Fast MAS 1H NMR Study of Water Adsorption and Dissociation on the (100) Surface of Ceria Nanocubes: A Fully Hydroxylated, Hydrophobic Ceria Surface

Gill, Lance; Beste, Ariana; Chen, Banghao; Li, Meijun; Mann, Amanda K.  P.; Overbury, Steven H.; Hagaman, Edward W.

doi:10.1021/acs.jpcc.6b12375

Title: Fast MAS ¹H NMR Study of Water Adsorption and Dissociation on the (100) Surface of Ceria Nanocubes: A Fully Hydroxylated, Hydrophobic Ceria Surface

Journal Article · Wed Mar 22 00:00:00 EDT 2017 · Journal of Physical Chemistry. C

DOI:https://doi.org/10.1021/acs.jpcc.6b12375· OSTI ID:1364294

Gill, Lance ^[1]; Beste, Ariana ^[2]; Chen, Banghao ^[1]; Li, Meijun ^[1]; Mann, Amanda K. P. ^[1]; Overbury, Steven H. ^[1];

^[1]

Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Chemical Sciences Division
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States). Joint Institute for Computational Sciences (JIBS) ; Univ. of Tennessee, Knoxville, TN (United States)

¹H nuclear magnetic resonance (NMR) spectroscopy was used to study hydroxylic surface species on ceria nanocubes, a crystalline, high-surface-area CeO₂ that presents mostly (100) facets. Water adsorption and desorption experiments in combination with fast magic angle spinning (MAS, 20–40 kHz) 1H NMR provide high-resolution ¹H spectra that allow the observation of ten resonance bands (water or hydroxyl) on or under the (100) surface. Assignments were made using a combination of adsorption and temperature-programmed desorption, quantitative spin counting, deuterium exchange, spin–lattice (T₁) and spin–spin (T₂) relaxation, and DFT calculations. In air, the (100) surface exists as a fully hydroxylated surface. Water adsorption and dissociation on dry ceria surfaces occur first at oxygen vacancies, but Ce³⁺ centers are not required since water dissociation is barrier-less on the fully oxidized surface. Surface $$-$$OH functionality occurs in two resolved bands representing isolated $$-$$OH (1 ppm) and hydrogen-bonded $$-$$OH (9 ppm), the latter being dominant. Deuterium exchange of surface hydroxyls with D₂O does not occur under mild or forcing conditions. Despite large differences in the T₁ of surface hydroxyls and physisorbed water, surface hydroxyl T₁ values are independent of the presence or absence of physisorbed water, demonstrating that the protons within these two functional group pools are not in intimate contact. These observations show that, once hydroxylated, the surface $$-$$OH functionality preferentially forms hydrogen bonds with surface lattice oxygen, i.e., the hydroxylated (100) surface of ceria is hydrophobic. Near this surface it is energetically more favorable for physisorbed water to hydrogen bond to itself rather than to the surface. DFT calculations support this notion. Impurity Na⁺ remaining in incompletely washed ceria nanocubes increases the surface hydrophilicity. In conclusion, sharp, low-field resonances observed in spectra of noncalcined nanocubes arise from kinetically trapped subsurface $$-$$OH.

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Research Organization:: Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC05-00OR22725; AC02-05CH11231

OSTI ID:: 1364294

Journal Information:: Journal of Physical Chemistry. C, Vol. 121, Issue 13; ISSN 1932-7447

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 22 works

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Title: Fast MAS ¹H NMR Study of Water Adsorption and Dissociation on the (100) Surface of Ceria Nanocubes: A Fully Hydroxylated, Hydrophobic Ceria Surface