Quantitative atomic-scale structure characterization of ordered mesoporous carbon materials by solid state NMR

Wang, Zhuoran; Opembe, Naftali; Kobayashi, Takeshi; Nelson, Nicholas C.; Slowing, Igor I.; Pruski, Marek

doi:10.1016/j.carbon.2018.01.087

Title: Quantitative atomic-scale structure characterization of ordered mesoporous carbon materials by solid state NMR

Journal Article · Sat Feb 03 04:00:00 UTC 2018 · Carbon

DOI: https://doi.org/10.1016/j.carbon.2018.01.087 · OSTI ID:1427734

Wang, Zhuoran ^[1];

^[2]; Kobayashi, Takeshi ^[2];

^[1]; Slowing, Igor I. ^[1];

^[1]

Iowa State Univ., Ames, IA (United States). Department of Chemistry; Ames Lab., Ames, IA (United States)
Ames Lab. and Iowa State Univ., Ames, IA (United States)

In this study, solid-state (SS)NMR techniques were applied to characterize the atomic-scale structures of ordered mesoporous carbon (OMC) materials prepared using Pluronic F127 as template with resorcinol and formaldehyde as polymerizing precursors. A rigorous quantitative analysis was developed using a combination of ¹³C SSNMR spectra acquired with direct polarization and cross polarization on natural abundant and selectively ¹³C-enriched series of samples pyrolyzed at various temperatures. These experiments identified and counted the key functional groups present in the OMCs at various stages of preparation and thermal treatment. Lastly, the chemical evolution of molecular networks, the average sizes of aromatic clusters and the extended molecular structures of OMCs were then inferred by coupling this information with the elemental analysis results.

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Research Organization:: Ames Laboratory (AMES), Ames, IA (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES) (SC-22). Chemical Sciences, Geosciences & Biosciences Division

Grant/Contract Number:: AC02-07CH11358

OSTI ID:: 1427734

Report Number(s):: IS-J--9597; PII: S0008622318300964

Journal Information:: Carbon, Journal Name: Carbon Journal Issue: C Vol. 131; ISSN 0008-6223

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

References (37)

Thermal Degradation of Polymers to Polymeric Carbon—An Approach to the Synthesis of New Materials Fitzer, Erich Angewandte Chemie International Edition in English, Vol. 19, Issue 5 https://doi.org/10.1002/anie.198003751	journal	May 1980
Synthesis of a Large-Scale Highly Ordered Porous Carbon Film by Self-Assembly of Block Copolymers Liang, Chengdu; Hong, Kunlun; Guiochon, Georges A. Angewandte Chemie International Edition, Vol. 43, Issue 43, p. 5785-5789 https://doi.org/10.1002/anie.200461051	journal	November 2004
Ordered Mesoporous Polymers and Homologous Carbon Frameworks: Amphiphilic Surfactant Templating and Direct Transformation Meng, Yan; Gu, Dong; Zhang, Fuqiang Angewandte Chemie International Edition, Vol. 44, Issue 43, p. 7053-7059 https://doi.org/10.1002/anie.200501561	journal	November 2005
Formation of Mesoporous Carbon With a Face-Centered-CubicFdm Structure and Bimodal Architectural Pores From the Reverse Amphiphilic Triblock Copolymer PPO-PEO-PPO Huang, Yan; Cai, Huaqiang; Yu, Ting Angewandte Chemie International Edition, Vol. 46, Issue 7, p. 1089-1093 https://doi.org/10.1002/anie.200603665	journal	February 2007
A Low-Concentration Hydrothermal Synthesis of Biocompatible Ordered Mesoporous Carbon Nanospheres with Tunable and Uniform Size Fang, Yin; Gu, Dong; Zou, Ying Angewandte Chemie International Edition, Vol. 49, Issue 43 https://doi.org/10.1002/anie.201002849	journal	September 2010
Magnetic Susceptibility Effects on 13C MAS NMR Spectra of Carbon Materials and Graphite Freitas, Jair C. C.; Emmerich, Francisco G.; Cernicchiaro, Geraldo R. C. Solid State Nuclear Magnetic Resonance, Vol. 20, Issue 1-2 https://doi.org/10.1006/snmr.2001.0030	journal	August 2001
Quantitative reliability of aromaticity and related measurements on coals by 13C n.m.r. A debate Snape, C.; Axelson, D.; Botto, R. Fuel, Vol. 68, Issue 5 https://doi.org/10.1016/0016-2361(89)90142-7	journal	May 1989
Quantitative 13C n.m.r. characterization of aqueous formaldehyde resins: 2. Resorcinol-formaldehyde resins Werstler, D. D. Polymer, Vol. 27, Issue 5 https://doi.org/10.1016/0032-3861(86)90136-9	journal	May 1986
Solid-state 13C NMR study of neutral insulating and electrochemically doped conducting poly (p-phenylene vinylene) Grobelny, J.; Obrzut, J.; Karasz, F. E. Synthetic Metals, Vol. 29, Issue 1 https://doi.org/10.1016/0379-6779(89)90282-8	journal	March 1989
Control of mesoporous structure of organic and carbon aerogels Tamon, H.; Ishizaka, H.; Araki, T. Carbon, Vol. 36, Issue 9 https://doi.org/10.1016/S0008-6223(97)00202-9	journal	September 1998
Formation and fate of PAH during the pyrolysis and fuel-rich combustion of coal primary tar Ledesma, E. B.; Kalish, M. A.; Nelson, P. F. Fuel, Vol. 79, Issue 14 https://doi.org/10.1016/S0016-2361(00)00044-2	journal	November 2000
Polycyclic aromatic hydrocarbons from the pyrolysis of catechol (ortho-dihydroxybenzene), a model fuel representative of entities in tobacco, coal, and lignin Wornat, Mary J.; Ledesma, Elmer B.; Marsh, Nathan D. Fuel, Vol. 80, Issue 12 https://doi.org/10.1016/S0016-2361(01)00057-6	journal	October 2001
Synthesis of ordered mesoporous carbon molecular sieves CMK-1 Joo, Sang Hoon; Jun, Shinae; Ryoo, Ryong Microporous and Mesoporous Materials, Vol. 44-45 https://doi.org/10.1016/S1387-1811(01)00179-2	journal	April 2001
KOH activation of mesoporous carbons obtained by soft-templating Górka, Joanna; Zawislak, Aleksandra; Choma, Jerzy Carbon, Vol. 46, Issue 8, p. 1159-1161 https://doi.org/10.1016/j.carbon.2008.03.024	journal	July 2008
Ordered mesoporous Fe (or Co)–N–graphitic carbons as excellent non-precious-metal electrocatalysts for oxygen reduction Kong, Aiguo; Kong, Yingying; Zhu, Xiaofang Carbon, Vol. 78 https://doi.org/10.1016/j.carbon.2014.06.047	journal	November 2014
Comparative study of carbon dioxide and nitrogen atmospheric effects on the chemical structure changes during pyrolysis of phenol–formaldehyde spheres Kim, Young Jeon; Kim, Myung Il; Yun, Chang Hun Journal of Colloid and Interface Science, Vol. 274, Issue 2 https://doi.org/10.1016/j.jcis.2003.12.029	journal	June 2004
Microenvironmental and conformational structure of triblock copolymers in aqueous solution by 1H and 13C NMR spectroscopy Ma, Junhe; Guo, Chen; Tang, Yalin Journal of Colloid and Interface Science, Vol. 299, Issue 2 https://doi.org/10.1016/j.jcis.2006.02.021	journal	July 2006
Ammonia-activated mesoporous carbon membranes for gas separations Mahurin, Shannon M.; Lee, Je Seung; Wang, Xiqing Journal of Membrane Science, Vol. 368, Issue 1-2 https://doi.org/10.1016/j.memsci.2010.11.007	journal	February 2011
The pyrolysis mechanism of phenol formaldehyde resin Jiang, Haiyun; Wang, Jigang; Wu, Shenqing Polymer Degradation and Stability, Vol. 97, Issue 8 https://doi.org/10.1016/j.polymdegradstab.2012.04.016	journal	August 2012
Spectral editing in 13C solid-state NMR at high magnetic field using fast MAS and spin-echo dephasing Mao, Kanmi; Kennedy, Gordon J.; Althaus, Stacey M. Solid State Nuclear Magnetic Resonance, Vol. 47-48 https://doi.org/10.1016/j.ssnmr.2012.07.003	journal	October 2012
Thermal reactions and properties of polycyclic aromatic hydrocarbons Stein, Stephen E. Accounts of Chemical Research, Vol. 24, Issue 11 https://doi.org/10.1021/ar00011a005	journal	November 1991
Synthesis of Polyacrylonitrile-Based Ordered Mesoporous Carbon with Tunable Pore Structures Lu, Anhui; Kiefer, Andreas; Schmidt, Wolfgang Chemistry of Materials, Vol. 16, Issue 1 https://doi.org/10.1021/cm031095h	journal	January 2004
A Family of Highly Ordered Mesoporous Polymer Resin and Carbon Structures from Organic−Organic Self-Assembly Meng, Yan; Gu, Dong; Zhang, Fuqiang Chemistry of Materials, Vol. 18, Issue 18 https://doi.org/10.1021/cm060921u	journal	September 2006
An Aqueous Cooperative Assembly Route To Synthesize Ordered Mesoporous Carbons with Controlled Structures and Morphology Zhang, Fuqiang; Meng, Yan; Gu, Dong Chemistry of Materials, Vol. 18, Issue 22, p. 5279-5288 https://doi.org/10.1021/cm061400+		September 2006
Carbon-13 solid-state NMR of Argonne-premium coals Solum, Mark S.; Pugmire, Ronald J.; Grant, David M. Energy & Fuels, Vol. 3, Issue 2 https://doi.org/10.1021/ef00014a012	journal	March 1989
Determination of the Average Aromatic Cluster Size of Fossil Fuels by Solid-State NMR at High Magnetic Field Mao, Kanmi; Kennedy, Gordon J.; Althaus, Stacey M. Energy & Fuels, Vol. 27, Issue 2 https://doi.org/10.1021/ef301804p	journal	February 2013
Selection of nonprotonated carbon resonances in solid-state nuclear magnetic resonance Opella, S. J.; Frey, M. H. Journal of the American Chemical Society, Vol. 101, Issue 19 https://doi.org/10.1021/ja00513a079	journal	September 1979
The Determination of Pore Volume and Area Distributions in Porous Substances. I. Computations from Nitrogen Isotherms Barrett, Elliott P.; Joyner, Leslie G.; Halenda, Paul P. Journal of the American Chemical Society, Vol. 73, Issue 1 https://doi.org/10.1021/ja01145a126	journal	January 1951
Adsorption of Gases in Multimolecular Layers Brunauer, Stephen; Emmett, P. H.; Teller, Edward Journal of the American Chemical Society, Vol. 60, Issue 2, p. 309-319 https://doi.org/10.1021/ja01269a023	journal	February 1938
Synthesis of Mesoporous Carbon Materials via Enhanced Hydrogen-Bonding Interaction Liang, Chengdu; Dai, Sheng Journal of the American Chemical Society, Vol. 128, Issue 16, p. 5316-5317 https://doi.org/10.1021/ja060242k	journal	April 2006
Synthesis of Highly Ordered Carbon Molecular Sieves via Template-Mediated Structural Transformation Ryoo, Ryong; Joo, Sang Hoon; Jun, Shinae The Journal of Physical Chemistry B, Vol. 103, Issue 37 https://doi.org/10.1021/jp991673a	journal	September 1999
Facile Synthesis of Ordered Mesoporous Carbons with High Thermal Stability by Self-Assembly of Resorcinol−Formaldehyde and Block Copolymers under Highly Acidic Conditions Wang, Xiqing; Liang, Chengdu; Dai, Sheng Langmuir, Vol. 24, Issue 14, p. 7500-7505 https://doi.org/10.1021/la800529v	journal	July 2008
Structurally Ordered Mesoporous Carbon Nanoparticles as Transmembrane Delivery Vehicle in Human Cancer Cells Kim, Tae-Wan; Chung, Po-Wen; Slowing, Igor I. Nano Letters, Vol. 8, Issue 11, p. 3724-3727 https://doi.org/10.1021/nl801976m	journal	November 2008
Ordered nanoporous arrays of carbon supporting high dispersions of platinum nanoparticles Joo, Sang Hoon; Choi, Seong Jae; Oh, Ilwhan Nature, Vol. 412, Issue 6843 https://doi.org/10.1038/35084046	journal	July 2001
Wall thickness determination of hydrophobically functionalized MCM-41 materials Schoeffel, Markus; Brodie–Linder, Nancy; Audonnet, Fabrice J. Mater. Chem., Vol. 22, Issue 2 https://doi.org/10.1039/C1JM11578B	journal	January 2012
A facile photo-induced synthesis of COOH functionalized meso-macroporous carbon films and their excellent sensing capability for aromatic amines Jia, Lichao; Mane, Gurudas P.; Anand, Chokkalingam Chemical Communications, Vol. 48, Issue 72 https://doi.org/10.1039/c2cc33651k	journal	January 2012
Hierarchical mesoporous/microporous carbon with graphitized frameworks for high-performance lithium-ion batteries Lv, Yingying; Wu, Zhangxiong; Fang, Yin APL Materials, Vol. 2, Issue 11 https://doi.org/10.1063/1.4897201	journal	November 2014

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Ni Prussian Blue Analogue/Mesoporous Carbon Composite as Electrode Material for Aqueous K-Ion Energy Storage: Effect of Carbon-Framework Interaction on Its Electrochemical Behavior Vázquez-Samperio, Juvencio; Sánchez-Padilla, N. M.; Acevedo-Peña, Próspero ChemistrySelect, Vol. 3, Issue 41 https://doi.org/10.1002/slct.201801333	journal	November 2018
Magic angle spinning spheres Chen, Pinhui; Albert, Brice J.; Gao, Chukun Science Advances, Vol. 4, Issue 9 https://doi.org/10.1126/sciadv.aau1540	journal	September 2018
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