沉淀胶溶法制备铝掺杂偏钛酸型锂离子筛前驱体  

Preparation of aluminum doped H_(2)TiO_(3)-lithium ion sieve precursor by the precipitation-peptization method

作　　者：张菁菁 张理元[1,2,3] 许霜 赵甜甜 刘佳 刘敏 ZHANG Jing-jing;ZHANG Li-yuan;XU Shuang;ZHAO Tian-tian;LIU Jia;LIU Min(College of Chemistry and Chemical Engineering,Neijiang Normal University,Neijiang 641112,China;Key Laboratory of Fruit Waste Treatment and Resource Recycling of the Sichuan Provincial College,Neijiang 641112,China;Special Agricultural Resources in Tuojiang River Basin Sharing and Service Platform of Sichuan Province,Neijiang 641112,China)

机构地区：[1]内江师范学院化学化工学院,四川内江641112 [2]果类废弃物资源化四川省高等学校重点实验室,四川内江641112 [3]沱江流域特色农业资源四川省科技资源共享服务平台,四川内江641112

出　　处：《化学研究与应用》2024年第12期2873-2884,共12页Chemical Research and Application

基　　金：四川省重点研发项目(2023YFG0247)资助;内江师范学院大学生创新项目(X2023001,X2024013)资助。

摘　　要：以Ti(SO_(4))_(2)为钛源、CH_(3)COOLi为锂源,AlCl_(3)为掺杂源,采用无机沉淀胶溶法制备铝掺杂锂离子筛前驱体,探究铝掺杂对Li_(2)TiO_(3)前驱体溶胶稳定性及前驱体形貌、组成等的影响。使用扫描电子显微镜(SEM)、X射线衍射仪(XRD)、透射电子显微镜(TEM)、X射线光电子能谱仪(XPS)、Zeta电位仪等对样品表面形貌、晶相组成、表面化学元素组成及其相应的化学价态、溶胶体系的分散性等进行表征。结果表明:在750℃煅烧下,当铝掺杂的固液比为1.087 g·L^(-1)时,溶胶ζ电位绝对值达到45.4 mV,溶胶的稳定性最好,可以得到结构完整的介孔状前驱体。铝掺杂使得锂离子筛前驱体的比表面积从5.22 m^(2)·g^(-1)增加到6.16 m^(2)·g^(-1),平均孔容从0.000967 cm^(3)·g^(-1)增加到0.002394 cm^(3)·g^(-1),平均孔径从14.76 nm增加到36.42 nm,晶面出现取向生长,有利于后续锂离子筛前驱体的洗脱、锂离子筛的吸附及循环稳定性。Aluminum doped lithium ion sieve precursors were prepared using an inorganic precipitation-peptization method with Ti(SO_(4))_(2) as the titanium source,CH_(3)COOLi as the lithium source and AICl,as the doping source.The effect of aluminum doping on the stability of Li_(2)TiO_(2)precursor sol and the morphology and composition of the precursor were investigated.Scanning electron microscopy(SEM),X-ray diffraction(XRD),transmission electron microscopy(TEM),X-ray photoelectron spectroscopy(XPS),Zeta potential analyzer was used to characterize the surface morphology,crystal phase composition,surface chemical element composition and their corresponding chemical valences,as well as the dispersibility of the colloidal system.The results indicated that when the solid-liquid ratio of aluminum is 1.087 g·L^(-1),the absolute value of the sol zeta potential reaches 45.4 mV,the stability of the sol is the best and a structurally intact mesoporous precursor can be obtained under calcination at 750 ℃.Aluminum doping increases the specific surface area of the lithium ion sieve precursorfrom 5.22 m^(2)·g^(-1)to 6.16 m^(2)·g^(-1),the average pore volume increases from 0.000967 cm^(3)·g^(-1)to 0.002394 cm^(3)·g^(-1),the average pore size increases from 14.76 nm to 36.42 nm,and the crystal plane exhibits oriented growth,which is beneficial for the subsequent elution of the precursor of the lithium ion sieve,the adsorption and cycling stability of lithium ion sieve.

关 键 词：钛锂离子筛 前驱体 AL掺杂 沉淀胶溶法 取向生长 

分 类 号：O614.3[理学—无机化学]