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NMR methods for characterizing the pore structures and hydrogen storage properties of microporous carbons.

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Date
2010-06-30
Authors
Anderson, Robert J
McNicholas, Thomas P
Kleinhammes, Alfred
Wang, Anmiao
Liu, Jie
Wu, Yue
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Abstract
(1)H NMR spectroscopy is used to investigate a series of microporous activated carbons derived from a poly(ether ether ketone) (PEEK) precursor with varying amounts of burnoff (BO). In particular, properties relevant to hydrogen storage are evaluated such as pore structure, average pore size, uptake, and binding energy. High-pressure NMR with in situ H(2) loading is employed with H(2) pressure ranging from 100 Pa to 10 MPa. An N(2)-cooled cryostat allows for NMR isotherm measurements at both room temperature ( approximately 290 K) and 100 K. Two distinct (1)H NMR peaks appear in the spectra which represent the gaseous H(2) in intergranular pores and the H(2) residing in micropores. The chemical shift of the micropore peak is observed to evolve with changing pressure, the magnitude of this effect being correlated to the amount of BO and therefore the structure. This is attributed to the different pressure dependence of the amount of adsorbed and non-adsorbed molecules within micropores, which experience significantly different chemical shifts due to the strong distance dependence of the ring current effect. In pores with a critical diameter of 1.2 nm or less, no pressure dependence is observed because they are not wide enough to host non-adsorbed molecules; this is the case for samples with less than 35% BO. The largest estimated pore size that can contribute to the micropore peak is estimated to be around 2.4 nm. The total H(2) uptake associated with pores of this size or smaller is evaluated via a calibration of the isotherms, with the highest amount being observed at 59% BO. Two binding energies are present in the micropores, with the lower, more dominant one being on the order of 5 kJ mol(-1) and the higher one ranging from 7 to 9 kJ mol(-1).
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Journal article
Permalink
https://hdl.handle.net/10161/4054
Published Version (Please cite this version)
10.1021/ja9109924
Publication Info
Anderson, Robert J; McNicholas, Thomas P; Kleinhammes, Alfred; Wang, Anmiao; Liu, Jie; & Wu, Yue (2010). NMR methods for characterizing the pore structures and hydrogen storage properties of microporous carbons. J Am Chem Soc, 132(25). pp. 8618-8626. 10.1021/ja9109924. Retrieved from https://hdl.handle.net/10161/4054.
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Scholars@Duke

Liu

Jie Liu

George Barth Geller Distinguished Professor of Chemistry
Dr. Liu’s research interests are focusing on the chemistry and material science of nanoscale materials. Specific topics in his current research program include: Self-assembly of nanostructures; Preparation and chemical functionalization of single walled carbon nanotubes; Developing carbon nanotube based chemical and biological sensors; SPM based fabrication and modification of functional nanostructures.
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