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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(H_2O)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(ZrH_(1.8))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∶nIPA∶nH_2O=1∶1∶5∶nH_2O(nH_2O=4.0~8.0),在此条件下所制备的溶胶,粘度范围为4.2~4.8 m Pa·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。
The organosilica sol was prepared by using TEOS, A171, IPA and deionized water (H_2O) as main raw materials and the sol - (ZrH_ (1.8)) surface was prepared sol coating. Thermogravimetry-Differential Thermal Analysis (DSC-TGA) showed that the coating materials were in phase stable state after being dried at 180 ℃ or sintered at 600 ℃ respectively. Through the single factor experiment, the influence of sol content on the viscosity of the sol was investigated. Based on the results of the WGR and the morphological changes of the samples after the single dipping coating was dried at 180 ℃ and sintered at 600 ℃, the hydrogenation The optimum mole ratio of the components prepared by zirconium surface coating is nTEOS:nA171:nIPA:nH_2O = 1: 1: 5: nH_2O (nH_2O = 4.0-8.0). The sol prepared under these conditions has the viscosity range of 4.2 ~ 4.8 mPa · S, and the sample weight gain ranged from 0.10% to 0.12% at 180 ℃. The surface of the coating was uniform and crack-free. The thickness of the coating was about 0.8-1.0 μm. The rate ranges from 0.16% to 0.18%. There are micro-cracks on the surface of the coating, but no obvious caving. The sintering process is accompanied by the densification of the coating with the coating thickness of about 0.6 μm.