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

Journal Article · · Carbon

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.

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
Alternate ID(s):
OSTI ID: 1505848
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 journal May 1980
Synthesis of a Large-Scale Highly Ordered Porous Carbon Film by Self-Assembly of Block Copolymers journal November 2004
Ordered Mesoporous Polymers and Homologous Carbon Frameworks: Amphiphilic Surfactant Templating and Direct Transformation 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 journal February 2007
A Low-Concentration Hydrothermal Synthesis of Biocompatible Ordered Mesoporous Carbon Nanospheres with Tunable and Uniform Size journal September 2010
Magnetic Susceptibility Effects on 13C MAS NMR Spectra of Carbon Materials and Graphite journal August 2001
Quantitative reliability of aromaticity and related measurements on coals by 13C n.m.r. A debate journal May 1989
Quantitative 13C n.m.r. characterization of aqueous formaldehyde resins: 2. Resorcinol-formaldehyde resins journal May 1986
Solid-state 13C NMR study of neutral insulating and electrochemically doped conducting poly (p-phenylene vinylene) journal March 1989
Control of mesoporous structure of organic and carbon aerogels journal September 1998
Formation and fate of PAH during the pyrolysis and fuel-rich combustion of coal primary tar journal November 2000
Polycyclic aromatic hydrocarbons from the pyrolysis of catechol (ortho-dihydroxybenzene), a model fuel representative of entities in tobacco, coal, and lignin journal October 2001
Synthesis of ordered mesoporous carbon molecular sieves CMK-1 journal April 2001
KOH activation of mesoporous carbons obtained by soft-templating journal July 2008
Ordered mesoporous Fe (or Co)–N–graphitic carbons as excellent non-precious-metal electrocatalysts for oxygen reduction journal November 2014
Comparative study of carbon dioxide and nitrogen atmospheric effects on the chemical structure changes during pyrolysis of phenol–formaldehyde spheres journal June 2004
Microenvironmental and conformational structure of triblock copolymers in aqueous solution by 1H and 13C NMR spectroscopy journal July 2006
Ammonia-activated mesoporous carbon membranes for gas separations journal February 2011
The pyrolysis mechanism of phenol formaldehyde resin journal August 2012
Spectral editing in 13C solid-state NMR at high magnetic field using fast MAS and spin-echo dephasing journal October 2012
Thermal reactions and properties of polycyclic aromatic hydrocarbons journal November 1991
Synthesis of Polyacrylonitrile-Based Ordered Mesoporous Carbon with Tunable Pore Structures journal January 2004
A Family of Highly Ordered Mesoporous Polymer Resin and Carbon Structures from Organic−Organic Self-Assembly journal September 2006
An Aqueous Cooperative Assembly Route To Synthesize Ordered Mesoporous Carbons with Controlled Structures and Morphology September 2006
Carbon-13 solid-state NMR of Argonne-premium coals journal March 1989
Determination of the Average Aromatic Cluster Size of Fossil Fuels by Solid-State NMR at High Magnetic Field journal February 2013
Selection of nonprotonated carbon resonances in solid-state nuclear magnetic resonance journal September 1979
The Determination of Pore Volume and Area Distributions in Porous Substances. I. Computations from Nitrogen Isotherms journal January 1951
Adsorption of Gases in Multimolecular Layers journal February 1938
Synthesis of Mesoporous Carbon Materials via Enhanced Hydrogen-Bonding Interaction journal April 2006
Synthesis of Highly Ordered Carbon Molecular Sieves via Template-Mediated Structural Transformation 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 journal July 2008
Structurally Ordered Mesoporous Carbon Nanoparticles as Transmembrane Delivery Vehicle in Human Cancer Cells journal November 2008
Ordered nanoporous arrays of carbon supporting high dispersions of platinum nanoparticles journal July 2001
Wall thickness determination of hydrophobically functionalized MCM-41 materials journal January 2012
A facile photo-induced synthesis of COOH functionalized meso-macroporous carbon films and their excellent sensing capability for aromatic amines journal January 2012
Hierarchical mesoporous/microporous carbon with graphitized frameworks for high-performance lithium-ion batteries journal November 2014

Cited By (3)

A Porous Carbon with Excellent Gas Storage Properties from Waste Polystyrene journal May 2019
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 journal November 2018
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