Quantification of passivation layer growth in inert anodes for molten salt electrochemistry by in situ energy-dispersive diffraction
An in situ energy‐dispersive X‐ray diffraction experiment was undertaken on operational titanium electrowinning cells to observe the formation of rutile (TiO2) passivation layers on Magnéli‐phase (TinO2n−1; n = 4–6) anodes and thus determine the relationship between passivation layer formation and e...
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| Veröffentlicht in: | Journal of applied crystallography 2012-02, Vol.45 (1), p.28-37 |
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| container_title | Journal of applied crystallography |
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| creator | Rowles, Matthew R. Styles, Mark J. Madsen, Ian C. Scarlett, Nicola V. Y. McGregor, Katherine Riley, Daniel P. Snook, Graeme A. Urban, Andrew J. Connolley, Thomas Reinhard, Christina |
| description | An in situ energy‐dispersive X‐ray diffraction experiment was undertaken on operational titanium electrowinning cells to observe the formation of rutile (TiO2) passivation layers on Magnéli‐phase (TinO2n−1; n = 4–6) anodes and thus determine the relationship between passivation layer formation and electrolysis time. Quantitative phase analysis of the energy‐dispersive data was undertaken using a crystal‐structure‐based Rietveld refinement. Layer formation was successfully observed and it was found that the rate of increase in layer thickness decreased with time, rather than remaining constant as observed in previous studies. The limiting step in rutile formation is thought to be the rate of solid‐state diffusion of oxygen within the anode structure. |
| doi_str_mv | 10.1107/S0021889811044104 |
| format | Article |
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Y. ; McGregor, Katherine ; Riley, Daniel P. ; Snook, Graeme A. ; Urban, Andrew J. ; Connolley, Thomas ; Reinhard, Christina</creator><creatorcontrib>Rowles, Matthew R. ; Styles, Mark J. ; Madsen, Ian C. ; Scarlett, Nicola V. Y. ; McGregor, Katherine ; Riley, Daniel P. ; Snook, Graeme A. ; Urban, Andrew J. ; Connolley, Thomas ; Reinhard, Christina</creatorcontrib><description>An in situ energy‐dispersive X‐ray diffraction experiment was undertaken on operational titanium electrowinning cells to observe the formation of rutile (TiO2) passivation layers on Magnéli‐phase (TinO2n−1; n = 4–6) anodes and thus determine the relationship between passivation layer formation and electrolysis time. Quantitative phase analysis of the energy‐dispersive data was undertaken using a crystal‐structure‐based Rietveld refinement. Layer formation was successfully observed and it was found that the rate of increase in layer thickness decreased with time, rather than remaining constant as observed in previous studies. The limiting step in rutile formation is thought to be the rate of solid‐state diffusion of oxygen within the anode structure.</description><identifier>ISSN: 1600-5767</identifier><identifier>ISSN: 0021-8898</identifier><identifier>EISSN: 1600-5767</identifier><identifier>DOI: 10.1107/S0021889811044104</identifier><language>eng</language><publisher>5 Abbey Square, Chester, Cheshire CH1 2HU, England: International Union of Crystallography</publisher><subject>Anodes ; Constraining ; Crystal structure ; Crystallography ; Diffraction ; Diffusion ; electrolysis ; Energy dissipation ; Fused salts ; in situ energy-dispersive diffraction ; Passivation ; Rietveld refinement ; Rutile ; Titanium dioxide ; X-rays</subject><ispartof>Journal of applied crystallography, 2012-02, Vol.45 (1), p.28-37</ispartof><rights>International Union of Crystallography, 2012</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c3924-1e42e38aceb6922ba66193350e883978feedf3915ee5beae968c4031a20011373</citedby><cites>FETCH-LOGICAL-c3924-1e42e38aceb6922ba66193350e883978feedf3915ee5beae968c4031a20011373</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://onlinelibrary.wiley.com/doi/pdf/10.1107%2FS0021889811044104$$EPDF$$P50$$Gwiley$$H</linktopdf><linktohtml>$$Uhttps://onlinelibrary.wiley.com/doi/full/10.1107%2FS0021889811044104$$EHTML$$P50$$Gwiley$$H</linktohtml><link.rule.ids>314,776,780,1411,27901,27902,45550,45551</link.rule.ids></links><search><creatorcontrib>Rowles, Matthew R.</creatorcontrib><creatorcontrib>Styles, Mark J.</creatorcontrib><creatorcontrib>Madsen, Ian C.</creatorcontrib><creatorcontrib>Scarlett, Nicola V. Y.</creatorcontrib><creatorcontrib>McGregor, Katherine</creatorcontrib><creatorcontrib>Riley, Daniel P.</creatorcontrib><creatorcontrib>Snook, Graeme A.</creatorcontrib><creatorcontrib>Urban, Andrew J.</creatorcontrib><creatorcontrib>Connolley, Thomas</creatorcontrib><creatorcontrib>Reinhard, Christina</creatorcontrib><title>Quantification of passivation layer growth in inert anodes for molten salt electrochemistry by in situ energy-dispersive diffraction</title><title>Journal of applied crystallography</title><addtitle>J. Appl. Cryst</addtitle><description>An in situ energy‐dispersive X‐ray diffraction experiment was undertaken on operational titanium electrowinning cells to observe the formation of rutile (TiO2) passivation layers on Magnéli‐phase (TinO2n−1; n = 4–6) anodes and thus determine the relationship between passivation layer formation and electrolysis time. Quantitative phase analysis of the energy‐dispersive data was undertaken using a crystal‐structure‐based Rietveld refinement. Layer formation was successfully observed and it was found that the rate of increase in layer thickness decreased with time, rather than remaining constant as observed in previous studies. The limiting step in rutile formation is thought to be the rate of solid‐state diffusion of oxygen within the anode structure.</description><subject>Anodes</subject><subject>Constraining</subject><subject>Crystal structure</subject><subject>Crystallography</subject><subject>Diffraction</subject><subject>Diffusion</subject><subject>electrolysis</subject><subject>Energy dissipation</subject><subject>Fused salts</subject><subject>in situ energy-dispersive diffraction</subject><subject>Passivation</subject><subject>Rietveld refinement</subject><subject>Rutile</subject><subject>Titanium dioxide</subject><subject>X-rays</subject><issn>1600-5767</issn><issn>0021-8898</issn><issn>1600-5767</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2012</creationdate><recordtype>article</recordtype><recordid>eNqFkU1P3DAQhiNEJT7aH9CbxYlLwB-J7RzRAltWKxB0qx4tr3cMhmy82A409_7wehtUofZQy9Z4pPd5PZ4pis8EnxCCxelXjCmRspE5q6p8dop9wjEua8HF7rv7XnEQ4yPGhAtK94uft73ukrPO6OR8h7xFGx2jexnTVg8Q0H3wr-kBuS5vCAnpzq8gIusDWvs2QYeibhOCFkwK3jzA2sUUBrQctkx0qUeQwfuhXLm4gZDtAa2ctUGb7TMfiw9WtxE-vcXD4tvlxWLypZzfTK8mZ_PSsIZWJYGKApPawJI3lC4156RhrMYgJWuEtAAryxpSA9RL0NBwaSrMiKb5u4QJdlgcj76b4J97iEnlQg20re7A91HlnhBGs1eVpUd_SR99H7pcnWoIr3leNIvIKDLBxxjAqk1wax0GRbDajkX9M5bMyJF5dS0M_wfUbHK3uKnxb7Qc0dxd-PEH1eFJccFErb5fT9UMV7fzO3GuCPsF8Uug0A</recordid><startdate>20120201</startdate><enddate>20120201</enddate><creator>Rowles, Matthew R.</creator><creator>Styles, Mark J.</creator><creator>Madsen, Ian C.</creator><creator>Scarlett, Nicola V. 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| ispartof | Journal of applied crystallography, 2012-02, Vol.45 (1), p.28-37 |
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| source | Wiley Online Library Journals Frontfile Complete; Alma/SFX Local Collection |
| subjects | Anodes Constraining Crystal structure Crystallography Diffraction Diffusion electrolysis Energy dissipation Fused salts in situ energy-dispersive diffraction Passivation Rietveld refinement Rutile Titanium dioxide X-rays |
| title | Quantification of passivation layer growth in inert anodes for molten salt electrochemistry by in situ energy-dispersive diffraction |
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