PZT陶瓷粉体的水热合成

doi:10.3724/SP.J.1077.2012.00507

无机材料学报 ›› 2012, Vol. 27 ›› Issue (5): 507-512.DOI: 10.3724/SP.J.1077.2012.00507 CSTR: 32189.14.SP.J.1077.2012.00507

PZT陶瓷粉体的水热合成

朱孔军, 朱仁强, 董娜娜, 顾洪汇, 裘进浩, 季宏丽

(南京航空航天大学机械结构力学及控制国家重点实验室, 南京 210016)

收稿日期:2011-06-02 修回日期:2011-07-26 出版日期:2012-05-10 网络出版日期:2012-03-31
基金资助:
国家自然科学基金(51172108);航空科学基金(2009ZF52058);教育部新世纪优秀人才支持计划(NCET-10-0070), 长江学者创新团队项目(IRT0968);江苏高校优势学科建设工程资助项目

PZT Powders Synthesized by Hydrothermal Method

ZHU Kong-Jun, ZHU Ren-Qiang, DONG Na-Na, GU Hong-Hui, QIU Jin-Hao, JI Hong-Li

(State Key Laboratory of Mechanics and Control of Mechanical Structures, Nanjing University of Aeronautics and Astronautics, Nanjing 210016, China)

Received:2011-06-02 Revised:2011-07-26 Published:2012-05-10 Online:2012-03-31
Supported by:
National Natural Science Foundation of China (51172108);Aeronautical Science Fund (2009ZF52058);Program for New Century Excellent Talents in University (NCET-10-0070);Program for Changjiang Scholars and Innovative Research Team in University (IRT0968);Priority Academic Program Development of the Jiangsu Higher Education Institutions

摘要/Abstract

摘要：

利用水热法合成了单相、立方体形貌且平均颗粒尺寸在1 μm的锆钛酸铅(PZT)陶瓷粉体. 研究了碱度、反应时间对最终产物的影响, 着重研究了不同碱度下Pb缺失的补偿问题. 结果表明: 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. 原料中适当的Pb过量能够有效补偿Pb离子的缺失, 碱度越高, 所需添加的Pb离子的过量程度也就越高. 但过多的Pb离子加入量会导致最终产物中出现第二相.

关键词: PZT 粉体, 水热合成, 铅过量

Abstract:

Lead zirconate titanate (PZT) powders with single-phase, cubic morphology and average size of 1 μm were synthesized using hydrothermal methods. Effects of KOH concentration, hydrothermal treatment time and Pb excess were investigated. The results show that KOH concentration has an important influence on the solid solubility of Pb ion in A-site of PZT perovskite structure. The concentration of Pb²⁺ vacancies increased with the increase of OH^-concentration. However, this kind of deficiency could be compensated by adding more Pb ions in the raw materials, and more Pb ions were needed to add with higher alkaline concentration in the starting solution. But excessive compensation of Pb ions would result in the appearance of the second phase.

Key words: PZT powder, hydrothermal syntheses, Pb excess

中图分类号:

TF125

朱孔军, 朱仁强, 董娜娜, 顾洪汇, 裘进浩, 季宏丽. PZT陶瓷粉体的水热合成[J]. 无机材料学报, 2012, 27(5): 507-512.

ZHU Kong-Jun, ZHU Ren-Qiang, DONG Na-Na, GU Hong-Hui, QIU Jin-Hao, JI Hong-Li. PZT Powders Synthesized by Hydrothermal Method[J]. Journal of Inorganic Materials, 2012, 27(5): 507-512.

图/表 11

图1 不同碱度下所得产物的XRD图谱

Fig. 1 XRD patterns of PZT powders prepared with different KOH concentrations Condition: 200℃, 4 h

Table 1 Crystal cell parameters of PZT powders prepared with different KOH concentrations

Series	Lattice constant /nm		c/a ratio
Series	a	c	c/a ratio
0.5 mol/L	0.399	0.412	1.033
1 mol/L	0.403	0.410	1.017

Table 2 ICP results of PZT powders prepared with different KOH concentrations

Series	KOH /(mol·L^-1)	X	Y
A	0.5	0.542	0.90
B	1	0.544	0.75
C	2	0.493	0.68

图2 不同碱度下产物的SEM照片

Fig. 2 SEM images of PZT powders prepared with different KOH concentrations Condition: 200℃, 4 h

图3 不同反应时间下产物的XRD图谱

Fig. 3 XRD patterns of PZT powders prepared with 1 mol/L KOH Condition: 200℃,1 mol/L KOH

图4 不同反应时间产物的SEM照片

Fig. 4 SEM images of PZT powders prepared for different hydrothermal treatment time Condition: 200℃, 1 mol/L KOH

图5 不同Pb过量度条件下所得产物的XRD图谱

Fig. 5 XRD patterns of PZT powders prepared for with different Pb excesses Condition: 200℃, 4 h, 0.5 mol/L KOH

Table 3 ICP results of PZT powders obtained at 200℃ for 4 h with different experimental parameters

Series	KOH /(mol·L^-1)	Pb excess /mol%	X	Y
A	0.5	0	0.542	0.90
B	0.5	20	0.513	1.05
C	1	0	0.544	0.75
D	1	40	0.514	1.03
E	1	60	0.514	1.03
F	2	0	0.493	0.68
G	2	60	0.512	0.97

图6 不同Pb过量程度条件下所得产物的SEM照片

Fig. 6 SEM images of PZT powders prepared with different Pb excesses Condition: 200℃, 4 h, 0.5 mol/L KOH

图7 不同Pb过量程度条件下所得产物的XRD图谱

Fig. 7 XRD patterns of PZT powders prepared with different Pb excesses Condition: 200℃, 2 mol/L KOH, 4 h

图8 不同Pb过量程度下所得产物的SEM照片

Fig. 8 SEM photographs of PZT powders prepared with different Pb excess Condition: 200℃, 2 mol/L KOH, 4 h

参考文献 15

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