A. Guillot, D. Giaume, A. Suvorova, M. N. Rager, J.-B. d’Espinose de Lacaillerie, C. Mir, X. Randrema, P. Barboux
{"title":"利用溶胶-凝胶工艺合成锂导电钛磷酸盐","authors":"A. Guillot, D. Giaume, A. Suvorova, M. N. Rager, J.-B. d’Espinose de Lacaillerie, C. Mir, X. Randrema, P. Barboux","doi":"10.1007/s10971-024-06461-2","DOIUrl":null,"url":null,"abstract":"<p>The synthesis of titanium and lithium phosphates was studied using the sol-gel method. Particular attention was paid to phosphate precursors, which were mixtures of phosphate mono- and diesters prepared by solvolysis of P<sub>4</sub>O<sub>10</sub> in isopropanol. The reaction of these precursors with titanium and lithium alkoxides yielded homogeneous gels and after drying and thermal cleavage of the esters at 300 °C, amorphous inorganic products. For the composition corresponding to the stoichiometric formula of a stable compound such as LiTi<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub>, the phase crystallized as early as 550 °C by nucleation from the amorphous mixture. Ionic conductivity measured at room temperature was of the order of 10<sup>−5</sup> S·cm<sup>−1</sup> which increased after heat treatment at higher temperatures. If the composition did not correspond to a stable thermodynamic phase, phase separation occurred, and ionic conductivity decreased between 500 °C and 700 °C.</p><h3 data-test=\"abstract-sub-heading\">Graphical Abstract</h3>","PeriodicalId":664,"journal":{"name":"Journal of Sol-Gel Science and Technology","volume":null,"pages":null},"PeriodicalIF":2.3000,"publicationDate":"2024-06-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Synthesis of lithium conducting titanium phosphates by the sol-gel process\",\"authors\":\"A. Guillot, D. Giaume, A. Suvorova, M. N. Rager, J.-B. d’Espinose de Lacaillerie, C. Mir, X. Randrema, P. Barboux\",\"doi\":\"10.1007/s10971-024-06461-2\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p>The synthesis of titanium and lithium phosphates was studied using the sol-gel method. Particular attention was paid to phosphate precursors, which were mixtures of phosphate mono- and diesters prepared by solvolysis of P<sub>4</sub>O<sub>10</sub> in isopropanol. The reaction of these precursors with titanium and lithium alkoxides yielded homogeneous gels and after drying and thermal cleavage of the esters at 300 °C, amorphous inorganic products. For the composition corresponding to the stoichiometric formula of a stable compound such as LiTi<sub>2</sub>(PO<sub>4</sub>)<sub>3</sub>, the phase crystallized as early as 550 °C by nucleation from the amorphous mixture. Ionic conductivity measured at room temperature was of the order of 10<sup>−5</sup> S·cm<sup>−1</sup> which increased after heat treatment at higher temperatures. If the composition did not correspond to a stable thermodynamic phase, phase separation occurred, and ionic conductivity decreased between 500 °C and 700 °C.</p><h3 data-test=\\\"abstract-sub-heading\\\">Graphical Abstract</h3>\",\"PeriodicalId\":664,\"journal\":{\"name\":\"Journal of Sol-Gel Science and Technology\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":2.3000,\"publicationDate\":\"2024-06-22\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Sol-Gel Science and Technology\",\"FirstCategoryId\":\"88\",\"ListUrlMain\":\"https://doi.org/10.1007/s10971-024-06461-2\",\"RegionNum\":4,\"RegionCategory\":\"材料科学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q2\",\"JCRName\":\"MATERIALS SCIENCE, CERAMICS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Sol-Gel Science and Technology","FirstCategoryId":"88","ListUrlMain":"https://doi.org/10.1007/s10971-024-06461-2","RegionNum":4,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q2","JCRName":"MATERIALS SCIENCE, CERAMICS","Score":null,"Total":0}
引用次数: 0
摘要
研究采用溶胶-凝胶法合成钛和锂磷酸盐。特别关注的是磷酸盐前体,它们是通过在异丙醇中溶解 P4O10 而制备的磷酸盐单酯和双酯混合物。这些前体与钛和锂烷氧基化物反应生成均匀的凝胶,在 300 °C 下干燥和热裂解酯后,生成无定形的无机产品。对于与稳定化合物(如 LiTi2(PO4)3)的化学计量式相对应的成分,无定形混合物最早在 550 ℃ 时就能通过成核形成结晶。室温下测得的离子电导率约为 10-5 S-cm-1,在较高温度下进行热处理后,离子电导率有所上升。如果组成不符合稳定的热力学相,则会发生相分离,离子导电率在 500 °C 至 700 °C 之间下降。
Synthesis of lithium conducting titanium phosphates by the sol-gel process
The synthesis of titanium and lithium phosphates was studied using the sol-gel method. Particular attention was paid to phosphate precursors, which were mixtures of phosphate mono- and diesters prepared by solvolysis of P4O10 in isopropanol. The reaction of these precursors with titanium and lithium alkoxides yielded homogeneous gels and after drying and thermal cleavage of the esters at 300 °C, amorphous inorganic products. For the composition corresponding to the stoichiometric formula of a stable compound such as LiTi2(PO4)3, the phase crystallized as early as 550 °C by nucleation from the amorphous mixture. Ionic conductivity measured at room temperature was of the order of 10−5 S·cm−1 which increased after heat treatment at higher temperatures. If the composition did not correspond to a stable thermodynamic phase, phase separation occurred, and ionic conductivity decreased between 500 °C and 700 °C.
期刊介绍:
The primary objective of the Journal of Sol-Gel Science and Technology (JSST), the official journal of the International Sol-Gel Society, is to provide an international forum for the dissemination of scientific, technological, and general knowledge about materials processed by chemical nanotechnologies known as the "sol-gel" process. The materials of interest include gels, gel-derived glasses, ceramics in form of nano- and micro-powders, bulk, fibres, thin films and coatings as well as more recent materials such as hybrid organic-inorganic materials and composites. Such materials exhibit a wide range of optical, electronic, magnetic, chemical, environmental, and biomedical properties and functionalities. Methods for producing sol-gel-derived materials and the industrial uses of these materials are also of great interest.