{"id":{"repo_id":"strathclyde","oai_identifier":"oai:strathclyde:rv042t11v"},"canonical_url":"https://search.dev.ndltd.org/etd/strathclyde/oai:strathclyde:rv042t11v","repository":{"repo_id":"strathclyde","name":"University of Strathclyde","base_url":"https://stax.strath.ac.uk/catalog/oai"},"display":{"title":"The low-temperature formation of mixed-metal oxides","abstract":"This thesis describes a new route to lithium molybdate, Li₂MoO₄, which involves grinding together LiOH·H₂O and MoO₃ in air at room temperature. X-ray powder diffraction data show that the formation of highly crystalline Li₂MoO₄ is largely complete after 10 min, and that this product crystallises with the phenacite structuretype. This structure is the same as that derived from an X-ray diffraction study of a single crystal of Li₂MoO₄ grown from aqueous solution [R3 ; a = 14.3178(14) Å, c = 9.5757(9) Å]. Differential scanning calorimetric measurements show that the reaction between the solid reagents proceeds spontaneously, even at sub-ambient temperatures, and is driven by the liberation of water from the lattice of LiOH·H₂O. In this manner, Li₂MoO₄ is prepared as mono-disperse particles, which are smaller and more regularly shaped than those yielded by other synthetic methods. This reaction has been developed further to provide a new route to the lithium ion exchange of a series of protonated Ruddlesden-Popper layered perovskites (HLaTiO₄, H₂SrTa₂O₇ and H₂La₂Ti₃O₁₀), with a controlled proton and lithium content. This involves grinding a stoichiometric quantity of LiOH·H₂O with each of the solid acids. X-ray powder diffraction data show that the reactions leading to H₁₋xLixLaTiO₄ [P4/nmm; x ≥ 0.1] and HLiSrTa₂O₇ [Ama2] are complete after 5 d, whilst those leading to H₂₋₂xLi₂xLa₂Ti₃O₁₀ [I4/mmm; x ≥ 0.125] are complete after 53 min. Neutron powder diffraction data of the intermediate members of the H₁₋xLixLaTiO₄ series indicate that the interlayer cations are disordered and remain on the 16k (H⁺) and 2b (Li⁺) sites identified in the end-member phases. The exchanged phases could be modified by dehydration at 360-480 °C to give new defective layered perovskites: ☐₁₋xLixLaTiO₄[(₁₋x)/₂] (0.5 ≤ x ≤ 0.9), ☐LiSrTa₂O₆.₅ and ☐LiLa₂Ti₃O₉.₅. AC impedance spectroscopy measurements indicate that these samples demonstrate a lower total ionic conductivity than that of the respective lithium end-members.","abstract_html":"This thesis describes a new route to lithium molybdate, Li₂MoO₄, which involves grinding together LiOH·H₂O and MoO₃ in air at room temperature. X-ray powder diffraction data show that the formation of highly crystalline Li₂MoO₄ is largely complete after 10 min, and that this product crystallises with the phenacite structuretype. This structure is the same as that derived from an X-ray diffraction study of a single crystal of Li₂MoO₄ grown from aqueous solution [R3 ; a = 14.3178(14) Å, c = 9.5757(9) Å]. Differential scanning calorimetric measurements show that the reaction between the solid reagents proceeds spontaneously, even at sub-ambient temperatures, and is driven by the liberation of water from the lattice of LiOH·H₂O. In this manner, Li₂MoO₄ is prepared as mono-disperse particles, which are smaller and more regularly shaped than those yielded by other synthetic methods. This reaction has been developed further to provide a new route to the lithium ion exchange of a series of protonated Ruddlesden-Popper layered perovskites (HLaTiO₄, H₂SrTa₂O₇ and H₂La₂Ti₃O₁₀), with a controlled proton and lithium content. This involves grinding a stoichiometric quantity of LiOH·H₂O with each of the solid acids. X-ray powder diffraction data show that the reactions leading to H₁₋xLixLaTiO₄ [P4/nmm; x ≥ 0.1] and HLiSrTa₂O₇ [Ama2] are complete after 5 d, whilst those leading to H₂₋₂xLi₂xLa₂Ti₃O₁₀ [I4/mmm; x ≥ 0.125] are complete after 53 min. Neutron powder diffraction data of the intermediate members of the H₁₋xLixLaTiO₄ series indicate that the interlayer cations are disordered and remain on the 16k (H⁺) and 2b (Li⁺) sites identified in the end-member phases. The exchanged phases could be modified by dehydration at 360-480 °C to give new defective layered perovskites: ☐₁₋xLixLaTiO₄[(₁₋x)/₂] (0.5 ≤ x ≤ 0.9), ☐LiSrTa₂O₆.₅ and ☐LiLa₂Ti₃O₉.₅. AC impedance spectroscopy measurements indicate that these samples demonstrate a lower total ionic conductivity than that of the respective lithium end-members.","abstract_has_math":false,"creators":["Yip, Thomas Wai Sing"],"institution":"University of Strathclyde","degree_name":"phd","degree_level":"doctoral-pg","degree_discipline":null,"degree_department":null,"school":null,"contributors":[],"advisors":[],"committee_chairs":[],"committee_members":[],"year":2011,"date_issued":"2011","date_published":"2011","updated_at":"2026-07-24T04:47:28Z","subjects":[],"languages":[],"rights":[],"rights_urls":[],"identifier_entries":[{"key":"dc:identifier.doi","label":"DOI","values":["10.48730/dx16-sp53"],"render_values":[{"text":"10.48730/dx16-sp53","href":"https://doi.org/10.48730/dx16-sp53","code":true}]},{"key":"dc:identifier","label":"Identifier","values":["T12873"],"render_values":[{"text":"T12873","href":null,"code":true}]}]},"links":{"outbound_url":"https://stax.strath.ac.uk/concern/theses/rv042t11v","outbound_label":"Repository record","outbound_source":"dc:identifier.uri"},"metadata_groups":[{"id":"people","label":"People","entries":[{"key":"dc:creator","label":"Author","values":["Yip, Thomas Wai Sing"]}]},{"id":"academic_context","label":"Academic Context","entries":[{"key":"dc:date","label":"Dc Date","values":["2011"]},{"key":"dc:date.issued","label":"Date","values":["2011"]},{"key":"dc:publisher.department","label":"Dc Publisher Department","values":["Department of Pure and Applied Chemistry"]},{"key":"dc:publisher.institution","label":"Dc Publisher Institution","values":["University of Strathclyde"]},{"key":"dc:type.qualificationlevel","label":"Dc Type Qualificationlevel","values":["doctoral-pg"]},{"key":"dc:type.qualificationname","label":"Dc Type Qualificationname","values":["phd"]}]},{"id":"identifiers","label":"Identifiers","entries":[{"key":"dc:identifier","label":"Identifier","values":["T12873"]},{"key":"dc:identifier.doi","label":"DOI","values":["10.48730/dx16-sp53"]},{"key":"dc:identifier.uri","label":"Identifier URI","values":["https://stax.strath.ac.uk/concern/theses/rv042t11v"]}]},{"id":"additional","label":"Additional Metadata","entries":[{"key":"dc:description","label":"Description","values":["This thesis describes a new route to lithium molybdate, Li₂MoO₄, which involves grinding together LiOH·H₂O and MoO₃ in air at room temperature. X-ray powder diffraction data show that the formation of highly crystalline Li₂MoO₄ is largely complete after 10 min, and that this product crystallises with the phenacite structuretype. This structure is the same as that derived from an X-ray diffraction study of a single crystal of Li₂MoO₄ grown from aqueous solution [R3 ; a = 14.3178(14) Å, c = 9.5757(9) Å]. Differential scanning calorimetric measurements show that the reaction between the solid reagents proceeds spontaneously, even at sub-ambient temperatures, and is driven by the liberation of water from the lattice of LiOH·H₂O. In this manner, Li₂MoO₄ is prepared as mono-disperse particles, which are smaller and more regularly shaped than those yielded by other synthetic methods. This reaction has been developed further to provide a new route to the lithium ion exchange of a series of protonated Ruddlesden-Popper layered perovskites (HLaTiO₄, H₂SrTa₂O₇ and H₂La₂Ti₃O₁₀), with a controlled proton and lithium content. This involves grinding a stoichiometric quantity of LiOH·H₂O with each of the solid acids. X-ray powder diffraction data show that the reactions leading to H₁₋xLixLaTiO₄ [P4/nmm; x ≥ 0.1] and HLiSrTa₂O₇ [Ama2] are complete after 5 d, whilst those leading to H₂₋₂xLi₂xLa₂Ti₃O₁₀ [I4/mmm; x ≥ 0.125] are complete after 53 min. Neutron powder diffraction data of the intermediate members of the H₁₋xLixLaTiO₄ series indicate that the interlayer cations are disordered and remain on the 16k (H⁺) and 2b (Li⁺) sites identified in the end-member phases. The exchanged phases could be modified by dehydration at 360-480 °C to give new defective layered perovskites: ☐₁₋xLixLaTiO₄[(₁₋x)/₂] (0.5 ≤ x ≤ 0.9), ☐LiSrTa₂O₆.₅ and ☐LiLa₂Ti₃O₉.₅. AC impedance spectroscopy measurements indicate that these samples demonstrate a lower total ionic conductivity than that of the respective lithium end-members."]},{"key":"dc:description.abstract","label":"Abstract","values":["This thesis describes a new route to lithium molybdate, Li₂MoO₄, which involves grinding together LiOH·H₂O and MoO₃ in air at room temperature. X-ray powder diffraction data show that the formation of highly crystalline Li₂MoO₄ is largely complete after 10 min, and that this product crystallises with the phenacite structuretype. This structure is the same as that derived from an X-ray diffraction study of a single crystal of Li₂MoO₄ grown from aqueous solution [R3 ; a = 14.3178(14) Å, c = 9.5757(9) Å]. Differential scanning calorimetric measurements show that the reaction between the solid reagents proceeds spontaneously, even at sub-ambient temperatures, and is driven by the liberation of water from the lattice of LiOH·H₂O. In this manner, Li₂MoO₄ is prepared as mono-disperse particles, which are smaller and more regularly shaped than those yielded by other synthetic methods. This reaction has been developed further to provide a new route to the lithium ion exchange of a series of protonated Ruddlesden-Popper layered perovskites (HLaTiO₄, H₂SrTa₂O₇ and H₂La₂Ti₃O₁₀), with a controlled proton and lithium content. This involves grinding a stoichiometric quantity of LiOH·H₂O with each of the solid acids. X-ray powder diffraction data show that the reactions leading to H₁₋xLixLaTiO₄ [P4/nmm; x ≥ 0.1] and HLiSrTa₂O₇ [Ama2] are complete after 5 d, whilst those leading to H₂₋₂xLi₂xLa₂Ti₃O₁₀ [I4/mmm; x ≥ 0.125] are complete after 53 min. Neutron powder diffraction data of the intermediate members of the H₁₋xLixLaTiO₄ series indicate that the interlayer cations are disordered and remain on the 16k (H⁺) and 2b (Li⁺) sites identified in the end-member phases. The exchanged phases could be modified by dehydration at 360-480 °C to give new defective layered perovskites: ☐₁₋xLixLaTiO₄[(₁₋x)/₂] (0.5 ≤ x ≤ 0.9), ☐LiSrTa₂O₆.₅ and ☐LiLa₂Ti₃O₉.₅. AC impedance spectroscopy measurements indicate that these samples demonstrate a lower total ionic conductivity than that of the respective lithium end-members."]},{"key":"dc:title","label":"Title","values":["The low-temperature formation of mixed-metal oxides"]}]}],"canonical_facts":{"dc:creator":["Yip, Thomas Wai Sing"],"dc:date":["2011"],"dc:date.issued":["2011"],"dc:description":["This thesis describes a new route to lithium molybdate, Li₂MoO₄, which involves grinding together LiOH·H₂O and MoO₃ in air at room temperature. X-ray powder diffraction data show that the formation of highly crystalline Li₂MoO₄ is largely complete after 10 min, and that this product crystallises with the phenacite structuretype. This structure is the same as that derived from an X-ray diffraction study of a single crystal of Li₂MoO₄ grown from aqueous solution [R3 ; a = 14.3178(14) Å, c = 9.5757(9) Å]. Differential scanning calorimetric measurements show that the reaction between the solid reagents proceeds spontaneously, even at sub-ambient temperatures, and is driven by the liberation of water from the lattice of LiOH·H₂O. In this manner, Li₂MoO₄ is prepared as mono-disperse particles, which are smaller and more regularly shaped than those yielded by other synthetic methods. This reaction has been developed further to provide a new route to the lithium ion exchange of a series of protonated Ruddlesden-Popper layered perovskites (HLaTiO₄, H₂SrTa₂O₇ and H₂La₂Ti₃O₁₀), with a controlled proton and lithium content. This involves grinding a stoichiometric quantity of LiOH·H₂O with each of the solid acids. X-ray powder diffraction data show that the reactions leading to H₁₋xLixLaTiO₄ [P4/nmm; x ≥ 0.1] and HLiSrTa₂O₇ [Ama2] are complete after 5 d, whilst those leading to H₂₋₂xLi₂xLa₂Ti₃O₁₀ [I4/mmm; x ≥ 0.125] are complete after 53 min. Neutron powder diffraction data of the intermediate members of the H₁₋xLixLaTiO₄ series indicate that the interlayer cations are disordered and remain on the 16k (H⁺) and 2b (Li⁺) sites identified in the end-member phases. The exchanged phases could be modified by dehydration at 360-480 °C to give new defective layered perovskites: ☐₁₋xLixLaTiO₄[(₁₋x)/₂] (0.5 ≤ x ≤ 0.9), ☐LiSrTa₂O₆.₅ and ☐LiLa₂Ti₃O₉.₅. AC impedance spectroscopy measurements indicate that these samples demonstrate a lower total ionic conductivity than that of the respective lithium end-members."],"dc:description.abstract":["This thesis describes a new route to lithium molybdate, Li₂MoO₄, which involves grinding together LiOH·H₂O and MoO₃ in air at room temperature. X-ray powder diffraction data show that the formation of highly crystalline Li₂MoO₄ is largely complete after 10 min, and that this product crystallises with the phenacite structuretype. This structure is the same as that derived from an X-ray diffraction study of a single crystal of Li₂MoO₄ grown from aqueous solution [R3 ; a = 14.3178(14) Å, c = 9.5757(9) Å]. Differential scanning calorimetric measurements show that the reaction between the solid reagents proceeds spontaneously, even at sub-ambient temperatures, and is driven by the liberation of water from the lattice of LiOH·H₂O. In this manner, Li₂MoO₄ is prepared as mono-disperse particles, which are smaller and more regularly shaped than those yielded by other synthetic methods. This reaction has been developed further to provide a new route to the lithium ion exchange of a series of protonated Ruddlesden-Popper layered perovskites (HLaTiO₄, H₂SrTa₂O₇ and H₂La₂Ti₃O₁₀), with a controlled proton and lithium content. This involves grinding a stoichiometric quantity of LiOH·H₂O with each of the solid acids. X-ray powder diffraction data show that the reactions leading to H₁₋xLixLaTiO₄ [P4/nmm; x ≥ 0.1] and HLiSrTa₂O₇ [Ama2] are complete after 5 d, whilst those leading to H₂₋₂xLi₂xLa₂Ti₃O₁₀ [I4/mmm; x ≥ 0.125] are complete after 53 min. Neutron powder diffraction data of the intermediate members of the H₁₋xLixLaTiO₄ series indicate that the interlayer cations are disordered and remain on the 16k (H⁺) and 2b (Li⁺) sites identified in the end-member phases. The exchanged phases could be modified by dehydration at 360-480 °C to give new defective layered perovskites: ☐₁₋xLixLaTiO₄[(₁₋x)/₂] (0.5 ≤ x ≤ 0.9), ☐LiSrTa₂O₆.₅ and ☐LiLa₂Ti₃O₉.₅. AC impedance spectroscopy measurements indicate that these samples demonstrate a lower total ionic conductivity than that of the respective lithium end-members."],"dc:identifier":["T12873"],"dc:identifier.doi":["10.48730/dx16-sp53"],"dc:identifier.uri":["https://stax.strath.ac.uk/concern/theses/rv042t11v"],"dc:publisher.department":["Department of Pure and Applied Chemistry"],"dc:publisher.institution":["University of Strathclyde"],"dc:title":["The low-temperature formation of mixed-metal oxides"],"dc:type.qualificationlevel":["doctoral-pg"],"dc:type.qualificationname":["phd"]},"updated_at":"2026-07-24T04:47:28Z"}