Characterization of Isolated Ga3+ Cations in Ga/H-MFI Prepared by Vapor-Phase Exchange of H-MFI Zeolite with GaCl3
Abstract
Ga/H-MFI was prepared by vapor-phase reaction of GaCl3 with Brønsted acid O-H groups in dehydrated H-MFI zeolite. The resulting [GaCl2]+ cations in the as-exchanged zeolite are treated in H2 at 823 K to stoichiometrically remove Cl ligands and form [GaH2]+ cations. Subsequent oxidation in O2 and characterization by IR spectroscopy and NH3-temperature-programmed desorption (TPD) suggests that, for Ga/Al ratios ≤0.3, Ga3+ exists predominantly as [Ga(OH)2]+-H+ cation pairs and to a lesser degree as [Ga(OH)]2+ cations at low Ga/Al ratios (~0.1); while both species are associated with proximate cation-exchange sites, calculated free energies of formation suggest that [Ga(OH)]2+ cations are more stable on cation-exchange sites associated with NNN (next-nearest neighbor) framework Al atoms than on those associated with NNNN (next-next-nearest neighbor) framework Al atoms. Ga K-edge X-ray Absorption Near Edge Spectroscopy (XANES) measurements indicate that, under oxidizing conditions and for all Ga/Al ratios, all Ga species are in the +3 oxidation state and are tetrahedrally coordinated to 4 O atoms. Fourier analysis of Ga K-edge Extended X-ray Absorption Fine Structure (EXAFS) data supports the conclusion that Ga3+ is present predominantly as [Ga(OH)2]+ cations (or [Ga(OH)2]+-H+ cation pairs). For Ga/Al ratios ≤0.3, wavelet analysis of EXAFS data provide evidence for backscattering frommore »
- Authors:
-
[1];
[3];
[1]
- Univ. of California, Berkeley, CA (United States). Dept. of Chemical and Biomolecular Engineering
- Ford Motor Company, Dearborn, MI (United States). Chemical Engineering Dept.
- Univ. of California, Berkeley, CA (United States). Dept. of Chemistry
- Publication Date:
- Research Org.:
- Lawrence Berkeley National Laboratory (LBNL), Berkeley, CA (United States)
- Sponsoring Org.:
- USDOE Office of Science (SC)
- OSTI Identifier:
- 1571105
- Grant/Contract Number:
- AC02-05CH11231
- Resource Type:
- Accepted Manuscript
- Journal Name:
- ACS Catalysis
- Additional Journal Information:
- Journal Volume: 8; Journal Issue: 7; Journal ID: ISSN 2155-5435
- Publisher:
- American Chemical Society (ACS)
- Country of Publication:
- United States
- Language:
- English
- Subject:
- 37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; gallium; cation-exchanged zeolites; vapor-phase ion exchange; X-ray absorption spectroscopy; heterogeneous catalysts; catalyst characterization; alkane dehydrogenation
Citation Formats
Phadke, Neelay M., Van der Mynsbrugge, Jeroen, Mansoor, Erum, Getsoian, Andrew Bean, Head-Gordon, Martin, and Bell, Alexis T. Characterization of Isolated Ga3+ Cations in Ga/H-MFI Prepared by Vapor-Phase Exchange of H-MFI Zeolite with GaCl3. United States: N. p., 2018.
Web. doi:10.1021/acscatal.8b01254.
Phadke, Neelay M., Van der Mynsbrugge, Jeroen, Mansoor, Erum, Getsoian, Andrew Bean, Head-Gordon, Martin, & Bell, Alexis T. Characterization of Isolated Ga3+ Cations in Ga/H-MFI Prepared by Vapor-Phase Exchange of H-MFI Zeolite with GaCl3. United States. https://doi.org/10.1021/acscatal.8b01254
Phadke, Neelay M., Van der Mynsbrugge, Jeroen, Mansoor, Erum, Getsoian, Andrew Bean, Head-Gordon, Martin, and Bell, Alexis T. Mon .
"Characterization of Isolated Ga3+ Cations in Ga/H-MFI Prepared by Vapor-Phase Exchange of H-MFI Zeolite with GaCl3". United States. https://doi.org/10.1021/acscatal.8b01254. https://www.osti.gov/servlets/purl/1571105.
@article{osti_1571105,
title = {Characterization of Isolated Ga3+ Cations in Ga/H-MFI Prepared by Vapor-Phase Exchange of H-MFI Zeolite with GaCl3},
author = {Phadke, Neelay M. and Van der Mynsbrugge, Jeroen and Mansoor, Erum and Getsoian, Andrew Bean and Head-Gordon, Martin and Bell, Alexis T.},
abstractNote = {Ga/H-MFI was prepared by vapor-phase reaction of GaCl3 with Brønsted acid O-H groups in dehydrated H-MFI zeolite. The resulting [GaCl2]+ cations in the as-exchanged zeolite are treated in H2 at 823 K to stoichiometrically remove Cl ligands and form [GaH2]+ cations. Subsequent oxidation in O2 and characterization by IR spectroscopy and NH3-temperature-programmed desorption (TPD) suggests that, for Ga/Al ratios ≤0.3, Ga3+ exists predominantly as [Ga(OH)2]+-H+ cation pairs and to a lesser degree as [Ga(OH)]2+ cations at low Ga/Al ratios (~0.1); while both species are associated with proximate cation-exchange sites, calculated free energies of formation suggest that [Ga(OH)]2+ cations are more stable on cation-exchange sites associated with NNN (next-nearest neighbor) framework Al atoms than on those associated with NNNN (next-next-nearest neighbor) framework Al atoms. Ga K-edge X-ray Absorption Near Edge Spectroscopy (XANES) measurements indicate that, under oxidizing conditions and for all Ga/Al ratios, all Ga species are in the +3 oxidation state and are tetrahedrally coordinated to 4 O atoms. Fourier analysis of Ga K-edge Extended X-ray Absorption Fine Structure (EXAFS) data supports the conclusion that Ga3+ is present predominantly as [Ga(OH)2]+ cations (or [Ga(OH)2]+-H+ cation pairs). For Ga/Al ratios ≤0.3, wavelet analysis of EXAFS data provide evidence for backscattering from nearest neighboring O atoms and from next-nearest neighboring framework Al atoms. For Ga/Al > 0.3, backscattering from next-nearest neighboring Ga atoms is also evident, characteristic of GaOx species. Here, upon reduction in H2, the oxidized Ga3+ species produce [Ga(OH)H]+-H+ cation pairs, [GaH2]+-H+ cation pairs, and [GaH]2+ cations. Computed phase diagrams indicate that the thermodynamic stability of the reduced Ga3+ species depends sensitively on temperature, Al-Al interatomic distance, and H2 and H2O partial pressures. For Ga/Al ratios ≤0.2, it is concluded that [GaH2]+-H+ cation pairs and [GaH]2+ cations are the predominant species present in Ga/H-MFI reduced above 673 K in 105Pa H2 and in the absence of water vapor.},
doi = {10.1021/acscatal.8b01254},
journal = {ACS Catalysis},
number = 7,
volume = 8,
place = {United States},
year = {Mon May 21 00:00:00 EDT 2018},
month = {Mon May 21 00:00:00 EDT 2018}
}
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