Preparation and characterization of silicon-calcium composite film on piezoelectric ceramic surface
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摘要: 采用溶胶-凝胶法制备了硅钙复合溶胶，并在压电陶瓷表面制备硅钙复合膜，以改善水泥基压电陶瓷复合材料界面。确定了溶胶配比，研究了陈化、低温热处理和硅烷偶联剂对覆硅钙复合膜压电陶瓷接触角、压电和介电性能的影响。结果表明，硅钙复合溶胶中Ca与Si摩尔比>0.2时不利于成膜；提高陈化温度和延长陈化时间可明显减小硅钙复合膜的接触角；硅钙复合膜层数最佳为3层，烧结温度不大于160℃；加入微量硅烷偶联剂可有效改善膜层开裂。制备的硅钙复合膜接触角最小为27°，亲水性好。Abstract: The silica-calcium composite sol was prepared by sol-gel method, and silica-calcium composite film was prepared on the surface of piezoelectric ceramics to improve the interface of cement-based piezoelectric ceramic composites. The sol ratio was determined, and the effects of aging, low temperature heat treatment and silane coupling agent on the contact angle, piezoelectricity and dielectric properties of piezoelectric ceramics with silica-calcium composite film were investigated. The results show that the molar ratio of Ca to Si greater than 0.2 in silica-calcium composite sol is not conducive to film formation; increasing the aging temperature and prolong the aging time can significantly reduce the contact angle; the optimal number of layers of silica-calcium composite film is 3, and sintering temperature is not more than 160℃; the addition of a trace amount of a silane coupling agent can effectively improve the cracking of the film layer. The prepared silica-calcium film has a minimum contact angle of 27° and good hydrophilicity.
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Key words:
- piezoelectric ceramic /
- silicon-calcium composite film /
- contact angle /
- sol-gel method /
- viscosity
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图 1 锆钛酸铅(PZT)压电陶瓷表面的微观形貌SEM图像
Figure 1. SEM images of Pb-based lanthanumdoped zirconate titanates(PZT) piezoelectric ceramic surface
图 2 不同Ca与Si摩尔比的硅钙复合溶胶胶凝时间的对比
Figure 2. Gelation time comparison of silica-calcium composite sol with different molar ratios of Ca to Si
图 3 不同Ca与Si摩尔比的硅钙复合溶胶黏度对比
Figure 3. Viscosity comparison of silica-calcium composite sol with different molar ratios of Ca to Si
图 4 覆硅钙复合膜压电陶瓷性能随陈化温度的变化
Figure 4. Variation of properties of silica-calcium composite film-coated piezoelectric ceramics with aging temperature
图 5 覆硅钙复合膜压电陶瓷性能随陈化时间的变化
Figure 5. Variation of properties of silica-calcium composite film-coated piezoelectric ceramics with aging time
图 6 覆膜压电陶瓷性能随膜层数的变化
Figure 6. Variation of properties of silica-calcium composite film-coated piezoelectric ceramics with the number of layers
图 7 不同层数的压电陶瓷表面硅钙复合膜的金相显微镜图像 (X=100)
Figure 7. Metallographic images of silicon-calcium composite film on piezoelectric ceramic surface with different layers (X=100)
图 8 覆硅钙复合膜压电陶瓷压电常数d33随烧结温度的变化
Figure 8. Variation of piezoelectric constant d33 of silica-calcium composite film-coated piezoelectric ceramics with sintering temperature
图 9 覆硅钙复合膜压电陶瓷烧结前后的性能对比
Figure 9. Performance comparison of silica-calcium composite film-coated piezoelectric ceramics before and after sintering
图 10 未添加和添加硅烷偶联剂KH570的压电陶瓷表面硅钙复合膜的SEM图像
Figure 10. SEM images of piezoelectric ceramic surface silica-calcium composite film with and without silane coupling agent KH570
图 12 压电陶瓷表面硅钙复合膜的EDS图谱
Figure 12. EDS spectrum of piezoelectric cramic surface silion-calcium composite film
图 13 压电陶瓷表面硅钙复合膜的FTIR图谱
Figure 13. FTIR spectra of piezoelectric ceramic surface silion-calcium composite film
表 1 引入钙源的SiO2溶胶稳定性实验结果
Table 1. Experimental results of stability of SiO2 sol incorporating calcium source
Type of calcium source Method (1) Method (2) Ca(CH3COO)2 Produces white floc, the agitation does not disappear, and a milky white sand is formed quickly. Solubility is very slow, and sol gelation occurs when added in small amounts. Ca(NO3)2 Transparent sol, but gelled during aging. Dissolve quickly and completely, no change at room temperature. 
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