Thin Films of Molybdenum Disulfide Doped with Chromium by Aerosol-Assisted Chemical Vapor Deposition (AACVD)
- David J. Lewis ,
- Aleksander A. Tedstone ,
- Xiang Li Zhong ,
- Edward A. Lewis ,
- Aidan Rooney ,
- Nicky Savjani ,
- Jack R. Brent ,
- Sarah J. Haigh ,
- M. Grace Burke ,
- Christopher A. Muryn ,
- James M. Raftery ,
- Chris Warrens ,
- Kevin West ,
- Sander Gaemers , and
- Paul O’Brien
Abstract

A combined single-source precursor approach has been developed for the deposition of thin films of Cr-doped molybdenum disulfide (MoS2) by aerosol-assisted chemical vapor deposition (AACVD). Tris(diethyldithiocarbamato)chromium(III) can also be used for the deposition of chromium sulfide (CrS). Films have been analyzed by a range of techniques including scanning electron microscopy (SEM), energy dispersive X-ray (EDX) spectroscopy, Raman spectroscopy, and powder X-ray diffraction (pXRD) to elucidate film morphology, composition, and crystallinity. The presence of Cr in the MoS2 films produces a number of striking morphological, crystallographic, and nanomechanical changes to the deposited films. The chromium dopant appears to be uniform throughout the MoS2 from the scanning transmission electron microscopy (STEM) EDX spectrum imaging of nanosheets produced by liquid-phase exfoliation of the thin films in N-methyl-2-pyrollidone.
Introduction
Figure 1

Figure 1. Layer structure of 2-H MoS2 after Pauling and co-workers. (17) Sulfur ions are represented by yellow spheres, molybdenum ions are represented by blue spheres. The unit cell is marked with a = 3.15(2) Å b= 3.15(2) Å c = 12.30(7) Å and α = 90° β = 90°, γ = 120°. Space group P63/mmc.
Experimental Section
General
Instrumentation
Tetrakis(diethyldithiocarbamato)molybdenum(IV) (MoL4)
Tris(diethyldithiocarbamato)chromium(III) (CrL3)
Aerosol-Assisted Chemical Vapor Deposition (AACVD)
Liquid-Phase Exfoliation of MoS2
Results and Discussion
Scheme 1

Figure 2

Figure 2. EDX spectroscopy of MoS2 thin films doped with varying amounts of chromium. (A) Comparison of theoretical amount of chromium doped into MoS2 films and the amount found experimentally by using EDX spectroscopy for deposition at 450 °C (● and - - - linear fit) and 500 °C (○ and ― linear fit). Secondary electron SEM images: (B) 0% Cr (MoS2), (C) 7.1% Cr, (D) 8.4 mol % Cr, (E) CrS; prepared at 450° by AACVD. All scale bars represent 5 μm.
Figure 3

Figure 3. (A) Raman spectra of 0% and 8.6% Cr-doped MoS2 thin films deposited at 450 °C. Insets: bright-field reflectance images of thin films at 50× magnification. (B) Plot of integrated peak intensity ratio at 227 and 408 cm–1 vs chromium dopant found experimentally by using EDX spectroscopy for deposition at 450 °C (●) and 500 °C (○). Line is provided as a trend guide and is not a fitted function.
Figure 4

Figure 4. Analysis of chromium-doped MoS2 thin films by powder X-ray diffraction. (A) Powder X-ray diffraction patterns for MoS2 thin films containing varying amounts of chromium deposited at 450 °C, deliberately y-offset for clarity. (B) Changes in d-spacing for the (002) plane vs chromium dopant found experimentally using EDX spectroscopy for deposition at 450 °C (●) and 500 °C (○). (C) Changes in the intensity of the (002) reflection vs chromium dopant found experimentally using EDX spectroscopy for deposition at 450 °C (● and linear fit - - -) and 500 °C (○ and linear fit ―).
Figure 5

Figure 5. Height profile images produced from atomic force microscopy of thin films grown at 450 °C. (A) MoS2, (B) 7.1 mol % Cr, (C) 8.6 mol % Cr, (D) 14.8 mol % Cr, (E) 17.7 mol % Cr, (F) CrS. Scale bars = 250 nm.
| film composition by EDXS | deposition temperature (°C) | arbitrary elastic modulus (Earb) |
|---|---|---|
| MoS2 – 31% Mo 69% S | 450 | 1.0 |
| MoS2 + 7.1% Cr | 450 | 1.4 |
| MoS2 + 8.6% Cr | 450 | 1.0 |
| MoS2 + 14.8% Cr | 450 | 0.5 |
| MoS2 + 17.7% Cr | 450 | 0.4 |
| CrS – 55% Cr 45% S | 450 | 1.2 |
| MoS2 – 36% Mo 63% S | 500 | 1.0 |
| MoS2 + 4.8% Cr | 500 | 2.0 |
| MoS2 + 8.7% Cr | 500 | 0.8 |
| MoS2 + 11.8% Cr | 500 | 1.5 |
| MoS2 + 16.6% Cr | 500 | N/Aa |
| CrS – 55% Cr 45% S | 500 | 2.3 |
Could not be measured due to roughness of film.
Figure 6

Figure 6. TEM imaging and HAADF STEM imaging of (A) undoped (0 mol % Cr, 450 °C) and (B) doped (7.1 mol % Cr, 450 °C) MoS2 nanosheets, respectively. Bright-field TEM images (left-hand images) and HAADF STEM images (center and left images) show the exfoliated flakes are typically >300 nm in diameter. High-resolution HAADF STEM images (right-hand images) of the undoped and doped samples, revealing atomic planes within the nanosheets (inset are Fourier transforms showing the different lattice orientations). The doped sample contains bundles of small randomly orientated flakes (although larger nanosheets with more uniform crystal structure are also found), whereas the undoped sample only shows larger highly crystalline sheets.
Figure 7

Figure 7. HAADF STEM and EDX spectrum imaging of (A) undoped (0 mol % Cr, 450 °C) and (B) doped (7.1 mol % Cr, 450 °C) MoS2 nanosheets, respectively. Deconvoluted elemental maps extracted from EDX spectrum images show that in both cases Mo and S are distributed uniformly throughout the flake at a spatial resolution approaching 10 nm. Carbon signal in (A) is from the amorphous carbon support film. For the doped sample in (B) the nanoscale distribution of Cr is found to be fairly uniform while for the undoped sample no Cr signal is detected.
Conclusions
Supporting Information
Powder X-ray diffraction patterns of CrS thin films on glass substrates; crystallography data and single crystal X-ray structure of CrL3; thermogravimetric analysis curve for CrL3; full powder X-ray diffraction patterns of MoS2 and Cr-doped MoS2 films grown at 450 °C by AACVD. This material is available free of charge via the Internet at http://pubs.acs.org.
Terms & Conditions
Most electronic Supporting Information files are available without a subscription to ACS Web Editions. Such files may be downloaded by article for research use (if there is a public use license linked to the relevant article, that license may permit other uses). Permission may be obtained from ACS for other uses through requests via the RightsLink permission system: http://pubs.acs.org/page/copyright/permissions.html.
Acknowledgment
D.J.L. and A.A.T. are funded by ICAM. S.J.H., A.R.. and E.A.L thank the U.S.A. Defense Threat Reduction Agency (grant no. HDTRA1-12-1-0013) as well as NoWNano CDT (EPSRC grant no. EP/G03737X/1) for funding support. The authors also wish to acknowledge funding support from H.M. Government (U.K.) for the FEI Titan G2 80-200 S/TEM associated with research capability of the Nuclear Advanced Manufacturing Research Centre. Some of the equipment used in this study were provided by the Engineering and Physical Sciences Research Council (Core Capability in Chemistry, EPSRC grant number EP/K039547/1). We would like to thank Dr. Caitlin Rice (University of Manchester) for useful discussion regarding MoS2 Raman spectral features and Dr. M. Azad Malik (University of Manchester) for useful discussions.
References
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- 32Finn, D. J.; Lotya, M.; Cunningham, G.; Smith, R. J.; McCloskey, D.; Donegan, J. F.; Coleman, J. N. J. Mater. Chem. C 2014, 2, 925– 932[Crossref], [CAS], Google Scholar32https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BC2cXit1Sksg%253D%253D&md5=6563c123fac83e549fb027b89a7ef55dInkjet deposition of liquid-exfoliated graphene and MoS2 nanosheets for printed device applicationsFinn, David J.; Lotya, Mustafa; Cunningham, Graeme; Smith, Ronan J.; McCloskey, David; Donegan, John F.; Coleman, Jonathan N.Journal of Materials Chemistry C: Materials for Optical and Electronic Devices (2014), 2 (5), 925-932CODEN: JMCCCX; ISSN:2050-7534. (Royal Society of Chemistry)Here we demonstrate inkjet printing of nanosheets of both graphene and MoS2 prepd. by liq. exfoliation. We describe a protocol for the prepn. of inks of nanosheets with well-defined size distribution and concn. up to 6 mg ml-1. Graphene traces were printed at low temp. (<70°) with no subsequent thermal or chem. treatment. Thin traces displayed percolation effects while traces with thickness above 160 nm displayed thickness-independent cond. of 3000 S m-1. We also demonstrate the printing of semiconducting traces using solvent-exfoliated, size-selected MoS2 nanosheets. Such traces can be combined with inkjet-printed graphene interdigitated array electrodes to produce all-printed photodetectors.
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- 49Brorson, M.; Carlsson, A.; Topsøe, H. Catal. Today 2007, 123, 31– 36[Crossref], [CAS], Google Scholar49https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BD2sXlsFKksLg%253D&md5=97ee64004f00128264578bc14ce8ea20The morphology of MoS2, WS2, Co-Mo-S, Ni-Mo-S and Ni-W-S nanoclusters in hydrodesulfurization catalysts revealed by HAADF-STEMBrorson, M.; Carlsson, A.; Topsoe, H.Catalysis Today (2007), 123 (1-4), 31-36CODEN: CATTEA; ISSN:0920-5861. (Elsevier B.V.)The HAADF-STEM technique (high-angle annular dark-field scanning transmission electron microscopy) allows the catalytically active edges to be imaged even for single layer metal sulfide structures. Unpromoted MoS2 and WS2 are predominantly present as slightly truncated triangular clusters contg. only a single S-M-S layer (M = Mo, W). The addn. of promoter atoms resulted in more heavy truncations consistent with the expected tendency for the Co-Mo-S structures to expose promoted S-type edges at the expense of unpromoted Mo-type edges. However, the HAADF-STEM results showed for the first time that Co-Mo-S and Ni-W-S may also expose extended high index truncations.
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Abstract

Figure 1

Figure 1. Layer structure of 2-H MoS2 after Pauling and co-workers. (17) Sulfur ions are represented by yellow spheres, molybdenum ions are represented by blue spheres. The unit cell is marked with a = 3.15(2) Å b= 3.15(2) Å c = 12.30(7) Å and α = 90° β = 90°, γ = 120°. Space group P63/mmc.
Scheme 1

Figure 2

Figure 2. EDX spectroscopy of MoS2 thin films doped with varying amounts of chromium. (A) Comparison of theoretical amount of chromium doped into MoS2 films and the amount found experimentally by using EDX spectroscopy for deposition at 450 °C (● and - - - linear fit) and 500 °C (○ and ― linear fit). Secondary electron SEM images: (B) 0% Cr (MoS2), (C) 7.1% Cr, (D) 8.4 mol % Cr, (E) CrS; prepared at 450° by AACVD. All scale bars represent 5 μm.
Figure 3

Figure 3. (A) Raman spectra of 0% and 8.6% Cr-doped MoS2 thin films deposited at 450 °C. Insets: bright-field reflectance images of thin films at 50× magnification. (B) Plot of integrated peak intensity ratio at 227 and 408 cm–1 vs chromium dopant found experimentally by using EDX spectroscopy for deposition at 450 °C (●) and 500 °C (○). Line is provided as a trend guide and is not a fitted function.
Figure 4

Figure 4. Analysis of chromium-doped MoS2 thin films by powder X-ray diffraction. (A) Powder X-ray diffraction patterns for MoS2 thin films containing varying amounts of chromium deposited at 450 °C, deliberately y-offset for clarity. (B) Changes in d-spacing for the (002) plane vs chromium dopant found experimentally using EDX spectroscopy for deposition at 450 °C (●) and 500 °C (○). (C) Changes in the intensity of the (002) reflection vs chromium dopant found experimentally using EDX spectroscopy for deposition at 450 °C (● and linear fit - - -) and 500 °C (○ and linear fit ―).
Figure 5

Figure 5. Height profile images produced from atomic force microscopy of thin films grown at 450 °C. (A) MoS2, (B) 7.1 mol % Cr, (C) 8.6 mol % Cr, (D) 14.8 mol % Cr, (E) 17.7 mol % Cr, (F) CrS. Scale bars = 250 nm.
Figure 6

Figure 6. TEM imaging and HAADF STEM imaging of (A) undoped (0 mol % Cr, 450 °C) and (B) doped (7.1 mol % Cr, 450 °C) MoS2 nanosheets, respectively. Bright-field TEM images (left-hand images) and HAADF STEM images (center and left images) show the exfoliated flakes are typically >300 nm in diameter. High-resolution HAADF STEM images (right-hand images) of the undoped and doped samples, revealing atomic planes within the nanosheets (inset are Fourier transforms showing the different lattice orientations). The doped sample contains bundles of small randomly orientated flakes (although larger nanosheets with more uniform crystal structure are also found), whereas the undoped sample only shows larger highly crystalline sheets.
Figure 7

Figure 7. HAADF STEM and EDX spectrum imaging of (A) undoped (0 mol % Cr, 450 °C) and (B) doped (7.1 mol % Cr, 450 °C) MoS2 nanosheets, respectively. Deconvoluted elemental maps extracted from EDX spectrum images show that in both cases Mo and S are distributed uniformly throughout the flake at a spatial resolution approaching 10 nm. Carbon signal in (A) is from the amorphous carbon support film. For the doped sample in (B) the nanoscale distribution of Cr is found to be fairly uniform while for the undoped sample no Cr signal is detected.
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- 44Wang, D.; Russell, T. P.; Nishi, T.; Nakajima, K. ACS Macro Lett. 2013, 2, 757– 760[ACS Full Text
], [CAS], Google Scholar44https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BC3sXht1WltrbN&md5=f288744ca2ae24e01d48db38c557ccfdAtomic Force Microscopy Nanomechanics Visualizes Molecular Diffusion and Microstructure at an InterfaceWang, Dong; Russell, Thomas P.; Nishi, Toshio; Nakajima, KenACS Macro Letters (2013), 2 (8), 757-760CODEN: AMLCCD; ISSN:2161-1653. (American Chemical Society)Here we demonstrate a simple, yet powerful method, at. force microscopy (AFM) nanomech. mapping, to directly visualize the interdiffusion and microstructure at the interface between two polymers. Nanomech. measurements on the interface between poly(vinyl chloride) (PVC) and poly(caprolactone) (PCL) allow quantification of diffusion kinetics, observation of microstructure, and evaluation of mech. properties of the interdiffusion regions. These results suggest that nanomech. mapping of interdiffusion enables the quantification of diffusion with high resoln. over large distances without the need of labeling and the assessment of mech. property changes resulting from the interdiffusion. - 45Savjani, N.; Lewis, E. A.; Pattrick, R. A. D.; Haigh, S. J.; O’Brien, P. RSC Adv. 2014, 4, 35609– 35613[Crossref], [CAS], Google Scholar45https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BC2cXht12msb3I&md5=bb8eaf86c9601e66958aab88d0f32db8MoS2 nanosheet production by the direct exfoliation of molybdenite minerals from several type-localitiesSavjani, Nicky; Lewis, Edward A.; Pattrick, Richard A. D.; Haigh, Sarah J.; O'Brien, PaulRSC Advances (2014), 4 (67), 35609-35613CODEN: RSCACL; ISSN:2046-2069. (Royal Society of Chemistry)Samples of the mineral molybdenite from three classic molybdenum mining localities were examd. as a potential source of molybdenum disulfide (MoS2) nanosheets. In all cases, ultrasonication-promoted exfoliation of these samples in N-methylpyrrolidone (NMP) was found to produce MoS2 as dispersed nanosheets with lateral sizes in the range of 200-600 nm and thicknesses between 1 and 10 at. trilayers. The MoS2 nanosheets obtained were found to be highly cryst. and largely defect-free, but tend to contain small amts. of aggregates on their surfaces. The exfoliated MoS2 dispersions were characterized by UV-Vis spectroscopy, Raman spectroscopy, SEM, (scanning) transmission electron microscopy ((S)TEM) and energy dispersive X-ray (EDX) spectroscopy. This work raises the possibility that mined, unrefined minerals could be a source of low-dimensional MoS2.
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], [CAS], Google Scholar47https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BC3MXhtlOksL3L&md5=af05fe19e2a019e7ce25373c42169ab1Photoluminescence from Chemically Exfoliated MoS2Eda, Goki; Yamaguchi, Hisato; Voiry, Damien; Fujita, Takeshi; Chen, Mingwei; Chhowalla, ManishNano Letters (2011), 11 (12), 5111-5116CODEN: NALEFD; ISSN:1530-6984. (American Chemical Society)A two-dimensional crystal of molybdenum disulfide (MoS2) monolayer is a photoluminescent direct gap semiconductor in striking contrast to its bulk counterpart. Exfoliation of bulk MoS2 via Li intercalation is an attractive route to large-scale synthesis of monolayer crystals. However, this method results in loss of pristine semiconducting properties of MoS2 due to structural changes that occur during Li intercalation. Here, we report structural and electronic properties of chem. exfoliated MoS2. The metastable metallic phase that emerges from Li intercalation was found to dominate the properties of as-exfoliated material, but mild annealing leads to gradual restoration of the semiconducting phase. Above an annealing temp. of 300°, chem. exfoliated MoS2 exhibit prominent band gap photoluminescence, similar to mech. exfoliated monolayers, indicating that their semiconducting properties are largely restored. - 48Bonde, J.; Moses, P. G.; Jaramillo, T. F.; Norskov, J. K.; Chorkendorff, I. Faraday Discuss. 2009, 140, 219– 231Google ScholarThere is no corresponding record for this reference.
- 49Brorson, M.; Carlsson, A.; Topsøe, H. Catal. Today 2007, 123, 31– 36[Crossref], [CAS], Google Scholar49https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BD2sXlsFKksLg%253D&md5=97ee64004f00128264578bc14ce8ea20The morphology of MoS2, WS2, Co-Mo-S, Ni-Mo-S and Ni-W-S nanoclusters in hydrodesulfurization catalysts revealed by HAADF-STEMBrorson, M.; Carlsson, A.; Topsoe, H.Catalysis Today (2007), 123 (1-4), 31-36CODEN: CATTEA; ISSN:0920-5861. (Elsevier B.V.)The HAADF-STEM technique (high-angle annular dark-field scanning transmission electron microscopy) allows the catalytically active edges to be imaged even for single layer metal sulfide structures. Unpromoted MoS2 and WS2 are predominantly present as slightly truncated triangular clusters contg. only a single S-M-S layer (M = Mo, W). The addn. of promoter atoms resulted in more heavy truncations consistent with the expected tendency for the Co-Mo-S structures to expose promoted S-type edges at the expense of unpromoted Mo-type edges. However, the HAADF-STEM results showed for the first time that Co-Mo-S and Ni-W-S may also expose extended high index truncations.
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- 51Bhachu, D. S.; Scanlon, D. O.; Saban, E. J.; Bronstein, H.; Parkin, I. P.; Carmalt, C. J.; Palgrave, R. G. J. Mater. Chem. A 2015, DOI: 10.1039/c4ta05522e
- 52Huang, C.-C.; Al-Saab, F.; Wang, Y.; Ou, J.-Y.; W. J, C.; Wang, S.; Gholipour, B.; Simpson, R. E.; Hewak, D. W. Nanoscale 2014, 6, 12792– 12797Google ScholarThere is no corresponding record for this reference.
- 53Derby, B. Annu. Rev. Mater. Res. 2010, 40, 395– 414[Crossref], [CAS], Google Scholar53https://chemport.cas.org/services/resolver?origin=ACS&resolution=options&coi=1%3ACAS%3A528%3ADC%252BC3cXhtVClt7bM&md5=c80b88344ad13a84d0497eff03d5e511Inkjet printing of functional and structural materials: fluid property requirements, feature stability, and resolutionDerby, BrianAnnual Review of Materials Research (2010), 40 (), 395-414CODEN: ARMRCU; ISSN:1531-7331. (Annual Reviews Inc.)A review. Inkjet printing is viewed as a versatile manufg. tool for applications in materials fabrication in addn. to its traditional role in graphics output and marking. The unifying feature in all these applications is the dispensing and precise positioning of very small vols. of fluid (1-100 pL) on a substrate before transformation to a solid. The application of inkjet printing to the fabrication of structures for structural or functional materials applications requires an understanding as to how the phys. processes that operate during inkjet printing interact with the properties of the fluid precursors used. Here we review the current state of understanding of the mechanisms of drop formation and how this defines the fluid properties that are required for a given liq. to be printable. The interactions between individual drops and the substrate as well as between adjacent drops are important in defining the resoln. and accuracy of printed objects. Pattern resoln. is limited by the extent to which a liq. drop spreads on a substrate and how spreading changes with the overlap of adjacent drops to form continuous features. There are clearly defined upper and lower bounds to the width of a printed continuous line, which can be defined in terms of materials and process variables. Finer-resoln. features can be achieved through appropriate patterning and structuring of the substrate prior to printing, which is essential if polymeric semiconducting devices are to be fabricated. Low advancing and receding contact angles promote printed line stability but are also more prone to solute segregation or "coffee staining" on drying.
Supporting Information
Supporting Information
ARTICLE SECTIONSPowder X-ray diffraction patterns of CrS thin films on glass substrates; crystallography data and single crystal X-ray structure of CrL3; thermogravimetric analysis curve for CrL3; full powder X-ray diffraction patterns of MoS2 and Cr-doped MoS2 films grown at 450 °C by AACVD. This material is available free of charge via the Internet at http://pubs.acs.org.
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