High-Speed in Situ X-ray Scattering of Carbon Nanotube Film Nucleation and Self-OrganizationClick to copy article linkArticle link copied!
- Eric R. Meshot
- Eric Verploegen
- Mostafa Bedewy
- Sameh Tawfick
- Arthur R. Woll
- Katherine S. Green
- Marianne Hromalik
- Lucas J. Koerner
- Hugh T. Philipp
- Mark W. Tate
- Sol M. Gruner
- A. John Hart
Abstract
The production of high-performance carbon nanotube (CNT) materials demands understanding of the growth behavior of individual CNTs as well as collective effects among CNTs. We demonstrate the first use of grazing incidence small-angle X-ray scattering to monitor in real time the synthesis of CNT films by chemical vapor deposition. We use a custom-built cold-wall reactor along with a high-speed pixel array detector resulting in a time resolution of 10 msec. Quantitative models applied to time-resolved X-ray scattering patterns reveal that the Fe catalyst film first rapidly dewets into well-defined hemispherical particles during heating in a reducing atmosphere, and then the particles coarsen slowly upon continued annealing. After introduction of the carbon source, the initial CNT diameter distribution closely matches that of the catalyst particles. However, significant changes in CNT diameter can occur quickly during the subsequent CNT self-organization process. Correlation of time-resolved orientation data to X-ray scattering intensity and height kinetics suggests that the rate of self-organization is driven by both the CNT growth rate and density, and vertical CNT growth begins abruptly when CNT alignment reaches a critical threshold. The dynamics of CNT size evolution and self-organization vary according to the catalyst annealing conditions and substrate temperature. Knowledge of these intrinsically rapid processes is vital to improve control of CNT structure and to enable efficient manufacturing of high-density arrays of long, straight CNTs.
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(11)
, 10589-10597. https://doi.org/10.1021/acsnano.3c01537
- Ahmed Aziz Ezzat, Mostafa Bedewy. Machine Learning for Revealing Spatial Dependence among Nanoparticles: Understanding Catalyst Film Dewetting via Gibbs Point Process Models. The Journal of Physical Chemistry C 2020, 124
(50)
, 27479-27494. https://doi.org/10.1021/acs.jpcc.0c07765
- Jaegeun Lee, Moataz Abdulhafez, Mostafa Bedewy. Decoupling Catalyst Dewetting, Gas Decomposition, and Surface Reactions in Carbon Nanotube Forest Growth Reveals Dependence of Density on Nucleation Temperature. The Journal of Physical Chemistry C 2019, 123
(47)
, 28726-28738. https://doi.org/10.1021/acs.jpcc.9b07894
- Jennifer Carpena-Núñez, Jorge Anibal Boscoboinik, Sammy Saber, Rahul Rao, Jian-Qiang Zhong, Matthew R. Maschmann, Piran R. Kidambi, Nicholas T. Dee, Dmitri N. Zakharov, A. John Hart, Eric A. Stach, Benji Maruyama. Isolating the Roles of Hydrogen Exposure and Trace Carbon Contamination on the Formation of Active Catalyst Populations for Carbon Nanotube Growth. ACS Nano 2019, 13
(8)
, 8736-8748. https://doi.org/10.1021/acsnano.9b01382
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(12)
, 11756-11784. https://doi.org/10.1021/acsnano.8b06511
- Eric R. Meshot, Darwin W. Zwissler, Ngoc Bui, Tevye R. Kuykendall, Cheng Wang, Alexander Hexemer, Kuang Jen J. Wu, and Francesco Fornasiero . Quantifying the Hierarchical Order in Self-Aligned Carbon Nanotubes from Atomic to Micrometer Scale. ACS Nano 2017, 11
(6)
, 5405-5416. https://doi.org/10.1021/acsnano.6b08042
- Viswanath Balakrishnan, Mostafa Bedewy, Eric R. Meshot, Sebastian W. Pattinson, Erik S. Polsen, Fabrice Laye, Dmitri N. Zakharov, Eric A. Stach, and A. John Hart . Real-Time Imaging of Self-Organization and Mechanical Competition in Carbon Nanotube Forest Growth. ACS Nano 2016, 10
(12)
, 11496-11504. https://doi.org/10.1021/acsnano.6b07251
- Tao Li, Andrew J. Senesi, and Byeongdu Lee . Small Angle X-ray Scattering for Nanoparticle Research. Chemical Reviews 2016, 116
(18)
, 11128-11180. https://doi.org/10.1021/acs.chemrev.5b00690
- Mostafa Bedewy, B. Viswanath, Eric R. Meshot, Dmitri N. Zakharov, Eric A. Stach, and A. John Hart . Measurement of the Dewetting, Nucleation, and Deactivation Kinetics of Carbon Nanotube Population Growth by Environmental Transmission Electron Microscopy. Chemistry of Materials 2016, 28
(11)
, 3804-3813. https://doi.org/10.1021/acs.chemmater.6b00798
- Jinjing Li, Mostafa Bedewy, Alvin Orbaek White, Erik S. Polsen, Sameh Tawfick, and A. John Hart . Highly Consistent Atmospheric Pressure Synthesis of Carbon Nanotube Forests by Mitigation of Moisture Transients. The Journal of Physical Chemistry C 2016, 120
(20)
, 11277-11287. https://doi.org/10.1021/acs.jpcc.6b02878
- C. Ryan Oliver, Erik S. Polsen, Eric R. Meshot, Sameh Tawfick, Sei Jin Park, Mostafa Bedewy, and A. John Hart . Statistical Analysis of Variation in Laboratory Growth of Carbon Nanotube Forests and Recommendations for Improved Consistency. ACS Nano 2013, 7
(4)
, 3565-3580. https://doi.org/10.1021/nn400507y
- Ramakrishna Surya, Gordon L. Koerner, Taher Hajilounezhad, Kaveh Safavigerdini, Martin Spies, Prasad Calyam, Filiz Bunyak, Kannappan Palaniappan, Matthew R. Maschmann. CNT forest self-assembly insights from in-situ ESEM synthesis. Carbon 2024, 229 , 119439. https://doi.org/10.1016/j.carbon.2024.119439
- Seong Jae Kim, Sanha Kim. Transfer printing techniques enabled by advanced carbon nanomaterials. 2024, 117-144. https://doi.org/10.1016/B978-0-443-18845-9.00006-5
- Shohei SAKURAI, Mayu IIDA, Kosei OKUNUKI, Masahito KUSHIDA. Effect of the State of Catalytic Nanoparticles on the Growth of Vertically Aligned Carbon Nanotubes. IEICE Transactions on Electronics 2023, E106.C
(6)
, 208-213. https://doi.org/10.1587/transele.2022OMP0005
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- Cheol-Hun Lee, Seongmin Park, Won Bae Kim, Haemin Lee, Sung-Hyun Lee, Kun-Hong Lee. Effect of carbonaceous impurities released from regenerated quartz tubes on the growth of ultra-long carbon nanotube forests. Carbon 2020, 167 , 181-187. https://doi.org/10.1016/j.carbon.2020.06.020
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- Adam Pander, Takatsugu Onishi, Akimitsu Hatta, Hiroshi Furuta. Study of self-organized structure in carbon nanotube forest by fractal dimension and lacunarity analysis. Materials Characterization 2020, 160 , 110086. https://doi.org/10.1016/j.matchar.2019.110086
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(45-46)
, 2815-2823. https://doi.org/10.1557/adv.2018.429
- Gyula Eres, C.M. Rouleau, A.A. Puretzky, D.B. Geohegan, H. Wang. Cooperative Behavior in the Evolution of Alignment and Structure in Vertically Aligned Carbon-Nanotube Arrays Grown using Chemical Vapor Deposition. Physical Review Applied 2018, 10
(2)
https://doi.org/10.1103/PhysRevApplied.10.024010
- Mostafa Bedewy. Data-driven understanding of collective carbon nanotube growth by
in situ
characterization and nanoscale metrology. Journal of Materials Research 2017, 32
(1)
, 153-165. https://doi.org/10.1557/jmr.2016.498
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(16)
, 5222-5233. https://doi.org/10.1039/C6NR09802A
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(16)
, 3787-3800. https://doi.org/10.1039/C7GC01421J
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(12)
https://doi.org/10.1126/sciadv.1601660
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- J. D. Beard, K. E. Evans, O. R. Ghita. Fabrication of three dimensional layered vertically aligned carbon nanotube structures and their potential applications. RSC Advances 2015, 5
(126)
, 104458-104466. https://doi.org/10.1039/C5RA18048A
- M. De Volder, S. Park, S. Tawfick, A. J. Hart. Strain-engineered manufacturing of freeform carbon nanotube microstructures. Nature Communications 2014, 5
(1)
https://doi.org/10.1038/ncomms5512
- Ming Liu, Rong Xiang, Wu Cao, Haiqiang Zeng, Yuquan Su, Xuchun Gui, Tianzhun Wu, Shigeo Maruyama, Zikang Tang. Is it possible to enhance Raman scattering of single-walled carbon nanotubes by metal particles during chemical vapor deposition?. Carbon 2014, 80 , 311-317. https://doi.org/10.1016/j.carbon.2014.08.069
- Périne Landois, Mathieu Pinault, Mickaël Huard, Valérie Reita, Stéphan Rouzière, Pascale Launois, Martine Mayne-L'Hermite, Nedjma Bendiab. Structure in nascent carbon nanotubes revealed by spatially resolved Raman spectroscopy. Thin Solid Films 2014, 568 , 102-110. https://doi.org/10.1016/j.tsf.2014.07.016
- Eric R. Meshot, Zhouzhou Zhao, Wei Lu, A. John Hart. Self-ordering of small-diameter metal nanoparticles by dewetting on hexagonal mesh templates. Nanoscale 2014, 6
(17)
, 10106-10112. https://doi.org/10.1039/C4NR01501K
- Brian A. Collins, Felicia A. Bokel, Dean M. DeLongchamp. Organic Photovoltaic Morphology. 2014, 377-420. https://doi.org/10.1002/9783527656912.ch12
- Erik S. Polsen, Mostafa Bedewy, A. John Hart. Decoupled Control of Carbon Nanotube Forest Density and Diameter by Continuous‐Feed Convective Assembly of Catalyst Particles. Small 2013, 9
(15)
, 2564-2575. https://doi.org/10.1002/smll.201202878
- Mostafa Bedewy, A. John Hart. Mechanical coupling limits the density and quality of self-organized carbon nanotube growth. Nanoscale 2013, 5
(7)
, 2928. https://doi.org/10.1039/c3nr34067h
- Mostafa Bedewy, Eric R. Meshot, A. John Hart. Diameter-dependent kinetics of activation and deactivation in carbon nanotube population growth. Carbon 2012, 50
(14)
, 5106-5116. https://doi.org/10.1016/j.carbon.2012.06.051
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