摘要
以正丙醇锆和正硅酸乙酯分别为锆源和硅源,正丙醇为溶剂,无水柠檬酸为辅助添加剂,采用非水解溶胶-凝胶结合浸渍-提拉镀膜工艺在碳化硅(SiC)基底上制备硅酸锆(ZrSiO4)抗氧化薄膜。采用XRD、FT-IR、SEM、EDS等分析测试手段研究了无水柠檬酸辅助ZrSiO4合成影响机理,以及无水柠檬酸添加量、镀膜次数对ZrSiO4合成和薄膜形貌的影响,并研究了薄膜的抗氧化性能。结果表明:无水柠檬酸能促进矿化剂氟化锂(LiF)在正丙醇中的溶解,从而促进纯相ZrSiO4的合成。当无水柠檬酸添加量(与正丙醇锆的摩尔比)为1.1︰1、镀膜次数为5次时可以在SiC基底上获得平整致密、无开裂、膜厚约为500nm的ZrSiO4薄膜。在1450°C高温氧化60h后,未镀膜的SiC基底单位面积增重为7.2354×10-4g/cm2,而镀上ZrSiO4薄膜后,单位面积增重仅为2.2283×10-4g/cm2,且样品表面相对平整、无裂纹,表明制备ZrSiO4薄膜具有优异的高温抗氧化性能。
Zirconium silicate(ZrSiO4)thin film was prepared on the Si C substrate by non-hydrolyzed sol-gel process combined with dip-coating using zirconium n-propoxide and ethyl orthosilicate as zirconium source and silicon source,respectively,using n-propanol as solvent and anhydrous citric acid as auxiliary additives.The effect mechanism of anhydrous citric acid-assisted ZrSiO4 synthesis as well as the effects of anhydrous citric acid addition and coating times on the synthesis of ZrSiO4 and the morphology of the film and the oxidation resistance of the film were studied via XRD,FT-IR,SEM,EDS and other methods.The results showed that anhydrous citric acid could promote the dissolution of the lithium fluoride(Li F)in n-propanol,resulting in the formation of pure ZrSiO4 phase.When the amount of anhydrous citric acid added(molar ratio to zirconium n-propoxide)was 1.1:1 and the number of coating times was 5,dense ZrSiO4 film with the thickness of 500 nm without cracking could be obtained on the Si C substrate.After oxidizing at 1450°C for 60 h,the weight gain per unit area of uncoated Si C substrate was 7.2354×10-4 g/cm2,while that of the sample coated with ZrSiO4 film was only 2.2283×10-4 g/cm2.The surface of the sample was relatively flat and free of cracks after oxidizing process,indicating that the ZrSiO4 film had excellent high temperature oxidation resistance.
作者
胡庆
谭广繁
汤惠东
江伟辉
刘健敏
陈婷
江峰
冯果
HU Qing;TAN Guangfan;TANG Huidong;JIANG Weihui;LIU Jianmin;CHEN Ting;JIANG Feng;FENG Guo(Jingdezhen Ceramic Institute,Jingdezhen 333403,Jiangxi,China;National Engineering Research Center for Domestic and Building Ceramics,Jingdezhen 333001,Jiangxi,China)
出处
《陶瓷学报》
CAS
北大核心
2019年第6期725-731,共7页
Journal of Ceramics
基金
国家自然科学基金(51602136,51662016)
江西省自然科学基金(20171BAB216010)
江西省教育厅科项目(GJJ180710,GJJ180740,GJJ180699)
江西省杰出青年人才资助计划(20171BCB23071)
关键词
硅酸锆薄膜
非水解溶胶-凝胶法
无水柠檬酸
抗氧化
ZrSiO4 thin film
non-hydrolyzed sol-gel
anhydrous citric acid
oxidation resistance
