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碱催化制备溶胶-凝胶ZrO2薄膜及性能研究
Preparation and Characterization of ZrO2 Thin Film by Sol-Gel Method
【Author】 LI Hai-yuan , TANG Yong-xing, HU Li-li (High Power Laser Physics National Laboratory, Shanghai Institute of Optics and Fine Mechanics, Chinese Academy of Sciences, Shanghai 201800, China)
【机构】 中科院上海光学精密机械研究所高功率激光物理国家实验室;
【摘要】 以Zr(OC3H7)4为前驱体,二甘醇为络合剂,在氨水的碱性条件下,水解制备ZrO2溶胶,并加入聚乙烯吡喏烷酮(PVP)来提高膜层的激光损伤阈值,提拉法涂膜。采用粘度、粒度分布、IR、DSC、XRD、AFM等测试手段对溶胶和薄膜性能进行表征。结果表明,ZrO2溶胶具有较好的粘度稳定性;薄膜表面均匀平整;ZrO2-PVP溶胶颗粒粒径分布比ZrO2 溶胶的集中;ZrO2凝胶粉在329℃附近由非晶态转变为四方晶相结构,在600℃时已有单斜晶相结构出现,随温度的升高由四方晶相向单斜晶相结构转变;加入PVP能有效提高膜层的激光损伤阈值,ZrO2膜的激光损伤阈值为10.2 J/cm2 (1 064 am,1 ns),ZrO2-PVP膜的激光损伤阈值为14.17 J/cm2(1 064 nm,1 ns)。
【Abstract】 ZrO2 sol was prepared by sol-gel process from a solution containing zirconium n-propoxide、 ammonia、 PVP and diglycol in ethanol. The thin films were deposited by dip technique. The characterization of ZrO2 sol and films was analyzed by viscosity, Particle size analyzer、IR、DSC、XRD and AFM analysis. The results showed that the sol had a good viscosity stability; The morphology of coatings surface was smooth; The average size distributing of ZrO2 sol particles was dispersed than the size of ZrO2-PVP sol; At 329℃ ,the structure of ZrO2 gel powder changed from amorphous to tetragonal crystalline phase, and monocline crystalline phase appeared at 600℃, then as the heated temperature rising, the structure changed from tetragonal to monocline crystalline phase;The laser induced damage threshold of coating was improved evidently by adding PVP, the LIDT of ZrO2 coating was 10.2 J/cm2( 1 064 ran, 1 ns) ,and the LIDT of ZrO2-PVP coating was 14.17 J/cm2( 1 064 nm, 1 as).
【Key words】 sol-gel; thin film; ZrO2; zirconium n-propoxide; PVP;
- 【会议录名称】 中国硅酸盐学会特种玻璃分会第三届全国特种玻璃会议论文集
- 【会议名称】中国硅酸盐学会特种玻璃分会第三届全国特种玻璃会议
- 【会议时间】2007-05
- 【会议地点】中国湖北武汉
- 【分类号】TB383.2
- 【主办单位】中国硅酸盐学会特种玻璃分会、中国科学院上海光机所