Joint Experimental and Computational 17 O and 1 H Solid State NMR Study of Ba 2 In 2 O 4 (OH) 2 Structure and Dynamics
Abstract
Here, a structural characterization of the hydrated form of the brownmillerite-type phase Ba2In2O5, Ba2In2O4(OH)2, is reported using experimental multinuclear NMR spectroscopy and density functional theory (DFT) energy and GIPAW NMR calculations. When the oxygen ions from H2O fill the inherent O vacancies of the brownmillerite structure, one of the water protons remains in the same layer (O3) while the second proton is located in the neighboring layer (O2) in sites with partial occupancies, as previously demonstrated by Jayaraman et al. (Solid State Ionics 2004, 170, 25–32) using X-ray and neutron studies. Calculations of possible proton arrangements within the partially occupied layer of Ba2In2O4(OH)2 yield a set of low energy structures; GIPAW NMR calculations on these configurations yield 1H and 17O chemical shifts and peak intensity ratios, which are then used to help assign the experimental MAS NMR spectra. Three distinct 1H resonances in a 2:1:1 ratio are obtained experimentally, the most intense resonance being assigned to the proton in the O3 layer. The two weaker signals are due to O2 layer protons, one set hydrogen bonding to the O3 layer and the other hydrogen bonding alternately toward the O3 and O1 layers. 1H magnetization exchange experiments reveal that all threemore »
- Authors:
-
- Department of Chemistry, Stony Brook University, Stony Brook, New York 11794-3400, United States, Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, U.K.
- Department of Chemistry, University of Cambridge, Lensfield Road, Cambridge CB2 1EW, U.K.
- Department of Materials Science and Engineering, University of Wisconsin, Madison, Wisconsin 53706, United States
- Publication Date:
- Research Org.:
- Univ. of Houston, TX (United States); Brookhaven National Laboratory (BNL), Upton, NY (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC), Basic Energy Sciences (BES)
- OSTI Identifier:
- 1203820
- Alternate Identifier(s):
- OSTI ID: 1452841
- Grant/Contract Number:
- SC0001284; AC02-98CH10886
- Resource Type:
- Journal Article: Published Article
- Journal Name:
- Chemistry of Materials
- Additional Journal Information:
- Journal Name: Chemistry of Materials Journal Volume: 27 Journal Issue: 11; Journal ID: ISSN 0897-4756
- Publisher:
- American Chemical Society (ACS)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
Citation Formats
Dervişoğlu, Rıza, Middlemiss, Derek S., Blanc, Frédéric, Lee, Yueh-Lin, Morgan, Dane, and Grey, Clare P. Joint Experimental and Computational 17 O and 1 H Solid State NMR Study of Ba 2 In 2 O 4 (OH) 2 Structure and Dynamics. United States: N. p., 2015.
Web. doi:10.1021/acs.chemmater.5b00328.
Dervişoğlu, Rıza, Middlemiss, Derek S., Blanc, Frédéric, Lee, Yueh-Lin, Morgan, Dane, & Grey, Clare P. Joint Experimental and Computational 17 O and 1 H Solid State NMR Study of Ba 2 In 2 O 4 (OH) 2 Structure and Dynamics. United States. https://doi.org/10.1021/acs.chemmater.5b00328
Dervişoğlu, Rıza, Middlemiss, Derek S., Blanc, Frédéric, Lee, Yueh-Lin, Morgan, Dane, and Grey, Clare P. 2015.
"Joint Experimental and Computational 17 O and 1 H Solid State NMR Study of Ba 2 In 2 O 4 (OH) 2 Structure and Dynamics". United States. https://doi.org/10.1021/acs.chemmater.5b00328.
@article{osti_1203820,
title = {Joint Experimental and Computational 17 O and 1 H Solid State NMR Study of Ba 2 In 2 O 4 (OH) 2 Structure and Dynamics},
author = {Dervişoğlu, Rıza and Middlemiss, Derek S. and Blanc, Frédéric and Lee, Yueh-Lin and Morgan, Dane and Grey, Clare P.},
abstractNote = {Here, a structural characterization of the hydrated form of the brownmillerite-type phase Ba2In2O5, Ba2In2O4(OH)2, is reported using experimental multinuclear NMR spectroscopy and density functional theory (DFT) energy and GIPAW NMR calculations. When the oxygen ions from H2O fill the inherent O vacancies of the brownmillerite structure, one of the water protons remains in the same layer (O3) while the second proton is located in the neighboring layer (O2) in sites with partial occupancies, as previously demonstrated by Jayaraman et al. (Solid State Ionics 2004, 170, 25–32) using X-ray and neutron studies. Calculations of possible proton arrangements within the partially occupied layer of Ba2In2O4(OH)2 yield a set of low energy structures; GIPAW NMR calculations on these configurations yield 1H and 17O chemical shifts and peak intensity ratios, which are then used to help assign the experimental MAS NMR spectra. Three distinct 1H resonances in a 2:1:1 ratio are obtained experimentally, the most intense resonance being assigned to the proton in the O3 layer. The two weaker signals are due to O2 layer protons, one set hydrogen bonding to the O3 layer and the other hydrogen bonding alternately toward the O3 and O1 layers. 1H magnetization exchange experiments reveal that all three resonances originate from protons in the same crystallographic phase, the protons exchanging with each other above approximately 150 °C. Three distinct types of oxygen atoms are evident from the DFT GIPAW calculations bare oxygens (O), oxygens directly bonded to a proton (H-donor O), and oxygen ions that are hydrogen bonded to a proton (H-acceptor O). The 17O calculated shifts and quadrupolar parameters are used to assign the experimental spectra, the assignments being confirmed by 1H–17O double resonance experiments.},
doi = {10.1021/acs.chemmater.5b00328},
url = {https://www.osti.gov/biblio/1203820},
journal = {Chemistry of Materials},
issn = {0897-4756},
number = 11,
volume = 27,
place = {United States},
year = {Fri May 22 00:00:00 EDT 2015},
month = {Fri May 22 00:00:00 EDT 2015}
}
Web of Science
Works referenced in this record:
Temperature Dependence of 207 Pb MAS Spectra of Solid Lead Nitrate. An Accurate, Sensitive Thermometer for Variable-Temperature MAS
journal, October 1995
- Bielecki, Anthony; Burum, Douglas P.
- Journal of Magnetic Resonance, Series A, Vol. 116, Issue 2
High-temperature C1-gas fuel cells using proton-conducting solid electrolytes
journal, May 1989
- Iwahara, H.; Uchida, H.; Morimoto, K.
- Journal of Applied Electrochemistry, Vol. 19, Issue 3
Ba2In2O4(OH)2: Proton sites, disorder and vibrational properties
journal, December 2007
- Martinez, Jean-Raphaël; Mohn, Chris E.; Stølen, Svein
- Journal of Solid State Chemistry, Vol. 180, Issue 12
An Improved Broadband Decoupling Sequence for Liquid Crystals and Solids
journal, January 2000
- Fung, B. M.; Khitrin, A. K.; Ermolaev, Konstantin
- Journal of Magnetic Resonance, Vol. 142, Issue 1
Generalized Gradient Approximation Made Simple
journal, October 1996
- Perdew, John P.; Burke, Kieron; Ernzerhof, Matthias
- Physical Review Letters, Vol. 77, Issue 18, p. 3865-3868
Characterization of perovskite systems derived from Ba2In2O5Part II: The proton compounds Ba2In2(1−x)Ti2xO4+2x(OH)y [0≤x≤1; y≤2(1−x)]
journal, May 2004
- Jayaraman, V.; Magrez, A.; Caldes, M.
- Solid State Ionics, Vol. 170, Issue 1-2
Improved background suppression in 1H MAS NMR using composite pulses
journal, August 2012
- Odedra, Smita; Wimperis, Stephen
- Journal of Magnetic Resonance, Vol. 221
Recent advances in solid-state NMR spectroscopy of spin I = 1/2 nuclei
journal, January 2009
- Lesage, Anne
- Physical Chemistry Chemical Physics, Vol. 11, Issue 32
Protonic conduction in Ba2In2O5
journal, December 1995
- Zhang, G.
- Solid State Ionics, Vol. 82, Issue 3-4
Probing Cation and Vacancy Ordering in the Dry and Hydrated Yttrium-Substituted BaSnO 3 Perovskite by NMR Spectroscopy and First Principles Calculations: Implications for Proton Mobility
journal, August 2012
- Buannic, Lucienne; Blanc, Frédéric; Middlemiss, Derek S.
- Journal of the American Chemical Society, Vol. 134, Issue 35
Protonic conduction in acceptor-doped KTaO3 crystals
journal, January 1986
- Lee, W.; Nowick, A.; Boatner, L.
- Solid State Ionics, Vol. 18-19
Proton-Conducting Oxides
journal, August 2003
- Kreuer, K. D.
- Annual Review of Materials Research, Vol. 33, Issue 1, p. 333-359
Characterization of perovskite systems derived from Ba2In2O5Part I: the oxygen-deficient Ba2In2(1−x)Ti2xO5+x1−x (0≤x≤1) compounds
journal, May 2004
- Jayaraman, V.; Magrez, A.; Caldes, M.
- Solid State Ionics, Vol. 170, Issue 1-2
Characterization of hydrous species in minerals by high-speed proton MAS-NMR
journal, March 1988
- Yesinowski, James P.; Eckert, Hellmut.; Rossman, George R.
- Journal of the American Chemical Society, Vol. 110, Issue 5
Perovskite-Structured BaScO 2 (OH) as a Novel Proton Conductor: Heavily Hydrated Phase Obtained via Low-Temperature Synthesis
journal, April 2013
- Cervera, Rinlee B.; Miyoshi, Shogo; Oyama, Yukiko
- Chemistry of Materials, Vol. 25, Issue 9
The oxygen and proton conductor Ba2In2O5: Thermogravimetry of proton uptake
journal, December 1998
- Schober, T.
- Solid State Ionics, Vol. 113-115, Issue 1-2
17 O Magic Angle Spinning NMR Studies of Brønsted Acid Sites in Zeolites HY and HZSM-5
journal, January 2007
- Peng, Luming; Huo, Hua; Liu, Yun
- Journal of the American Chemical Society, Vol. 129, Issue 2
Carbon-13 nuclear magnetic resonance of polymers spinning at the magic angle
journal, February 1976
- Schaefer, Jacob; Stejskal, E. O.
- Journal of the American Chemical Society, Vol. 98, Issue 4
Phases in the System Ba2M2-xCuxO4+δ, M = In, Sc: Structure and Oxygen Stoichiometry
journal, November 1993
- Gregory, D. H.; Weller, M. T.
- Journal of Solid State Chemistry, Vol. 107, Issue 1
The combined neutron scattering and first-principles study of solid state protonic conductors
journal, December 2001
- Yildirim, T.; Reisner, B.; Udovic, T. J.
- Solid State Ionics, Vol. 145, Issue 1-4
Proton conduction in sintered oxides and its application to steam electrolysis for hydrogen production
journal, August 1981
- Iwahara, H.; Esaka, T.; Uchida, H.
- Solid State Ionics, Vol. 3-4
Phase transition in the oxygen and proton conductor Ba2In2O5 in humid atmospheres below 300°C
journal, August 1997
- Schober, T.; Friedrich, J.; Krug, F.
- Solid State Ionics, Vol. 99, Issue 1-2
An Investigation of Weak CH···O Hydrogen Bonds in Maltose Anomers by a Combination of Calculation and Experimental Solid-State NMR Spectroscopy
journal, July 2005
- Yates, Jonathan R.; Pham, Tran N.; Pickard, Chris J.
- Journal of the American Chemical Society, Vol. 127, Issue 29
Recent advances in experimental solid state NMR methodology for half-integer spin quadrupolar nuclei
journal, March 1999
- Smith, M.
- Progress in Nuclear Magnetic Resonance Spectroscopy, Vol. 34, Issue 2
Cation Disorder in Pyrochlore Ceramics: 89 Y MAS NMR and First-Principles Calculations
journal, October 2009
- Reader, Simon W.; Mitchell, Martin R.; Johnston, Karen E.
- The Journal of Physical Chemistry C, Vol. 113, Issue 43
All-electron magnetic response with pseudopotentials: NMR chemical shifts
journal, May 2001
- Pickard, Chris J.; Mauri, Francesco
- Physical Review B, Vol. 63, Issue 24
119 Sn MAS NMR and first-principles calculations for the investigation of disorder in stannate pyrochlores
journal, January 2011
- Mitchell, Martin R.; Reader, Simon W.; Johnston, Karen E.
- Phys. Chem. Chem. Phys., Vol. 13, Issue 2
Accurate First Principles Prediction of 17 O NMR Parameters in SiO 2 : Assignment of the Zeolite Ferrierite Spectrum
journal, January 2003
- Profeta, Mickael; Mauri, Francesco; Pickard, Chris J.
- Journal of the American Chemical Society, Vol. 125, Issue 2
A Thermometer for Nonspinning Solid-State NMR Spectroscopy
journal, October 2000
- Beckmann, Peter A.; Dybowski, Cecil
- Journal of Magnetic Resonance, Vol. 146, Issue 2
Ab initio study of structurally bound water at cation vacancy sites in Fe- and Al-oxyhydroxide materials
journal, August 2013
- Pinney, Nathan; Morgan, Dane
- Geochimica et Cosmochimica Acta, Vol. 114
1 H shielding anisotropy in Mg(OH) 2 : The isolated OH − group
journal, February 1988
- Sears, R. E. J.; Kaliaperumal, R.; Manogaran, S.
- The Journal of Chemical Physics, Vol. 88, Issue 4
matNMR: A flexible toolbox for processing, analyzing and visualizing magnetic resonance data in Matlab®
journal, July 2007
- van Beek, Jacco D.
- Journal of Magnetic Resonance, Vol. 187, Issue 1
Structural transformation of the oxygen and proton conductor Ba2In2O5 in humid air: an in-situ X-ray powder diffraction study
journal, January 1999
- Fischer, W.
- Solid State Ionics, Vol. 116, Issue 3-4
Solid-State MAS NMR Studies of Brønsted Acid Sites in Zeolite H-Mordenite
journal, May 2012
- Huo, Hua; Peng, Luming; Gan, Zhehong
- Journal of the American Chemical Society, Vol. 134, Issue 23
Thermodynamics of Al-substitution in Fe-oxyhydroxides
journal, November 2013
- Pinney, Nathan; Morgan, Dane
- Geochimica et Cosmochimica Acta, Vol. 120
Towards homonuclear J solid-state NMR correlation experiments for half-integer quadrupolar nuclei: experimental and simulated 11B MAS spin-echo dephasing and calculated 2JBB coupling constants for lithium diborate
journal, January 2011
- Barrow, Nathan S.; Yates, Jonathan R.; Feller, Steven A.
- Physical Chemistry Chemical Physics, Vol. 13, Issue 13
Combining Multinuclear High-Resolution Solid-State MAS NMR and Computational Methods for Resonance Assignment of Glutathione Tripeptide
journal, May 2012
- Sardo, Mariana; Siegel, Renée; Santos, Sérgio M.
- The Journal of Physical Chemistry A, Vol. 116, Issue 25
Oxide-ion and proton conducting electrolyte materials for clean energy applications: structural and mechanistic features
journal, January 2010
- Malavasi, Lorenzo; Fisher, Craig A. J.; Islam, M. Saiful
- Chemical Society Reviews, Vol. 39, Issue 11
Calculation of NMR chemical shifts for extended systems using ultrasoft pseudopotentials
journal, July 2007
- Yates, Jonathan R.; Pickard, Chris J.; Mauri, Francesco
- Physical Review B, Vol. 76, Issue 2
SIMPSON: A General Simulation Program for Solid-State NMR Spectroscopy
journal, December 2000
- Bak, Mads; Rasmussen, Jimmy T.; Nielsen, Niels Chr
- Journal of Magnetic Resonance, Vol. 147, Issue 2
Fast high-temperature proton transport in nonstoichiometric mixed perovskites
journal, July 1994
- Liang, K.; Du, Y.; Nowick, A.
- Solid State Ionics, Vol. 69, Issue 2
VESTA : a three-dimensional visualization system for electronic and structural analysis
journal, May 2008
- Momma, Koichi; Izumi, Fujio
- Journal of Applied Crystallography, Vol. 41, Issue 3
Short-range structure of the brownmillerite-type oxide Ba 2 In 2 O 5 and its hydrated proton-conducting form BaInO 3 H
journal, January 2014
- Bielecki, Johan; Parker, Stewart F.; Ekanayake, Dharshani
- J. Mater. Chem. A, Vol. 2, Issue 40
High Temperature Solid Electrolyte Fuel Cells Using Perovskite-Type Oxide Based on BaCeO[sub 3]
journal, January 1990
- Iwahara, H.
- Journal of The Electrochemical Society, Vol. 137, Issue 2
High-temperature protonic conduction in mixed perovskite ceramics
journal, May 1993
- Liang, K.; Nowick, A.
- Solid State Ionics, Vol. 61, Issue 1-3
Defects in Doped LaGaO 3 Anionic Conductors: Linking NMR Spectral Features, Local Environments, and Defect Thermodynamics
journal, November 2011
- Blanc, Frédéric; Middlemiss, Derek S.; Gan, Zhehong
- Journal of the American Chemical Society, Vol. 133, Issue 44
Defect, protons and conductivity in brownmillerite-structured Ba2In2O5
journal, March 1999
- Fisher, C.
- Solid State Ionics, Vol. 118, Issue 3-4
Complete 1H resonance assignment of β-maltose from 1H–1H DQ-SQ CRAMPS and 1H (DQ-DUMBO)–13C SQ refocused INEPT 2D solid-state NMR spectra and first principles GIPAW calculations
journal, January 2010
- Webber, Amy L.; Elena, Bénédicte; Griffin, John M.
- Physical Chemistry Chemical Physics, Vol. 12, Issue 26
Nuclear Double Resonance in the Rotating Frame
journal, December 1962
- Hartmann, S. R.; Hahn, E. L.
- Physical Review, Vol. 128, Issue 5
The Polar Phase of NaNbO 3 : A Combined Study by Powder Diffraction, Solid-State NMR, and First-Principles Calculations
journal, June 2010
- Johnston, Karen E.; Tang, Chiu C.; Parker, Julia E.
- Journal of the American Chemical Society, Vol. 132, Issue 25
High temperature proton conducting oxides and their applications to solid electrolyte fuel cells and steam electrolyzer for hydrogen production
journal, September 1988
- Iwahara, H.
- Solid State Ionics, Vol. 28-30
Year-2008 nuclear quadrupole moments
journal, August 2008
- Pyykkö, Pekka
- Molecular Physics, Vol. 106, Issue 16-18
Proton Distributions and Hydrogen Bonding in Crystalline and Glassy Hydrous Silicates and Related Inorganic Materials: Insights from High-Resolution Solid-State Nuclear Magnetic Resonance Spectroscopy
journal, December 2009
- Xue, Xianyu; Kanzaki, Masami
- Journal of the American Ceramic Society, Vol. 92, Issue 12
First principles methods using CASTEP
journal, January 2005
- Clark, Stewart J.; Segall, Matthew D.; Pickard, Chris J.
- Zeitschrift für Kristallographie - Crystalline Materials, Vol. 220, Issue 5/6
Solid-state NMR calculations for metal oxides and gallates: Shielding and quadrupolar parameters for perovskites and related phases
journal, May 2010
- Middlemiss, Derek S.; Blanc, Frédéric; Pickard, Chris J.
- Journal of Magnetic Resonance, Vol. 204, Issue 1
Joint experimental and computational 17O solid state NMR study of Brownmillerite Ba2In2O5
journal, January 2014
- Dervişoğlu, Rıza; Middlemiss, Derek S.; Blanc, Frédéric
- Physical Chemistry Chemical Physics, Vol. 16, Issue 6
The crystal structure of brownmillerite, Ca2FeAlO5
journal, December 1971
- Colville, A. A.; Geller, S.
- Acta Crystallographica Section B Structural Crystallography and Crystal Chemistry, Vol. 27, Issue 12