水热法制备锆钛酸铅基压电陶瓷粉体的研究

发布时间：2018-01-21 11:57

本文关键词： PZT基压电陶瓷 PZT PLZT Pb过量共沉淀结合水热法压电性能　出处：《南京航空航天大学》2011年硕士论文　论文类型：学位论文

【摘要】：PZT基压电陶瓷材料已被广泛应用于传感器、驱动器、换能器等各个领域。因此,对高性能PZT基压电陶瓷的研究具有重要的意义。而陶瓷粉体制备工艺又是其中重要的环节,本研究尝试通过水热法合成高性能PZT和PLZT压电陶瓷粉体,主要研究工作和结果如下: (1)利用一步水热法可以成功合成单相,纯净,立方体形貌且平均颗粒尺寸在1μm的PZT陶瓷粉体,是品质非常良好的陶瓷烧结用原料粉体。碱度对最终PZT产物A位Pb离子的固溶程度有着重要的影响。碱度越高,A位缺失的Pb离子就越多。但这种缺失是可以通过在原料中添加过量的Pb离子来补偿的,碱度越高,所需补偿的Pb离子就越多,所需添加的Pb离子的过量程度也就越高。但在特定碱度下不是Pb离子可以无限过量的,过多的Pb离子加入量会导致最终产物中出现第二相。实验证明,反应温度200℃,反应时间4 h,碱度2M,Pb过量80%的水热条件下所得粉体通过常压烧结工艺得到的PZT压电陶瓷具有最优的压电性能。性能参数为:d33=225pC/N,kp=44.6%,Qm=305.4。 (2)利用一步水热法合成PLZT粉体过程中,原料在反应溶液中混合的均匀程度会影响到最终产物的物相。当原料在水热反应前达到分子或原子级均匀混合,将非常有利于PLZT晶相的生成。在反应溶液中加入适量的表面活性剂CTAB,能够抑制针状La(OH)3杂相的出现。在反应温度为200℃,反应时间为8 h的水热条件下,当CTAB的添加量为0.05 mol/L时可以得到单相PLZT陶瓷粉体。 (3)利用共沉淀法辅助水热合成PLZT粉体的试验中,在反应温度为200oC,反应时间为24h,矿化剂KOH浓度为5M的水热反应条件下,能够合成PLZT纳米球壳结构,球壳直径大概在4nm左右。矿化剂KOH的浓度对最终PLZT产物的形貌和成分有重要的影响。当矿化剂浓度过高达到7M时,水热条件下无定形前驱体在溶液中的溶解度很高,从而发生快速形核,形成了大量PLZT晶核。相反,当矿化剂浓度较低为2M时,无定形固态颗粒转变形成颗粒状的PLZT纳米颗粒;当矿化剂浓度达到合适的5M时,得到了PLZT球壳结构。此外,KOH浓度对最终PLZT产物中La, Zr和Ti元素影响较小,对Pb离子影响较大,因为不同KOH浓度下会在PLZT中产生A位Pb空位。感谢国家自然科学基金(No. 50872053)、“新世纪优秀人才支持计划”(NCET-10-0070)、教育部重点科学与技术培育基金项目(No. 707031)的资助。
[Abstract]:PZT based piezoelectric ceramics have been widely used in various fields of sensors, actuators, transducers and so on. Therefore, it is important to study the high performance of PZT based piezoelectric ceramics and ceramic powder preparation technology is one of the important issues, this study attempts to synthesis of high performance PZT and PLZT piezoelectric ceramic powder by hydrothermal method, the main research work and results are as follows:
(1) using a one-step hydrothermal method can be successfully synthesized single phase pure cubic morphology and average size of PZT ceramic powder 1 m body, with raw powder sintering quality was very good. Have an important influence on the final product A PZT alkalinity Pb ion solution alkalinity. The higher the Pb ion A deletion. The more but this is missing can be compensated by adding an excess of Pb ions in the raw material, the higher basicity, Pb ions are required for the compensation of the more excess required degree of Pb ions added is higher. But the specific alkalinity is not Pb ion unlimited excessive, excessive amount of Pb ions leads to the appearance of the second phase of the final product. The experimental results show that the reaction temperature is 200 DEG C, the reaction time is 4 h, alkalinity 2M, water and heat conditions in excess of 80% Pb under the powder by Pressureless Sintering of PZT piezoelectric ceramics with optimal pressure Electrical performance. The performance parameters are: d33=225pC/N, kp=44.6%, Qm=305.4.
(2) the synthesis of PLZT powder by one-step hydrothermal method, uniform mixing of raw materials in the reaction solution will affect the final product phase. When the raw materials reach the atomic or molecular level mixing in the hydrothermal reaction, will be very conducive to the formation of PLZT phase. The addition of surface active amount agent CTAB in the reaction solution, can inhibit the acicular La (OH) 3 phase. The reaction temperature is 200 DEG C, the reaction time is 8 h under hydrothermal conditions, when adding 0.05 CTAB to mol/L could be obtained when single-phase PLZT ceramic powder.
(3) the test of heat assisted water synthesis of PLZT powder by co precipitation, the reaction temperature is 200oC, reaction time was 24h, KOH concentration of hydrothermal mineralization agent under 5M reaction conditions to synthesis of PLZT nano spherical shell structure, shell diameter was about 4nm. The concentration of mineralization has important influence agent KOH on the final PLZT product appearance and composition. When the mineralizer concentration is too high to 7M, under hydrothermal conditions no amorphous precursor solubility in solution is very high, resulting in rapid nucleation, the formation of a large number of PLZT nuclei. On the contrary, when the mineralizer concentration is low to 2M, amorphous solid particle transformation of PLZT nanoparticles formed granular; when the mineralizer concentration reached the appropriate 5M, PLZT spherical shell structure is obtained. In addition, the concentration of KOH on the final PLZT product in La, effects of Zr and Ti elements is small, a greater impact on the Pb ion, because of the different concentration of KOH produced in PLZT A Pb vacancy. Thank the National Natural Science Foundation of China (No. 50872053), the new century excellent talent support plan (NCET-10-0070) and the Ministry of education's key science and technology cultivation fund project (No. 707031).

【学位授予单位】：南京航空航天大学
【学位级别】：硕士
【学位授予年份】：2011
【分类号】：TB383.3

【引证文献】