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Title: An in-situ cell for characterization of solids by soft X-rayabsorption

Abstract

An in-situ cell using ''lab-on-a-chip'' technologies has been designed and tested for characterization of catalysts and environmental materials using soft X-ray absorption spectroscopy and spectromicroscopy at photon energies above 250 eV. The sample compartment is 1.0 mm in diameter with a gas path length of 0.8 mm to minimize X-ray absorption in the gas phase. The sample compartment can be heated to 533 K by an Al resistive heater and gas flows up to 5.0 cm{sup 3} min{sup -1} can be supplied to the sample compartment through microchannels. The performance of the cell was tested by acquiring Cu L{sub 3}-edge XANES data during the reduction and oxidation of a silica-supported Cu catalyst using the beam line 11.0.2 Scanning Transmission X-ray Microscope (STXM) at the Advanced Light Source of LBNL. Two-dimensional images of individual catalyst particles were recorded at photon energies between 926 eV and 937 eV, the energy range in which the Cu(II) and Cu(I) L{sub 3} absorption edges are observed. Oxidation state specific images of the catalyst clearly show the disappearance of Cu(II) species during the exposure of the oxidized sample to 4% CO in He while increasing the temperature from 308 K to 473 K. Reoxidation restores themore » intensity of the image associated with Cu(II). L-edge XANES spectra obtained from stacks of STXM images show that with increasing temperature the Cu(II) peak intensity decreases as the Cu(I) peak intensity increases.« less

Authors:
; ; ; ; ; ; ;
Publication Date:
Research Org.:
Ernest Orlando Lawrence Berkeley NationalLaboratory, Berkeley, CA (US)
Sponsoring Org.:
USDOE Director. Office of Science. Office of AdvancedScientific Computing Research. Office of Basic Energy Sciences. ChemicalSciences Geosciences and Biosciences Division; National Institutes ofHealth HG01399; British Petroleum. Methane ConversionCooperative
OSTI Identifier:
900699
Report Number(s):
LBNL-57017; LBNL-55334
Journal ID: ISSN 0034-6748; RSINAK; R&D Project: CB1102; BnR: KC0302030; TRN: US0702368
DOE Contract Number:  
DE-AC02-05CH11231
Resource Type:
Journal Article
Resource Relation:
Journal Name: Review of Scientific Instruments; Journal Volume: 75; Journal Issue: 10; Related Information: Journal Publication Date: October 2004
Country of Publication:
United States
Language:
English
Subject:
37; 36; 47; ABSORPTION; ABSORPTION SPECTROSCOPY; ADVANCED LIGHT SOURCE; CATALYSTS; COMPARTMENTS; ENERGY RANGE; ENVIRONMENTAL MATERIALS; GAS FLOW; HEATERS; MICROSCOPES; OXIDATION; PERFORMANCE; PHOTONS; SPECTRA; VALENCE

Citation Formats

Drake, Ian J., Liu, Teris C.N., Gilles, Mary, Tyliszczak, Tolek, Kilcoyne, A.L. David, Shuh, David K., Mathies, Richard A., and Bell, Alexis T. An in-situ cell for characterization of solids by soft X-rayabsorption. United States: N. p., 2007. Web.
Drake, Ian J., Liu, Teris C.N., Gilles, Mary, Tyliszczak, Tolek, Kilcoyne, A.L. David, Shuh, David K., Mathies, Richard A., & Bell, Alexis T. An in-situ cell for characterization of solids by soft X-rayabsorption. United States.
Drake, Ian J., Liu, Teris C.N., Gilles, Mary, Tyliszczak, Tolek, Kilcoyne, A.L. David, Shuh, David K., Mathies, Richard A., and Bell, Alexis T. Thu . "An in-situ cell for characterization of solids by soft X-rayabsorption". United States. doi:. https://www.osti.gov/servlets/purl/900699.
@article{osti_900699,
title = {An in-situ cell for characterization of solids by soft X-rayabsorption},
author = {Drake, Ian J. and Liu, Teris C.N. and Gilles, Mary and Tyliszczak, Tolek and Kilcoyne, A.L. David and Shuh, David K. and Mathies, Richard A. and Bell, Alexis T.},
abstractNote = {An in-situ cell using ''lab-on-a-chip'' technologies has been designed and tested for characterization of catalysts and environmental materials using soft X-ray absorption spectroscopy and spectromicroscopy at photon energies above 250 eV. The sample compartment is 1.0 mm in diameter with a gas path length of 0.8 mm to minimize X-ray absorption in the gas phase. The sample compartment can be heated to 533 K by an Al resistive heater and gas flows up to 5.0 cm{sup 3} min{sup -1} can be supplied to the sample compartment through microchannels. The performance of the cell was tested by acquiring Cu L{sub 3}-edge XANES data during the reduction and oxidation of a silica-supported Cu catalyst using the beam line 11.0.2 Scanning Transmission X-ray Microscope (STXM) at the Advanced Light Source of LBNL. Two-dimensional images of individual catalyst particles were recorded at photon energies between 926 eV and 937 eV, the energy range in which the Cu(II) and Cu(I) L{sub 3} absorption edges are observed. Oxidation state specific images of the catalyst clearly show the disappearance of Cu(II) species during the exposure of the oxidized sample to 4% CO in He while increasing the temperature from 308 K to 473 K. Reoxidation restores the intensity of the image associated with Cu(II). L-edge XANES spectra obtained from stacks of STXM images show that with increasing temperature the Cu(II) peak intensity decreases as the Cu(I) peak intensity increases.},
doi = {},
journal = {Review of Scientific Instruments},
number = 10,
volume = 75,
place = {United States},
year = {Thu Jan 04 00:00:00 EST 2007},
month = {Thu Jan 04 00:00:00 EST 2007}
}