以硅酸乙酯(TEOS)、乙烯基三甲氧基硅烷(A171)、异丙醇(IPA)和去离子水(H2O)为主要原料制备有机硅溶胶,并采用溶胶-凝胶技术在氢化锆(ZrH1.8)表面制备了溶胶涂层。热失重-差热分析(DSC—TGA)显示,经180℃干燥或600℃烧结处理,涂层物质分别处于阶段稳定状态。通过单因素实验,考察溶胶各组分含量对溶胶粘度的影响,结合单次浸渍提拉涂层样品经180℃干燥和600℃烧结处理后增重率(WGR)及形貌变化,筛选出氢化锆表面制备涂层溶胶各组分最佳摩尔配比为nTEOS:nA171:nPA:nH2O=1:1:5:nH2O(nH2O=4.0~8.0),在此条件下所制备的溶胶,粘度范围为4.2~4.8mPa·S,180℃干燥涂层样品增重率范围为0.10%~0.12%,涂层表面均匀无裂纹,涂层厚度约为0.8~1.0μm;600℃烧结涂层样品增重率范围为0.16%~0.18%,涂层表面存在微裂纹,但无明显崩落,烧结过程伴随涂层致密化,涂层厚度约为0.6μm。
Silica sol coating was prepared on the surface of zirconium hydride (ZrHl.s ) by sol-gel technology using ethyl silicate (TEOS) , vinyl trimethoxy silane ( A171 ) , isopropyl alcohol (IPA) and H2O as main raw materials. Differential scanning calorimetry- differential thermal analysis (DSC-TGA) showed that the material of sol coating was in stable state after drying under 180℃ or sintering under 600℃. Single factor experiment was conducted to study the effects of each component content on viscosity of the sol, weight gain rate (WGR) and morphology changes of single dip-coating samples heat treated under 180 and 600 ℃. The optimal components molar ratio for sol and coating on ZrHI s preparation was determined as nTEOS:nA171:nPA:nH2O=1:1:5: nH2O ( nH2O = 4. 0 - 8.0). Viscosity of the sol with optimized ratio was in the range of 4.2-4.8 mPa ·S. WGR of single dip-coating samples dried at 180℃ was 0. 10%- 0.12%. Their coatings were even, crack-free and 0.8 - 1.0 μm thick. WGR of corresponding samples sintered at 600℃was 0.16%- 0.18%. And there were micro-cracks existed in the coatings but without severe fragmentation. Coating densification occurred in sintering process, and the final thickness was about 0.6 μm.