非水解溶 胶-凝胶法低温制备硅酸锆薄膜  

Preparation of ZrSiO_4 Film via Non-Hydrolytic Sol-Gel Method at Low Temperature

作　　者：曹昉[1] 陈婷[1,2] 查剑锐 江伟辉[1,2] 刘健敏[1] 吴倩[1] 

机构地区：[1]景德镇陶瓷学院材料科学与工程学院,江西景德镇333403 [2]国家日用及建筑陶瓷工程技术研究中心,江西景德镇333001

出　　处：《陶瓷学报》2015年第5期464-469,共6页Journal of Ceramics

基　　金：国家自然科学基金(编号:51362014;51402135);江西省科技厅青年科学基金(编号:20142BAB216006);江西省教育厅青年基金(编号:GJJ13621);景德镇市级科技局项目(编号:701301-323)

摘　　要：采用非水解溶胶-凝胶法于n型单晶硅基片表面制备出硅酸锆薄膜,并对其相组成及表面形貌进行了研究。运用XRD和FE-SEM研究了热处理温度、前驱体浓度和镀膜次数对硅酸锆合成及薄膜形貌的影响。结果表明:在矿化剂Li F引入的条件下,750℃时可以合成硅酸锆粉体,850℃时可以制备出致密光滑的硅酸锆薄膜。与粉体的合成相比,薄膜生长属于二维传质,矿化剂作用于薄膜制备时,反应活性效果减弱。在该温度下,前驱体浓度为0.7 mol·L-1时,通过两次镀膜可以获得表面光滑,致密无开裂的硅酸锆薄膜,而继续升高热处理温度则会导致晶粒长大,加剧二次再结晶作用,薄膜的致密性下降。Zirconium silicate （ZrSiO4） film was prepared on n-type silicon substrate via nonhydrolytic sol-gel method. The phase composition and the microstructure of samples were studied. Meanwhile, the influences of heat treatment temperature, precursor concentration and coating times on the microstructure and the morphology of ZrSiO4film were investigated by means of XRD and FE-SEM. The results indicated that ZrSiO4 powder was synthesized at 750℃ by introducing mineralizer LiF. However, the dense and smooth ZrSiO4 film was fabricated at 850℃ because the ionic migration of the two-dimensional film was more difficult than that of powder, which weakened the synthesis effect of zirconium silicate films correspondingly. At this temperature, the dense and smooth ZrSiO4 film was obtained with the precursor concentration of 0.7 mol · L^-1 after coating twice. Increasing the heat treatment temperature, the ZrSiO4 grain grew and recrystallized, which caused the decrease of film density.

关 键 词：硅酸锆 薄膜 非水解溶胶-凝胶法 致密 

分 类 号：TQ174.75[化学工程—陶瓷工业]