIR, and XPS spectral analyses, the reason for high P content and the mechanism of free radical scavenging of P-GQDs are studied.
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    29. 29
      Yuan, C.; Chen, M.; Zhu, K.; Ni, J.; Wang, S.; Cao, B.; Zhong, S.; Zhou, J.; Wang, S. Facile synthesis of nitrogen-doped interconnected porous carbons derived from reed and chlorella for high-performance supercapacitors. Fuel Process. Technol. 2022, 238, 107466,  DOI: 10.1016/j.fuproc.2022.107466
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      29
      Facile synthesis of nitrogen-doped interconnected porous carbons derived from reed and chlorella for high-performance supercapacitors
      Yuan, Chuan; Chen, Mao; Zhu, Kai; Ni, Jun; Wang, Shuang; Cao, Bin; Zhong, Shan; Zhou, Jingsong; Wang, Shurong
      Fuel Processing Technology (2022), 238 (), 107466CODEN: FPTEDY; ISSN:0378-3820. (Elsevier Ltd.)
      Three-dimensionally (3D) nitrogen (N)-doped interconnected porous carbons (IPC) derived from cost-effective biomasses were facilely prepd. by one-step method and utilized as electrochem. double layer capacitor (EDLC) electrodes. The reed and chlorella derived interconnected porous carbons (denoted as IPC-R and IPC-C) through carbonization with chem. activation both exhibited typical capacitive behaviors; importantly, by introducing N-rich chlorella into N-free reed by interactive-carbonization, the resultant N-doped interconnected porous carbons (IPC-RC) pos. demonstrated a high N content, a large sp. surface area and pore vol. as well as a high graphitization, which are crucial for fast ion diffusion and thus enhancing the electrochem. properties of supercapacitor. In the three-electrode system, the IPC-RC1.2 showed a superb specific capacitance of 340.4 F/g at a c.d. of 1 A/g, one of the highest capacitances for biomass derived-carbon electrodes reported so far. Even at 20 A/g, the capacitance could achieve 265.5 F/g, revealing the superb rate capability. In the sym. two-electrode system, the max. power d. and energy d. reached up to 23.6 Wh/kg and 15,000 W/kg, resp. Besides, an outstanding cycling stability was obsd. after 10,000 cycles.
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    30. 30
      Hou, S.; Cai, X.; Wu, H.; Yu, X.; Peng, M.; Yan, K.; Zou, D. Nitrogen-doped graphene for dye-sensitized solar cells and the role of nitrogen states in triiodide reduction. Energy Environ. Sci. 2013, 6, 3356– 3362,  DOI: 10.1039/c3ee42516a
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      Nitrogen-doped graphene for dye-sensitized solar cells and the role of nitrogen states in triiodide reduction
      Hou, Shaocong; Cai, Xin; Wu, Hongwei; Yu, Xiao; Peng, Ming; Yan, Kai; Zou, Dechun
      Energy & Environmental Science (2013), 6 (11), 3356-3362CODEN: EESNBY; ISSN:1754-5706. (Royal Society of Chemistry)
      Nitrogen-doped graphene was demonstrated as an efficient and alternative metal-free electrocatalyst for dye-sensitized solar cells. Electrochem. measurements showed that the nitrogen-doping process can remarkably improve the catalytic activity of graphene toward triiodide redn., lower the charge transfer resistance, and thus enhance the corresponding photovoltaic performance. Furthermore, the nitrogen doping levels ranging from 3.5 at% to 18 at%, as well as the nitrogen states (including pyrrolic, pyridinic and quaternary configurations) in graphene, were controlled to interpret the roles of graphene structure in catalytic activity and device performance. The results suggested that the nitrogen states, rather than the total N content, have a significant effect on the catalytic activity. Both pyridinic and quaternary nitrogen states can provide active sites for promoting triiodide redn. reaction, probably due to the shift in redox potential and the lowered adsorption energy.
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    31. 31
      Wei, M.; Marrakchi, F.; Yuan, C.; Cheng, X.; Jiang, D.; Zafar, F. F.; Fu, Y.; Wang, S. Adsorption modeling, thermodynamics, and DFT simulation of tetracycline onto mesoporous and high-surface-area NaOH-activated macroalgae carbon. J. Hazard. Mater. 2022, 425, 127887,  DOI: 10.1016/j.jhazmat.2021.127887
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      31
      Adsorption modeling, thermodynamics, and DFT simulation of tetracycline onto mesoporous and high-surface-area NaOH-activated macroalgae carbon
      Wei, Manman; Marrakchi, Fatma; Yuan, Chuan; Cheng, Xiaoxue; Jiang, Ding; Zafar, Fatemeh Fazeli; Fu, Yanxia; Wang, Shuang
      Journal of Hazardous Materials (2022), 425 (), 127887CODEN: JHMAD9; ISSN:0304-3894. (Elsevier B.V.)
      Activated carbon (ENAC) was prepd. by NaOH activation, using macroalgae (Enteromorpha clathrate) as raw material. The prepd. activated carbon has a large surface area (1238.491 m2 g-1) and its total pore vol. and av. pore size are 0.6823 cm3g-1 and 2.2038 nm, resp. The ENAC was characterized by SEM, FTIR, BET and XPS. The effects of contact time (0-960 min), initial tetracycline (TC) concn. (50-500 mg L-1), temp. (30-50°C) and initial pH (2-11) on TC adsorption were evaluated. The adsorption isotherm and adsorption kinetics were discussed. Results showed that the adsorption isotherm was the Langmuir model, and the adsorption process can be described by the pseudo-second-order model. The N2 adsorption-desorption isotherm was type IV, indicating that the activated carbon had mesoporous structure. Thermodn. anal. showed that the adsorption process was endothermic and spontaneous. The max. adsorption capacity of TC was 381.584 mg g-1. D. functional theory (DFT) was used to simulate and analyze the adsorption process, and the influence of different types of N on the adsorption was expounded. The results showed that there are electrostatic interactions, π-π interactions and hydrogen bonding between the adsorbent and TC. These results indicated that the prepd. ENAC had a great application prospect in the removal of antibiotics from aq. soln.
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    32. 32
      Sun, L.; Tian, C.; Li, M.; Meng, X.; Wang, L.; Wang, R.; Yin, J.; Fu, H. From coconut shell to porous graphene-like nanosheets for high-power supercapacitors. J. Mater. Chem. A 2013, 1, 6462– 6470,  DOI: 10.1039/c3ta10897j
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      32
      From coconut shell to porous graphene-like nanosheets for high-power supercapacitors
      Sun, Li; Tian, Chungui; Li, Meitong; Meng, Xiangying; Wang, Lei; Wang, Ruihong; Yin, Jie; Fu, Honggang
      Journal of Materials Chemistry A: Materials for Energy and Sustainability (2013), 1 (21), 6462-6470CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
      Sheet-like graphitic carbon with a porous structure can provide low-resistant pathways and short ion-diffusion channels for energy storage, and thus is expected to be an excellent material for high-power supercapacitors. Herein, porous graphene-like nanosheets (PGNSs) with a large surface area were synthesized for the first time via an easy and cost-effective SAG (simultaneous activation-graphitization) route from renewable biomass waste coconut shell. In the synthesis, the graphitic catalyst precursor (FeCl3) and activating agent (ZnCl2) were introduced simultaneously into the skeleton of the coconut shell through coordination of the metal precursor with the functional groups in the coconut shell, thus making simultaneous realization of activation and graphitization of the carbon source under heat treatment. Notably, the iron catalyst in the framework of the coconut shell can generate a carburized phase which plays a key role in the formation of a graphene-like structure during the pyrolytic process. The results indicated that PGNSs possess good elec. cond. due to the high graphitic degree, exceptionally high Brunauer-Emmett-Teller surface area (SBET = 1874 m2 g-1) and large pore vol. (1.21 cm3 g-1). While being used as a supercapacitor electrode without the use of any conductive additives, PGNSs exhibit a high specific capacitance of 268 F g-1, much higher than that of activated carbon (210 F g-1) fabricated by only activation and graphitic carbon (117 F g-1) by only graphitization at 1 A g-1. Also, PGNSs show superior cycle durability and Coulombic efficiency over 99.5% after 5000 cycles in KOH. Remarkably, in an org. electrolyte, PGNSs also display an outstanding capacitance of 196 F g-1 at 1 A g-1. An energy d. of up to 54.7 W h kg-1 could be achieved at a high power d. of 10 kW kg-1. The SAG strategy developed here would provide a novel route for low-cost and large-scale prodn. of PGNS electrode materials for high-power supercapacitors.
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      Chen, W.; Wang, X.; Feizbakhshan, M.; Liu, C.; Hong, S.; Yang, P.; Zhou, X. Preparation of lignin-based porous carbon with hierarchical oxygen enriched structure for high-performance supercapacitors. J. Colloid Interface Sci. 2019, 540, 524– 534,  DOI: 10.1016/j.jcis.2019.01.058
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      33
      Preparation of lignin-based porous carbon with hierarchical oxygen-enriched structure for high-performance supercapacitors
      Chen, Weimin; Wang, Xin; Feizbakhshan, Mohammad; Liu, Chaozheng; Hong, Shu; Yang, Pei; Zhou, Xiaoyan
      Journal of Colloid and Interface Science (2019), 540 (), 524-534CODEN: JCISA5; ISSN:0021-9797. (Elsevier B.V.)
      The biomass-based porous carbon produced by the conventional two-step method (carbonization followed by chem. activation) has a high prodn. cost and an undeveloped mesopore/macropore structure. In this study, lignin was successfully converted into porous carbon (LPC) in one step by microwave heating combined with the use of humidified nitrogen. The obtained LPC had abundant micropores (0.70 cm-3·g-1), hierarchical pore distribution (mesopore ratio: 65.8%), and an oxygen-enriched chem. structure (surface oxygen content: 16.5%). These characteristics provided a high energy d. (23.0 kW·kg-1 at 10 A·g-1) and excellent rate capability of the prepd. supercapacitor in a gel electrolyte (polyvinyl alc./LiCl), leading to a high specific capacitance of 173 F·g-1 at 0.5 A·g-1, and 71.1% at 10 A·g-1 remains. The prepd. supercapacitor could deliver a high power d. of 1.1 kW·kg-1 at the max. energy d. The obtained results demonstrate the feasibility of the proposed energy-saving cost-effective prepn. approach to obtain a high-performance supercapacitor with a low prodn. cost.
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      Song, M.; Zhou, Y.; Ren, X.; Wan, J.; Du, Y.; Wu, G.; Ma, F. Biowaste-based porous carbon for supercapacitor: The influence of preparation processes on structure and performance. J. Colloid Interface Sci. 2019, 535, 276– 286,  DOI: 10.1016/j.jcis.2018.09.055
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      34
      Biowaste-based porous carbon for supercapacitor: The influence of preparation processes on structure and performance
      Song, Mingyuan; Zhou, Yuhao; Ren, Xue; Wan, Jiafeng; Du, Yueyao; Wu, Guang; Ma, Fangwei
      Journal of Colloid and Interface Science (2019), 535 (), 276-286CODEN: JCISA5; ISSN:0021-9797. (Elsevier B.V.)
      Here, a series of porous carbon based supercapacitor electrode materials have been synthesized by means of pyrolysis and hydrothermal methods combining with KOH activation using the biomass wastes mung bean husks as resources. The influence of synthesis process on the morphol., structure and supercapacitor performance of mung bean husks derived porous carbons has been investigated systematically. Esp., it is found that these oxygen-contg. groups on the biochar play a crucial role in fabricating the three-dimensional (3D) hierarchical porous structure carbon. The original bio-structured porous carbon (PC3-600), the 3D architecture porous carbon (HPC2-700) and the porous carbon block (HPPC2-700) have a high sp. surface area, and the former mainly contains micropores and the latter two possess multistage pores. The specific capacitance of PC3-600, HPC2-700 and HPPC2-700 is resp. up to 390 F g-1, 353 F g-1, 304 F g-1 at 1 A g-1, and still maintains as high as 287 F g-1, 270 F g-1 and 235 F g-1 with corresponding retention ratio of 73.5%, 76.48%, 77.3% even at a high c.d. of 50 A g-1. HPC2-700//HPC2-700 sym. supercapacitor achieves a high energy d. of 20.4 Wh kg-1 at 872 W kg-1 in 1 M Na2SO4 electrolyte.
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    35. 35
      Peiris, C.; Nayanathara, O.; Navarathna, C.-M.; Jayawardhana, Y.; Nawalage, S.; Burk, G.; Karunanayake, A. G.; Madduri, S. B.; Vithanage, M.; Kaumal, M. N.; Mlsna, T. E.; Hassan, E. B.; Abeysundara, S.; Ferezi, F.; Gunatilake, S. R. The influence of three acid modifications on the physicochemical characteristics of tea-waste biochar pyrolyzed at different temperatures: a comparative study. RSC Adv. 2019, 9, 17612– 17622,  DOI: 10.1039/C9RA02729G
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      The influence of three acid modifications on the physicochemical characteristics of tea-waste biochar pyrolyzed at different temperatures: a comparative study
      Peiris, Chathuri; Nayanathara, Oshani; Navarathna, Chanaka M.; Jayawardhana, Yohan; Nawalage, Samadhi; Burk, Griffin; Karunanayake, Akila G.; Madduri, Sunith B.; Vithanage, Meththika; Kaumal, M. N.; Mlsna, Todd E.; Hassan, El Barbary; Abeysundara, Sachith; Ferez, Felio; Gunatilake, Sameera R.
      RSC Advances (2019), 9 (31), 17612-17622CODEN: RSCACL; ISSN:2046-2069. (Royal Society of Chemistry)
      Tea-waste is an abundant feedstock for producing biochar (BC) which is considered to be a cost effective carbonaceous adsorbent useful for water remediation and soil amendment purposes. In the present study, tea-waste BC (TWBC) produced at three different temps. were subjected to nitric, sulfuric and hydrochloric acid modifications (abbreviated as NM, SM and HM resp.). Characteristics of the raw and modified BC such as ultimate and proximate analyses, surface morphol., surface acidity and functionality, point of zero charge, cation exchange capacity (CEC) and thermal stability were compared to evaluate the influence of pyrolysis temp. and of modifications incorporated. The amt. of carboxylic and phenolic surface functionalities on TWBC was seen to decrease by 93.44% and 81.06% resp. when the pyrolysis temp. was increased from 300 to 700°. Addnl., the yield of BC was seen to decrease by 46% upon the latter temp. increment. The elemental anal. results provided justification for high-temp. BC being more hydrophobic as was obsd. by the 61% increase in H/C ratio which is an indication of augmented aromatization. The CEC was the highest for the low-temp. BC and was seen to further increase by NM which is attributed to the 81.89% increase in carboxylic functionalities. The surface area was seen to significantly increase for BC700 upon NM (∼27 times). The SM led to pore wall destruction which was obsd. in SEM images. Findings would enable the rational use of these particular modifications in relevant remediation and soil amendment applications.
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      Thithai, V.; Jin, X.; Ajaz Ahmed, M.; Choi, J.-W. Physicochemical Properties of Activated Carbons Produced from Coffee Waste and Empty Fruit Bunch by Chemical Activation Method. Energies 2021, 14, 3002,  DOI: 10.3390/en14113002
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      Physicochemical properties of activated carbons produced from coffee waste and empty fruit bunch by chemical activation method
      Thithai, Vilaysit; Jin, Xuanjun; Ahmed, Muhammed Ajaz; Choi, Joon-Weon
      Energies (Basel, Switzerland) (2021), 14 (11), 3002CODEN: ENERGA; ISSN:1996-1073. (MDPI AG)
      In this study, coffee waste (CW) and empty fruit bunches (EFB) were employed as pre-cursors for the prodn. of activated carbons by a chem. activation method. KOH, ZnCl2, and H3PO4 were used as activating agents along with their three mixing ratios of 1:0, 1:1, 1:3, wt./wt., and carbonization temps. of 600°C, 700°C, and 800°C were used to prep. these activated carbons. The highest yields of produced activated carbons were obsd. at 600°C with a value of 45.20% for coffee waste and 48.20% for empty fruit bunch, with a 1:3 wt./wt. (H3PO4) ratio. However, the max. sp. surface area was 3068 m2 g-1, and 2147 m2 g-1 obtained at 800°C for coffee waste and empty fruit bunch activated carbons, resp. The surface features of these products exhibited acute morphol. changes, as were clearly noticed via SEM studies. Moreover, in the Van Krevelen diagram, it was also obsd. that both the H/C and O/C ratios were dramatically decreased to 0.0019 and 0.0759, and 0.0066 and 0.1659 for coffee waste and empty fruit bunch at 800°C with a (1:3) potassium hydroxide and zinc chloride ratio, resp., and this similar phenomenon was also supported by a thermal gravimetric anal. All these results, together with the specific characteristics of the products, suggest that this scheme can be an effective strategy for the activated carbon prodn. from such residues.
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    37. 37
      Chatir, E. M.; El Hadrami, A.; Ojala, S.; Brahmi, R. Production of activated carbon with tunable porosity and surface chemistry via chemical activation of hydrochar with phosphoric acid under oxidizing atmosphere. Surf. Interfaces 2022, 30, 101849,  DOI: 10.1016/j.surfin.2022.101849
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      Production of activated carbon with tunable porosity and surface chemistry via chemical activation of hydrochar with phosphoric acid under oxidizing atmosphere
      Chatir, El Mehdi; El Hadrami, Abdelouahab; Ojala, Satu; Brahmi, Rachid
      Surfaces and Interfaces (2022), 30 (), 101849CODEN: SIUNCN; ISSN:2468-0230. (Elsevier B.V.)
      This work highlights the chem. activation of hydrothermally carbonized biomass with phosphoric acid under static air as activating atm. Argan nut shells were hydrothermally carbonized, and then chem. activated with phosphoric acid under oxidizing atm. The activated carbons displayed excellent sp. surface areas (from 1200 m2g-1 to 1880 m2g-1) and the material yield were in acceptable level (between 27 and 50%). The varied activation conditions provided a distinctive possibility for creating and controlling the mesoporosity of the activated carbons. At 500°C, a mesoporosity around of 93% could be reached by an H3PO4 impregnation ratio of 4. The activating temp. 500°C and the impregnation ratio of 3 were obsd. as optimum for achieving the best textural properties. The optimized material HC-500-3 exhibited a specific area of 1880 m2g-1, pore vol. and av. pore diam. of 1.36 cm3g-1 and 2.9 nm, as well as good amt. of oxygen functional groups (2.25 mmolg-1) including carboxyl, phenol, and lactone groups. The adsorption performance of optimized material was evaluated using Bisphenol A as a target mol. The adsorption process could be described by Weber Morris and Langmuir isotherm models. At a temp. of 25°C, Langmuir monolayer adsorption capacity was obsd. to be 420 mgg-1 which is comparable or higher than those reported previously. The estd. thermodn. parameters indicate spontaneous and exothermic adsorption process (ΔH° = -19.39 kJmol-1; -5.58 kJmol-1 ≤ ΔG° ≤ -4.65 kJmol-1). The mesoporous activated carbon prepd. by chem. activation of biomass-derived hydrochar under atm. air proved to be very potential adsorbent for Bisphenol A removal.
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    38. 38
      Chen, W.; Gong, M.; Li, K.; Xia, M.; Chen, Z.; Xiao, H.; Fang, Y.; Chen, Y.; Yang, H.; Chen, H. Insight into KOH activation mechanism during biomass pyrolysis: Chemical reactions between O-containing groups and KOH. Appl. Energy 2020, 278, 115730,  DOI: 10.1016/j.apenergy.2020.115730
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      Insight into KOH activation mechanism during biomass pyrolysis: Chemical reactions between O-containing groups and KOH
      Chen, Wei; Gong, Meng; Li, Kaixu; Xia, Mingwei; Chen, Zhiqun; Xiao, Haoyu; Fang, Yang; Chen, Yingquan; Yang, Haiping; Chen, Hanping
      Applied Energy (2020), 278 (), 115730CODEN: APENDX; ISSN:0306-2619. (Elsevier Ltd.)
      In this study, the effects of KOH/biomass ratios (1:8 to 1:1) and temps. (400-800°C) on biomass pyrolysis were investigated. The KOH chem. activation mechanism was explored by revealing the evolution mechanisms of the gaseous product, bio-oil, biochar, and KOH, based on expts. and quantum calcns. Results showed that KOH can react with active O-contg. species in biomass, which was the main reaction at lower ratios (1:8-1:2) or lower temps. (400-600°C). Here, KOH was completely transformed to K2CO3, leading to the formation of large amts. of gaseous products and phenols (reaching 75%). The reaction between KOH and more stable carbon fragments, however, was enhanced at higher ratios (>1:2) or higher temps. (700-800°C), such that it became the main reaction. With a significant decrease in the phenols and O-species, the hydrocarbons became the dominant species (reaching a content of 57.43%). For biochar, the reactions among KOH, O-contg. species, and carbon fragments generated an abundance of vacancies in the biochar. The OH- from KOH rapidly entered these vacancies, forming a large amt. of new O-contg. groups (i.e., C=O, -OH, C-O, O-C=O, and -COOH groups). This also caused an increase in oxygen content (reaching 23.68 wt%) in biochar. At higher temps., the reactions between KOH and biomass were significantly enhanced, along with a sharp increase in the sp. surface area (reaching 1351.13 m2/g).
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      Guo, S.; Chen, Y.; Shi, L.; Dong, Y.; Ma, J.; Chen, X.; Song, H. Nitrogen-doped biomass-based ultra-thin carbon nanosheets with interconnected framework for High-Performance Lithium-Ion Batteries. Appl. Surf. Sci. 2018, 437, 136– 143,  DOI: 10.1016/j.apsusc.2017.12.144
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      Nitrogen-doped biomass-based ultra-thin carbon nanosheets with interconnected framework for High-Performance Lithium-Ion Batteries
      Guo, Shasha; Chen, Yaxin; Shi, Liluo; Dong, Yue; Ma, Jing; Chen, Xiaohong; Song, Huaihe
      Applied Surface Science (2018), 437 (), 136-143CODEN: ASUSEE; ISSN:0169-4332. (Elsevier B.V.)
      In this paper, a low-cost and environmental friendly synthesis strategy is proposed to fabricate nitrogen-doped biomass-based ultra-thin carbon nanosheets (N-CNS) with interconnected framework by using soybean milk as the carbon precursor and sodium chloride as the template. The interconnected porous nanosheet structure is beneficial for lithium ion transportation, and the defects introduced by pyridine nitrogen doping are favorable for lithium storage. When used as the anodes for lithium-ion batteries, the N-CNS electrode shows a high initial reversible specific capacity of 1334 mAh g-1 at 50 mA g-1, excellent rate performance (1212, 555 and 336 mAh g-1 at 0.05, 0.5 and 2 A g-1, resp.) and good cycling stability (355 mAh g-1 at 1 A g-1 after 1000 cycles). Furthermore, this study demonstrates the prospects of biomass and soybean milk, as the potential anode for the application of electrochem. energy storage devices.
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      Bello, A.; Fashedemi, O. O.; Barzegar, F.; Madito, M. J.; Momodu, D. Y.; Masikhwa, T. M.; Dangbegnon, J. K.; Manyala, N. Microwave synthesis: Characterization and electrochemical properties of amorphous activated carbon-MnO2 nanocomposite electrodes. J. Alloys Compd. 2016, 681, 293– 300,  DOI: 10.1016/j.jallcom.2016.04.227
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      Microwave synthesis: Characterization and electrochemical properties of amorphous activated carbon-MnO2 nanocomposite electrodes
      Bello, A.; Fashedemi, O. O.; Barzegar, F.; Madito, M. J.; Momodu, D. Y.; Masikhwa, T. M.; Dangbegnon, J. K.; Manyala, N.
      Journal of Alloys and Compounds (2016), 681 (), 293-300CODEN: JALCEU; ISSN:0925-8388. (Elsevier B.V.)
      The green chem. route (microwave) was used to produce nanocomposite materials based on activated carbon (AC) and manganese (Mn) oxide nanostructures. XRD anal. revealed that amorphous and cryst. oxide structures were synthesized. SEM studies revealed rod-like α-MnO2 for the pristine sample, while cubic Mn3O4 and irregularly shaped MnO2 structures anchored on the AC substrate, with the nanostructures being uniformly distributed on the AC. The electrochem. tests of the composites as electrodes showed that the amorphous AC-MnO2 had a specific capacitance of 180 F g-1, nearly four times higher than that of the cryst. AC-Mn3O4 composite electrode (55 F g-1). The coulombic efficiency for the AC-MnO2 cell was 98% after 5000 cycles, indicating only a small loss of capacitance. The green route technique and good electrochem. properties indicate that the amorphous AC-MnO2 nanocomposite could be a good material for high-capacity, low-cost, and environmentally friendly electrodes for electrochem. capacitors.
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      Neiva, D. M.; Araújo, S.; Gominho, J.; Carneiro, A. d. C.; Pereira, H. An integrated characterization of Picea abies industrial bark regarding chemical composition, thermal properties and polar extracts activity. PLoS One 2018, 13, e0208270  DOI: 10.1371/journal.pone.0208270
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      An integrated characterization of Picea abies industrial bark regarding chemical composition, thermal properties and polar extracts activity
      Neiva, Duarte M.; Araujo, Solange; Gominho, Jorge; Carneiro, Angelica de Cassia; Pereira, Helena
      PLoS One (2018), 13 (11), e0208270/1-e0208270/14CODEN: POLNCL; ISSN:1932-6203. (Public Library of Science)
      Present work dets. chem. and thermal characteristics as well as phytochem. and antioxidant potential of polar extractives of the Picea abies bark from industrial mill, their wood and bark components and also different bark fractions obtained by mech fractionization. Aim is to increase knowledge on Picea abies bark to better det. possible uses other than burning for energy prodn. and to test initial size redn. process to achieve fractions with different characteristics. Compared to wood, bark presented similar lignin higher mineral and extractives and lower polysaccharides contents. Regarding bark fractions the fines showed higher ash , extractives and lignin than the coarse fraction. Phytochem. profile of ethanol and water exts. presented higher contents for bark than wood of total phenols (2x higher), flavonoids (3x higher) and tannins (4-10× higher) with an increasing tendency with particle size. Bark antioxidant activity was higher than that of wood for ferric-reducing antioxidant power and free radical scavenging activity methods. Bark thermal properties showed a much lower volatiles to fixed carbon ratio (V/FC) than wood (3.1 vs 5.2) although the same higher heating value. Bark presented chem. features that point to their possible upgrade, whether by taking advantage of the high extractives with bioactive compds. or the prodn. potential for hemicellulose-derived oligomers with possible use in nutraceutical and pharmaceutical industries.
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      Thyrel, M.; Backman, R.; Boström, D.; Skyllberg, U.; Lestander, T. A. Phase transitions involving Ca – The most abundant ash forming element – In thermal treatment of lignocellulosic biomass. Fuel 2021, 285, 119054,  DOI: 10.1016/j.fuel.2020.119054
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      Phase transitions involving Ca - The most abundant ash forming element - In thermal treatment of lignocellulosic biomass
      Thyrel, Mikael; Backman, Rainer; Bostroem, Dan; Skyllberg, Ulf; Lestander, Torbjoern A.
      Fuel (2021), 285 (), 119054CODEN: FUELAC; ISSN:0016-2361. (Elsevier Ltd.)
      Torrefaction, pyrolysis and gasification are of interest to convert lignocellulosic biomass into fuels and chems. These techniques involve thermal treatment at low partial pressures of oxygen. However, little is known about the transformation of ash elements during these processes. The phase transition of the major ash element calcium (Ca) was therefore studied with powder from pine as biomass model treated at temps. 300-800° under atmospheres of 100% N2, 3% O2 and 6% O2 and thermodn. equil. modeling. For evaluation, x-ray powder diffraction and synchrotron Ca K-edge x-ray absorption near edge structure (XANES) spectroscopy in combination with linear combination fitting and ref. compds. was used. The most abundant Ca-contg. species in the untreated material was thermally unstable Ca oxalate (CaC2O4) primarily decompg. into Ca phases dominated by carbonates at temps. up to 600°. Double carbonates of calcium and potassium were obsd. in the form of fairchildiite/butscheliite (K2Ca(CO3)2), and these phases were stable over the low temp. range studied. Hydroxyapatite (Ca5(PO4)3OH) was expected to be present and thermally stable over the entire temp. interval and was found in untreated material. At temps. above 600° calcium oxide (CaO) was formed. The amt. of oxygen had little effect on the phase transitions. The results of thermodn. modeling were in agreement with XANES showing that this is a versatile technique that can be applied to systems as complex as Ca phase transitions in thermally treated lignocellulosic biomass at low partial pressures of oxygen.
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      Zhu, C.; Chen, J.; Liu, S.; Cheng, B.; Xu, Y.; Zhang, P.; Zhang, Q.; Li, Y.; Zhong, S. Improved electrochemical performance of bagasse and starch-modified LiNi0.5Mn0.3Co0.2O2 materials for lithium-ion batteries. J. Mater. Sci. 2018, 53, 5242– 5254,  DOI: 10.1007/s10853-017-1926-4
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      Improved electrochemical performance of bagasse and starch-modified LiNi0.5Mn0.3Co0.2O2 materials for lithium-ion batteries
      Zhu, Caijian; Chen, Jun; Liu, Shanshan; Cheng, Boming; Xu, Yong; Zhang, Pengwei; Zhang, Qian; Li, Yutao; Zhong, Shengwen
      Journal of Materials Science (2018), 53 (7), 5242-5254CODEN: JMTSAS; ISSN:0022-2461. (Springer)
      Org. C-coated LiNi0.5Mn0.3Co0.2O2 materials are prepd. by mixing 2 or 5% starch or bagasse evenly with the synthesized LiNi0.5Mn0.3Co0.2O2 material and calcining for 10 h at 750°. The microstructures and electrochem. performance are studied by x-ray diffraction, SEM, C/S anal., TEM and electrochem. testing. The org. C coated on the surface of LiNi0.5Mn0.3Co0.2O2 material does not change the surface morphol. and crystal structure, but greatly improves the cond., rate and cycle performance of the LiNi0.5Mn0.3Co0.2O2 cathode in a Li-ion battery. The initial discharge capacity of the synthesized LiNi0.5Mn0.3Co0.2O2 material is 147.8 mAh g-1, which increases to 152.4 and 153.3 mAh g-1 for 2% starch and bagasse, resp. After 100 cycles, the capacity retention rates are 70.7% (uncoated), 83.3% (coated with 2% starch), 90.1% (coated with 2% bagasse), 83.1% (coated with 5% starch) and 91.1% (coated with 5% bagasse). The influence of the percentage of coated C and its dispersion uniformity on the performance of the battery is analyzed. A small coating capacity and uniform C film can achieve better performance. Rational org. C coating technol. is an effective way to improve the electrochem. performance of LiNi1-x-yMnxCoyO2-based material.
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      Meddings, N.; Heinrich, M.; Overney, F.; Lee, J.-S.; Ruiz, V.; Napolitano, E.; Seitz, S.; Hinds, G.; Raccichini, R.; Gaberšček, M.; Park, J. J. Power Sources 2020, 480, 228742,  DOI: 10.1016/j.jpowsour.2020.228742
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      Application of electrochemical impedance spectroscopy to commercial Li-ion cells: A review
      Meddings, Nina; Heinrich, Marco; Overney, Frederic; Lee, Jong-Sook; Ruiz, Vanesa; Napolitano, Emilio; Seitz, Steffen; Hinds, Gareth; Raccichini, Rinaldo; Gaberscek, Miran; Park, Juyeon
      Journal of Power Sources (2020), 480 (), 228742CODEN: JPSODZ; ISSN:0378-7753. (Elsevier B.V.)
      A review. Electrochem. impedance spectroscopy (EIS) is a widely applied non-destructive method of characterization of Li-ion batteries. Despite its ease of application, there are inherent challenges in ensuring the quality and reproducibility of the measurement, as well as reliable interpretation and validation of impedance data. Here, we present a focus review summarizing best metrol. practice in the application of EIS to com. Li-ion cells. State-of-the-art methods of EIS interpretation and validation are also reported and examd. to highlight the benefits and drawbacks of the technique.
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      Subramaniyam, C. M.; Srinivasan, N. R.; Tai, Z.; Liu, H. K.; Goodenough, J. B.; Dou, S. X. Self-assembled porous carbon microparticles derived from halloysite clay as a lithium battery anode. J. Mater. Chem. A 2017, 5, 7345– 7354,  DOI: 10.1039/C7TA00940B
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      Self-assembled porous carbon microparticles derived from halloysite clay as a lithium battery anode
      Subramaniyam, Chandrasekar M.; Srinivasan, N. R.; Tai, Zhixin; Liu, Hua Kun; Goodenough, John B.; Dou, Shi Xue
      Journal of Materials Chemistry A: Materials for Energy and Sustainability (2017), 5 (16), 7345-7354CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
      A naturally available clay mineral, halloysite, is used as a templating agent for the prepn. of porous C microparticles (PCMs); these PCMs were studied as a candidate for Li-ion battery (LIB) anodes. The PCMs are obtained with furfuryl alc. as the C precursor; we also propose a possible mechanism for their self-assembled structure. This structure exhibits a Brunauer-Emmett-Teller surface area of 329 m2/g, which is higher than that of halloysite (50 m2/g). Even after 300 cycles, the PCMs exhibited a stable reversible discharge capacity of 600 mAh/g when tested at 100 mA/g. The presence of porous structure in PCM electrode provides surface controlled reaction, contributing pseudocapacitance (58.5%) to the total charge storage capacity.
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      Choi, C.; Ashby, D. S.; Butts, D. M.; DeBlock, R. H.; Wei, Q.; Lau, J.; Dunn, B. Achieving high energy density and high power density with pseudocapacitive materials. Nature Rev. Mater. 2019, 5, 5– 19,  DOI: 10.1038/s41578-019-0142-z
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      Augustyn, V.; Simon, P.; Dunn, B. Pseudocapacitive oxide materials for high-rate electrochemical energy storage. Energy Environ. Sci. 2014, 7, 1597– 1614,  DOI: 10.1039/c3ee44164d
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      Pseudocapacitive oxide materials for high-rate electrochemical energy storage
      Augustyn, Veronica; Simon, Patrice; Dunn, Bruce
      Energy & Environmental Science (2014), 7 (5), 1597-1614CODEN: EESNBY; ISSN:1754-5706. (Royal Society of Chemistry)
      Electrochem. energy storage technol. is based on devices capable of exhibiting high energy d. (batteries) or high power d. (electrochem. capacitors). There is a growing need, for current and near-future applications, where both high energy and high power densities are required in the same material. Pseudocapacitance, a faradaic process involving surface or near surface redox reactions, offers a means of achieving high energy d. at high charge-discharge rates. Here, we focus on the pseudocapacitive properties of transition metal oxides. First, we introduce pseudocapacitance and describe its electrochem. features. Then, we review the most relevant pseudocapacitive materials in aq. and non-aq. electrolytes. The major challenges for pseudocapacitive materials along with a future outlook are detailed at the end.
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      Surace, Y.; Leanza, D.; Mirolo, M.; Kondracki, Ł.; Vaz, C. A. F.; El Kazzi, M.; Novák, P.; Trabesinger, S. Evidence for stepwise formation of solid electrolyte interphase in a Li-ion battery. Energy Storage Mater. 2022, 44, 156– 167,  DOI: 10.1016/j.ensm.2021.10.013
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      Hong, K.-L.; Qie, L.; Zeng, R.; Yi, Z.-Q.; Zhang, W.; Wang, D.; Yin, W.; Wu, C.; Fan, Q. J.; Zhang, W.-X.; Huang, Y.-H. Biomass derived hard carbon used as a high performance anode material for sodium ion batteries. J. Mater. Chem. A 2014, 2, 12733,  DOI: 10.1039/C4TA02068E
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      Biomass derived hard carbon used as a high performance anode material for sodium ion batteries
      Hong, Kun-lei; Long, Qie; Zeng, Rui; Yi, Zi-qi; Zhang, Wei; Wang, Duo; Yin, Wei; Wu, Chao; Fan, Qing-jie; Zhang, Wu-xing; Huang, Yun-hui
      Journal of Materials Chemistry A: Materials for Energy and Sustainability (2014), 2 (32), 12733-12738CODEN: JMCAET; ISSN:2050-7496. (Royal Society of Chemistry)
      A porous hard carbon material was synthesized by the simple pyrolysis of H3PO4-treated biomass, i.e., pomelo peels, at 700 °C in N2. The as-obtained hard carbon had a 3D connected porous structure and a large sp. surface area of 1272 m2 g-1. XPS anal. showed that the carbon material was functionalized by O-contg. and P-contg. groups. The porous hard carbon was used as an anode for sodium ion batteries and exhibited good cycling stability and rate capability, delivering a capacity of 181 mA h g-1 at 200 mA g-1 after 220 cycles and retaining a capacity of 71 mA h g-1 at 5 A g-1. The sodium storage mechanisms of the porous hard carbon can be explained by Na+ intercalation into the disordered graphene layers, redox reaction of the surface O-contg. functional groups and Na+ storage in the nanoscale pores. However, the porous hard carbon demonstrated a low coulombic efficiency of 27%, resulting from the formation of a solid electrolyte interphase film and the side reactions of surface phosphorus groups.
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      Ghani, U.; Iqbal, N.; Aboalhassan, A. A.; Liu, B.; Aftab, T.; Zada, I.; Ullah, F.; Gu, J.; Li, Y.; Zhu, S.; Liu, Q. One-step sonochemical fabrication of biomass-derived porous hard carbons; towards tuned-surface anodes of sodium-ion batteries. J. Colloid Interface Sci. 2022, 611, 578– 587,  DOI: 10.1016/j.jcis.2021.12.104
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      One-step sonochemical fabrication of biomass-derived porous hard carbons; towards tuned-surface anodes of sodium-ion batteries
      Ghani, Usman; Iqbal, Nousheen; Aboalhassan, Ahmed A.; Liu, Bowen; Aftab, Tabish; Zada, Imran; Ullah, Farman; Gu, Jiajun; Li, Yao; Zhu, Shenmin; Liu, Qinglei
      Journal of Colloid and Interface Science (2022), 611 (), 578-587CODEN: JCISA5; ISSN:0021-9797. (Elsevier B.V.)
      A facile one-step sonochem. activation method is utilized to fabricate biomass-derived 3D porous hard carbon (PHC-1) with tuned-surface and is compared with the conventional two-step activation method. As raw biomass offers good KOH impregnation, ultrasonication power diffuses both K+ and OH- ions deep into its interior, creating various nanopores and attaching copious functional groups. In contrast, conventional activation lacks these features under the same carbonization/activation parameters. The high porosity (1599 m2/g), rich functional groups (O = 8.10%, N = 0.95%), and well-connected nanoporous network resulting from sonochem. activation, remarkably increased specific capacity, surface wettability, and electrode stability, consequently improved electrochem. performance. Benefiting from its suitable microstructure, PHC-1 possesses superior specific capacity (330 mAh/g at 20 mA/g), good capacity retention (89.5%), and excellent structural stability over 500 sodiation/desodiation cycles at high c.d. (1000 mA/g). Apart from modus operandi comparison, the two activation methods also provide mechanistic insights as the low-voltage plateau region and graphitic layers decrease simultaneously. This work suggests a scalable and economical approach for synthesizing large-scale activated porous carbons that are used in various applications, be it energy storage, water purifn., or gas storage, to name a few.
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      Campbell, B.; Ionescu, R.; Favors, Z.; Ozkan, C. S.; Ozkan, M. Bio-derived, binderless, hierarchically porous carbon anodes for Li-ion batteries. Sci. Rep. 2015, 5, 14575– 14580,  DOI: 10.1038/srep14575
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      Bio-Derived, Binderless, Hierarchically Porous Carbon Anodes for Li-ion Batteries
      Campbell, Brennan; Ionescu, Robert; Favors, Zachary; Ozkan, Cengiz S.; Ozkan, Mihrimah
      Scientific Reports (2015), 5 (), 14575CODEN: SRCEC3; ISSN:2045-2322. (Nature Publishing Group)
      Here we explore the electrochem. performance of pyrolyzed skins from the species A. bisporus, also known as the Portobello mushroom, as free-standing, binder-free, and current collector-free Li-ion battery anodes. At temps. above 900 °C, the biomass-derived carbon nanoribbon-like architectures undergo unique processes to become hierarchically porous. During heat-treatment, the oxygen and heteroatom-rich orgs. and potassium compds. naturally present in the mushroom skins play a mutual role in creating inner void spaces throughout the resulting carbon nanoribbons, which is a process analogous to KOH-activation of carbon materials seen in literature. The pores formed in the pyrolytic carbon nanoribbons range in size from sub-nanometer to tens of nanometers, making the nanoribbons micro, meso, and macroporous. Detailed studies were conducted on the carbon nanoribbons using SEM and TEM to study morphol., as well as XRD and EDS to study compn. The self-supporting nanoribbon anodes demonstrate significant capacity increase as they undergo addnl. charge/discharge cycles. After a pyrolysis temp. of 1100 °C, the pristine anodes achieve over 260 mAh/g after 700 cycles and a Coulombic efficiency of 101.1%, without the use of harmful solvents or chem. activation agents.
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      Porous carbons with a high surface area have been prepd. from rice straw. The hierarchical porous network with large macroporous channels and micropores within the channel walls enable the porous carbons to provide the pathways for easy accessibility of electrolytes and fast transportation of lithium ions. These porous carbons which show a particular large reversible capacity are proved to be promising anode materials for high-rate and high-capacity lithium ion batteries.
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      Materials Letters (2022), 319 (), 132216CODEN: MLETDJ; ISSN:0167-577X. (Elsevier B.V.)
      Sodium ion batteries is regarded as promising energy storage devise for large scale application. Essentially, highly reversible anode material is crit. to promote its commercialization. Herein, new Zn-substituted NaZnV2(PO4)3/C nano composites were synthesized by a facile sol-gel method and the influence of the synthesizing temp. on the phase compn., morphol. and sodium-storage properties were investigated. The material synthesized at 800 °C showed the best cyclability and rate capability in the voltage range of 0.05 - 3.0 V. A high reversible capacity of 107 mAh g-1 was obtained at 2C, with a high capacity retention of 98% cycles after 100 cycles. The av. working potential is around 1.0 V, makes it a promising candidate as an anode material for sodium-ion batteries.
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      Sodium-ion batteries (SIBs) are regarded as an attractive alternative to lithium-ion batteries (LIBs) for large-scale com. applications, because of the abundant terrestrial reserves of sodium. Exporting suitable anode materials is the key to the development of SIBs and LIBs. In this contribution, we report on the fabrication of Bi@C microspheres using aerosol spray pyrolysis technique. When used as SIBs anode materials, the Bi@C microsphere delivered a high capacity of 123.5 mA h g-1 after 100 cycles at 100 mA g-1. The rate performance is also impressive (specific capacities of 299, 252, 192, 141, and 90 mA h g-1 are obtained under current densities of 0.1, 0.2, 0.5, 1, and 2 A g-1, resp.). Furthermore, the Bi@C microsphere also proved to be suitable LIB anode materials. The excellent electrochem. performance for both SIBs and LIBs can attributed to the Bi@C microsphere structure with Bi nanoparticles uniformly dispersed in carbon spheres.
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      A review. The purpose of this editorialis to sharpen the distinction using a short list of criteria alreadyoutlined in the papers, so that we are all speaking the samelanguage.
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    The Supporting Information is available free of charge at https://pubs.acs.org/doi/10.1021/acsomega.2c06054.

    • Figure S1, pore size distributions of Biochar-1 and Biochar-2. Figure S2, TEM images of Biochar-1 (a) and Biochar-2 (b). Figure S3, XRD patterns of Biochar-1 and Biochar-2. Figure S4, impedance spectra of a Biochar-1//Li cell after 5000 cycles (inset: simulated equivalent electrical circuit). Figure S5, determination of the Warburg constant from the slopes of the plots of Z′ vs ω–1/2 of (a) Biochar-1 and (b) Biochar-2. Figure S6, CV with mapping of lithium diffusion-controlled mechanism and capacitive effect in Biochar-1 at various scan rates. Table S1, comparative electrochemical performances of Biochar-1 and biomass carbonaceous materials as LIB anodes. Table S2, comparative electrochemical performances of Biochar-1 and biomass carbonaceous materials as NIB anodes. Figure S7, morphology of the Biochar-1 electrode at 3000× magnification: (a) fresh electrode and (b) after 5000 cycles. The fresh electrode composition consisted of Biochar-1 and a PVDF binder at a 9:1 weight ratio. Electrochemical performance of full cell using Biochar-1 as the anode and LiFePO4 as the cathode; (c) charge–discharge plot and (d) long cycling stability at various current densities (PDF)


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