Versatile in situ powder X-ray diffraction cells for solid–gas investigations
Identifieur interne : 002479 ( Pmc/Curation ); précédent : 002478; suivant : 002480Versatile in situ powder X-ray diffraction cells for solid–gas investigations
Auteurs : Torben R. Jensen [Danemark] ; Thomas K. Nielsen [Danemark] ; Yaroslav Filinchuk [France] ; Jens-Erik J Rgensen [Danemark] ; Yngve Cerenius [Suède] ; Evan Maca. Gray [Australie] ; Colin J. Webb [Australie]Source :
- Journal of Applied Crystallography [ 0021-8898 ] ; 2010.
Abstract
Two multipurpose sample cells of quartz (SiO2) or sapphire (Al2O3) capillaries, developed for the study of solid–gas reactions in dosing or flow mode, are presented. They allow fast change of pressure up to 100 or 300 bar (1 bar = 100 000 Pa) and can also handle solid–liquid–gas studies.
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DOI: 10.1107/S0021889810038148
PubMed: 22477780
PubMed Central: 3253740
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en">Versatile <italic>in situ</italic> powder X-ray diffraction cells for solid–gas investigations</title><author><name sortKey="Jensen, Torben R" sort="Jensen, Torben R" uniqKey="Jensen T" first="Torben R." last="Jensen">Torben R. Jensen</name><affiliation wicri:level="1"><nlm:aff id="a">Center for Energy Materials, Center for Materials Crystallography, iNANO and Chemistry Department, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C,<country>Denmark</country></nlm:aff><country xml:lang="fr">Danemark</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Nielsen, Thomas K" sort="Nielsen, Thomas K" uniqKey="Nielsen T" first="Thomas K." last="Nielsen">Thomas K. Nielsen</name><affiliation wicri:level="1"><nlm:aff id="a">Center for Energy Materials, Center for Materials Crystallography, iNANO and Chemistry Department, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C,<country>Denmark</country></nlm:aff><country xml:lang="fr">Danemark</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Filinchuk, Yaroslav" sort="Filinchuk, Yaroslav" uniqKey="Filinchuk Y" first="Yaroslav" last="Filinchuk">Yaroslav Filinchuk</name><affiliation wicri:level="1"><nlm:aff id="b">Swiss–Norwegian Beam Lines, European Synchrotron Radiation Facility, 38043 Grenoble,<country>France</country></nlm:aff><country xml:lang="fr">France</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="J Rgensen, Jens Erik" sort="J Rgensen, Jens Erik" uniqKey="J Rgensen J" first="Jens-Erik" last="J Rgensen">Jens-Erik J Rgensen</name><affiliation wicri:level="1"><nlm:aff id="a">Center for Energy Materials, Center for Materials Crystallography, iNANO and Chemistry Department, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C,<country>Denmark</country></nlm:aff><country xml:lang="fr">Danemark</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Cerenius, Yngve" sort="Cerenius, Yngve" uniqKey="Cerenius Y" first="Yngve" last="Cerenius">Yngve Cerenius</name><affiliation wicri:level="1"><nlm:aff id="c">MAX-lab, Lund University, S-22100 Lund,<country>Sweden</country></nlm:aff><country xml:lang="fr">Suède</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Gray, Evan Maca" sort="Gray, Evan Maca" uniqKey="Gray E" first="Evan Maca." last="Gray">Evan Maca. Gray</name><affiliation wicri:level="1"><nlm:aff id="d">Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan 4111, Brisbane,<country>Australia</country></nlm:aff><country xml:lang="fr">Australie</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Webb, Colin J" sort="Webb, Colin J" uniqKey="Webb C" first="Colin J." last="Webb">Colin J. Webb</name><affiliation wicri:level="1"><nlm:aff id="d">Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan 4111, Brisbane,<country>Australia</country></nlm:aff><country xml:lang="fr">Australie</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author></titleStmt><publicationStmt><idno type="wicri:source">PMC</idno><idno type="pmid">22477780</idno><idno type="pmc">3253740</idno><idno type="url">http://www.ncbi.nlm.nih.gov/pmc/articles/PMC3253740</idno><idno type="RBID">PMC:3253740</idno><idno type="doi">10.1107/S0021889810038148</idno><date when="2010">2010</date><idno type="wicri:Area/Pmc/Corpus">002629</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Corpus" wicri:corpus="PMC">002629</idno><idno type="wicri:Area/Pmc/Curation">002479</idno><idno type="wicri:explorRef" wicri:stream="Pmc" wicri:step="Curation">002479</idno></publicationStmt><sourceDesc><biblStruct><analytic><title xml:lang="en" level="a" type="main">Versatile <italic>in situ</italic> powder X-ray diffraction cells for solid–gas investigations</title><author><name sortKey="Jensen, Torben R" sort="Jensen, Torben R" uniqKey="Jensen T" first="Torben R." last="Jensen">Torben R. Jensen</name><affiliation wicri:level="1"><nlm:aff id="a">Center for Energy Materials, Center for Materials Crystallography, iNANO and Chemistry Department, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C,<country>Denmark</country></nlm:aff><country xml:lang="fr">Danemark</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Nielsen, Thomas K" sort="Nielsen, Thomas K" uniqKey="Nielsen T" first="Thomas K." last="Nielsen">Thomas K. Nielsen</name><affiliation wicri:level="1"><nlm:aff id="a">Center for Energy Materials, Center for Materials Crystallography, iNANO and Chemistry Department, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C,<country>Denmark</country></nlm:aff><country xml:lang="fr">Danemark</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Filinchuk, Yaroslav" sort="Filinchuk, Yaroslav" uniqKey="Filinchuk Y" first="Yaroslav" last="Filinchuk">Yaroslav Filinchuk</name><affiliation wicri:level="1"><nlm:aff id="b">Swiss–Norwegian Beam Lines, European Synchrotron Radiation Facility, 38043 Grenoble,<country>France</country></nlm:aff><country xml:lang="fr">France</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="J Rgensen, Jens Erik" sort="J Rgensen, Jens Erik" uniqKey="J Rgensen J" first="Jens-Erik" last="J Rgensen">Jens-Erik J Rgensen</name><affiliation wicri:level="1"><nlm:aff id="a">Center for Energy Materials, Center for Materials Crystallography, iNANO and Chemistry Department, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C,<country>Denmark</country></nlm:aff><country xml:lang="fr">Danemark</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Cerenius, Yngve" sort="Cerenius, Yngve" uniqKey="Cerenius Y" first="Yngve" last="Cerenius">Yngve Cerenius</name><affiliation wicri:level="1"><nlm:aff id="c">MAX-lab, Lund University, S-22100 Lund,<country>Sweden</country></nlm:aff><country xml:lang="fr">Suède</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Gray, Evan Maca" sort="Gray, Evan Maca" uniqKey="Gray E" first="Evan Maca." last="Gray">Evan Maca. Gray</name><affiliation wicri:level="1"><nlm:aff id="d">Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan 4111, Brisbane,<country>Australia</country></nlm:aff><country xml:lang="fr">Australie</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author><author><name sortKey="Webb, Colin J" sort="Webb, Colin J" uniqKey="Webb C" first="Colin J." last="Webb">Colin J. Webb</name><affiliation wicri:level="1"><nlm:aff id="d">Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan 4111, Brisbane,<country>Australia</country></nlm:aff><country xml:lang="fr">Australie</country><wicri:regionArea># see nlm:aff country strict</wicri:regionArea></affiliation></author></analytic><series><title level="j">Journal of Applied Crystallography</title><idno type="ISSN">0021-8898</idno><imprint><date when="2010">2010</date></imprint></series></biblStruct></sourceDesc></fileDesc><profileDesc><textClass></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en"><p>Two multipurpose sample cells of quartz (SiO<sub>2</sub>) or sapphire (Al<sub>2</sub>O<sub>3</sub>) capillaries, developed for the study of solid–gas reactions in dosing or flow mode, are presented. They allow fast change of pressure up to 100 or 300 bar (1 bar = 100 000 Pa) and can also handle solid–liquid–gas studies.</p></div></front><back><div1 type="bibliography"><listBibl><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct><biblStruct></biblStruct></listBibl></div1></back></TEI><pmc article-type="research-article"><pmc-dir>properties open_access</pmc-dir>
<front><journal-meta><journal-id journal-id-type="nlm-ta">J Appl Crystallogr</journal-id><journal-id journal-id-type="publisher-id">J. Appl. Cryst.</journal-id><journal-title-group><journal-title>Journal of Applied Crystallography</journal-title></journal-title-group><issn pub-type="ppub">0021-8898</issn><publisher><publisher-name>International Union of Crystallography</publisher-name></publisher></journal-meta><article-meta><article-id pub-id-type="pmid">22477780</article-id><article-id pub-id-type="pmc">3253740</article-id><article-id pub-id-type="publisher-id">db5089</article-id><article-id pub-id-type="doi">10.1107/S0021889810038148</article-id><article-id pub-id-type="coden">JACGAR</article-id><article-id pub-id-type="pii">S0021889810038148</article-id><article-categories><subj-group subj-group-type="heading"><subject>Research Papers</subject></subj-group></article-categories><title-group><article-title>Versatile <italic>in situ</italic> powder X-ray diffraction cells for solid–gas investigations</article-title><alt-title>Powder X-ray diffraction cells</alt-title></title-group><contrib-group><contrib contrib-type="author"><name><surname>Jensen</surname><given-names>Torben R.</given-names></name><xref ref-type="aff" rid="a">a</xref><xref ref-type="corresp" rid="cor">*</xref></contrib><contrib contrib-type="author"><name><surname>Nielsen</surname><given-names>Thomas K.</given-names></name><xref ref-type="aff" rid="a">a</xref></contrib><contrib contrib-type="author"><name><surname>Filinchuk</surname><given-names>Yaroslav</given-names></name><xref ref-type="aff" rid="b">b</xref></contrib><contrib contrib-type="author"><name><surname>Jørgensen</surname><given-names>Jens-Erik</given-names></name><xref ref-type="aff" rid="a">a</xref></contrib><contrib contrib-type="author"><name><surname>Cerenius</surname><given-names>Yngve</given-names></name><xref ref-type="aff" rid="c">c</xref></contrib><contrib contrib-type="author"><name><surname>Gray</surname><given-names>Evan MacA.</given-names></name><xref ref-type="aff" rid="d">d</xref></contrib><contrib contrib-type="author"><name><surname>Webb</surname><given-names>Colin J.</given-names></name><xref ref-type="aff" rid="d">d</xref></contrib><aff id="a"><label>a</label>Center for Energy Materials, Center for Materials Crystallography, iNANO and Chemistry Department, University of Aarhus, Langelandsgade 140, DK-8000 Aarhus C,<country>Denmark</country></aff><aff id="b"><label>b</label>Swiss–Norwegian Beam Lines, European Synchrotron Radiation Facility, 38043 Grenoble,<country>France</country></aff><aff id="c"><label>c</label>MAX-lab, Lund University, S-22100 Lund,<country>Sweden</country></aff><aff id="d"><label>d</label>Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan 4111, Brisbane,<country>Australia</country></aff></contrib-group><author-notes><corresp id="cor">Correspondence e-mail: <email>trj@chem.au.dk</email></corresp></author-notes><pub-date pub-type="ppub"><day>01</day><month>12</month><year>2010</year></pub-date><pub-date pub-type="epub"><day>20</day><month>10</month><year>2010</year></pub-date><pub-date pub-type="pmc-release"><day>20</day><month>10</month><year>2010</year></pub-date><pmc-comment> PMC Release delay is 0 months and 0 days and was based on the
<volume>43</volume><issue>Pt 6</issue><issue-id pub-id-type="publisher-id">j100600</issue-id><fpage>1456</fpage><lpage>1463</lpage><history><date date-type="received"><day>12</day><month>7</month><year>2010</year></date><date date-type="accepted"><day>24</day><month>9</month><year>2010</year></date></history><permissions><copyright-statement>© Torben R. Jensen et al. 2010</copyright-statement><copyright-year>2010</copyright-year><license license-type="open-access" xlink:href="http://creativecommons.org/licenses/by/2.0/uk/"><license-p>This is an open-access article distributed under the terms of the Creative Commons Attribution Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited.</license-p></license></permissions><self-uri xlink:type="simple" xlink:href="http://dx.doi.org/10.1107/S0021889810038148">A full version of this article is available from Crystallography Journals Online.</self-uri><abstract abstract-type="toc"><p>Two multipurpose sample cells of quartz (SiO<sub>2</sub>) or sapphire (Al<sub>2</sub>O<sub>3</sub>) capillaries, developed for the study of solid–gas reactions in dosing or flow mode, are presented. They allow fast change of pressure up to 100 or 300 bar (1 bar = 100 000 Pa) and can also handle solid–liquid–gas studies.</p></abstract><abstract><p>This paper describes new sample cells and techniques for <italic>in situ</italic> powder X-ray diffraction specifically designed for gas absorption studies up to <italic>ca</italic> 300 bar (1 bar = 100 000 Pa) gas pressure. The cells are for multipurpose use, in particular the study of solid–gas reactions in dosing or flow mode, but can also handle samples involved in solid–liquid–gas studies. The sample can be loaded into a single-crystal sapphire (Al<sub>2</sub>O<sub>3</sub>) capillary, or a quartz (SiO<sub>2</sub>) capillary closed at one end. The advantages of a sapphire single-crystal cell with regard to rapid pressure cycling are discussed, and burst pressures are calculated and measured to be ∼300 bar. An alternative and simpler cell based on a thin-walled silicate or quartz glass capillary, connected to a gas source <italic>via</italic> a VCR fitting, enables studies up to ∼100 bar. Advantages of the two cell types are compared and their applications are illustrated by case studies.</p></abstract><kwd-group><kwd>powder X-ray diffraction</kwd><kwd>X-ray diffraction cells</kwd><kwd>solid–gas reactions</kwd><kwd>hydrogen absorption</kwd></kwd-group></article-meta></front><floats-group><fig id="fig1" position="float"><label>Figure 1</label><caption><p>The cell based on a sapphire capillary, (A). A flexible stainless steel capillary connects the two ends of the sample holder and allows dosing of the sample with a selected gas from both ends simultaneously, and also allows for an easy and fast change of sample.</p></caption><graphic xlink:href="j-43-01456-fig1"></graphic></fig><fig id="fig2" position="float"><label>Figure 2</label><caption><p>The cell based on a thin-walled glass/quartz capillary, (B). Top: the sample is loaded under Ar into a capillary closed at one end, the funnel is sealed with vacuum grease, and the capillary is glued into a socket weld gland with the funnel on the side of the VCR fitting. A 1/8 inch metal gasket is placed next to a 1 cent coin. Middle: the Tee union is fixed in the goniometer head and connected on one side <italic>via</italic> a PEEK capillary to a gas system; the spare outlet is closed by a cap. Bottom: the cell in operation, the nozzle of the Oxford Cryostream pointing from the top to the same position on the sample as the X-ray beam; the beamstop is shown on the right. During temperature-programmed scans, the cell is typically rotated by Δϕ = ±30° during each X-ray exposure within the same angular range.</p></caption><graphic xlink:href="j-43-01456-fig2"></graphic></fig><fig id="fig3" position="float"><label>Figure 3</label><caption><p>Isothermal hydrogen release and uptake reactions studied for a sample of magnesium hydride ball-milled with scandium chloride (5.0 mol%). The SR-PXD data were collected using the sapphire-based cell (A) at a fixed temperature of 593 K for a period of 30 min and the hydrogen pressure varied in the range ∼10<sup>−3</sup> to 100 bar. The X-ray exposure time was 5 s, the time resolution was 9.95 s per powder pattern and the selected X-ray wavelength was λ = 0.94608 Å.</p></caption><graphic xlink:href="j-43-01456-fig3"></graphic></fig><fig id="fig4" position="float"><label>Figure 4</label><caption><p>Integrated normalized diffracted intensity, α(<italic>t</italic>), from Mg and MgH<sub>2</sub> at 543 and 593 K during release and uptake of hydrogen. The PXD data were collected using the sapphire-based cell (A) and extracted from Fig. 3<xref ref-type="fig" rid="fig3"> ▶</xref>.</p></caption><graphic xlink:href="j-43-01456-fig4"></graphic></fig><fig id="fig5" position="float"><label>Figure 5</label><caption><p>Isothermal hydrogen release and uptake reactions studied for a sample of magnesium hydride ball-milled with scandium chloride (5.0 mol%). SR-PXD data were collected at 723 K over a period of 20 min, performed as a continuation of the experiment shown in Fig. 3<xref ref-type="fig" rid="fig3"> ▶</xref>. The PXD data were collected using the sapphire-based cell (A) using an X-ray exposure time of 5 s, a time resolution of 9.95 s per powder pattern and λ = 0.94608 Å. The hydrogen pressure was either ∼10<sup>−2</sup> or 100 bar.</p></caption><graphic xlink:href="j-43-01456-fig5"></graphic></fig><fig id="fig6" position="float"><label>Figure 6</label><caption><p>A single crystal mounted on a needle and fixed inside a thin-walled capillary tube using sample holder (B). This setup allows single-crystal diffraction studies under a gas loading (Miller <italic>et al.</italic>, 2009<xref ref-type="bibr" rid="bb25"> ▶</xref>).</p></caption><graphic xlink:href="j-43-01456-fig6"></graphic></fig><fig id="fig7" position="float"><label>Figure 7</label><caption><p>The cyclic behaviour of CO<sub>2</sub> absorption by a flexible metal–organic framework (Serre <italic>et al.</italic>, 2007<xref ref-type="bibr" rid="bb34"> ▶</xref>). Closed and open forms, shown schematically on the right, are reversibly transformed into each other as the gas pressure periodically varies from 0 to 10 bar (vertical scale). SR-PXD data collected <italic>in situ</italic> using the capillary cell (B) are shown on the left.</p></caption><graphic xlink:href="j-43-01456-fig7"></graphic></fig></floats-group></pmc></record>Pour manipuler ce document sous Unix (Dilib)
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