New Method for the Preparation and Stabilization of Nanoparticulate t‐ZrO2 by a Combined Sol–Gel and Solvothermal Process
New Method for the Preparation and Stabilization of Nanoparticulate t‐ZrO2 by a Combined Sol–Gel and Solvothermal Process
复制标题
溶胶-凝胶和溶剂热相结合制备和稳定纳米颗粒 t-ZrO2 的新方法
DOI：
10.1111/j.1551-2916.2007.01567.x
复制
发表时间：
2007
期刊：
影响因子：
--
通讯作者：
H. Schmidt
中科院分区：
文献类型：
--
作者：
T. Schmidt;M. Mennig;H. Schmidt
采用溶胶凝胶法和溶剂热法相结合的方法制备了尺寸在3~4 nm之间的非稳定化和二氧化硅稳定化氧化锆微晶。在异丁醇、丙酸和水的溶液中加入丙氧锆后，采用溶胶-凝胶法合成了透明的纳米粒子溶胶。非晶态纳米颗粒的平均流体力学直径约为5 nm。随后的溶剂热过程导致了粉末的结晶部分由31wt%的四方(T)相ZrO2组成。加入10mol%的3-甲基丙烯酰氧丙基三甲氧基硅烷(MPTS)后，这一组分增加了一倍，达到61wt%，随后在800℃下焙烧，其含量增加到96wt%，并用Brunauer-Emmett-Teller和高分辨电子显微镜对其进行了表征。
Nonstabilized and silica-stabilized zirconia (ZrO2) crystallites with sizes between 3 and 4 nm were synthesized by a novel combined sol–gel and solvothermal process. After adding zirconium n-propoxide to a solution of isobutanol, propionic acid, and water, a transparent nanoparticulate sol was synthesized by a sol–gel process. The average hydrodynamic diameter of the amorphous ZrO2 nanoparticles was approximately 5 nm. A following solvothermal process led to a crystalline fraction of the powder consisting of 31 wt% tetragonal (t) phase ZrO2. This fraction was doubled to 61 wt% by adding 10 mol% 3-methacryloxypropyl trimethoxysilane (MPTS) and increased to 96 wt% by a subsequent calcination at 800°C. The crystallite sizes were also confirmed by means of Brunauer–Emmett–Teller and high-resolution transmission electron microscopy.