CN108585851A - 一种铌酸钠基无铅无钾大功率压电陶瓷及其制备方法 - Google Patents

一种铌酸钠基无铅无钾大功率压电陶瓷及其制备方法 Download PDF

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CN108585851A
CN108585851A CN201810749844.4A CN201810749844A CN108585851A CN 108585851 A CN108585851 A CN 108585851A CN 201810749844 A CN201810749844 A CN 201810749844A CN 108585851 A CN108585851 A CN 108585851A
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左如忠
祁核
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Abstract

本发明涉及一种铌酸钠基无铅无钾大功率压电陶瓷及其制备方法，其特征在于，组成通式为：(1‑z)[(1‑x‑y)NaNbO3+xM1+yABO3]+zM2来表示，其中x、y、z表示摩尔分数，0<x<0.08，0<y<0.08，0<z<0.06，M2为一种或多种金属氧化物，本发明的陶瓷可采用常规陶瓷制备方法制备合成，无铅压电陶瓷不含钾元素，性能稳定性好，具有优良的压电性能和高机械品质因数，适合在大功率换能器领域应用。

Description

一种铌酸钠基无铅无钾大功率压电陶瓷及其制备方法
技术领域
本发明属于功能陶瓷材料领域，具体涉及一种铌酸钠基无铅无钾大功率压电陶瓷及其制备方法。
背景技术
压电陶瓷具有体积小，位移分辨率极高，响应速度快、低电压驱动、输出力大等特点，广泛应用于机电换能器，能将电信号与机械位移相互转换，并应用于传感器、调节控制***。随着在生产中应用的扩展，压电陶瓷换能器逐渐向大功率、微型化方向发展，要求优良压电性能、高机械品质因数Qm、低介电损耗。目前市场上占主导地位的是锆钛酸铅基压电陶瓷材料，然而，这些材料的使用通常都会使用大量的铅，从而带来严重的环境污染问题，因此开发同时具有高压电性能和高机械品质因数的无铅压电陶瓷具有重大的社会与经济价值。
NaNbO3陶瓷在室温下具有反铁电结构，当加入少量第二组元时可稳定其铁电正交相结构。具有铁电正交相的NaNbO3基无铅压电陶瓷一般具有较高的机械品质因数，其机械品质因数Qm值均高于500，从而成为大功率领域研究的潜在对象。然而，这些具有高品质因数的二元系组成一般都具有较低的压电系数~50 pC/N。此外，含钾原材料中的K2CO3在室温空气中极易吸水潮解，使其制备工艺复杂且稳定性差， 钾在高温下极易挥发，使其烧结相对困难。基于以上原因，通过在NaNbO3基体中加入第二和第三钙钛矿组成以及不同的改性掺杂物，有望对结构与性能进行进一步调控，获得同时具有高压电性能和高机械品质因数的无铅无钾压电陶瓷材料，使其无铅陶瓷在大功率器件中的实际应用。
发明内容
本发明是为克服现有技术所不足，提供一种高性能铌酸钠基无铅无钾大功率压电陶瓷及其制备方法，该体系的陶瓷组成同时具有高压电性能和高机械品质因数，不含钾元素，制备工艺简单。
为达到以上目的，本发明所采用的技术方案如下：
一种铌酸钠基无铅无钾大功率压电陶瓷，其特征在于：所述的压电陶瓷的组成由以下通式表示：
(1-z)[(1-x-y)NaNbO3+xM1+yABO3]+zM2；
所述的通式中x，y，z为各元素在材料组分中所占的原子百分比，0<x<0.08，0<y<0.08，0<z<0.06;
所述的通式中的M1选自BaTiO3和LiNbO3中的一种或选为两种时，其摩尔分数之和为1;
所述的通式中的ABO3的A选自Ba2+、Ca2+、Sr2+、La3+、Bi3+、Na+、Li+中的至少一种；B选自Zr4+、Ti4+、Sn4+、Hf4+、Mg2+、Zn2+、Al3+、Nb5+、Ta5+、Sb5+、W6+中的至少一种；
所述的通式中的ABO3为不同于M1的一种钙钛矿化合物；
所述的通式中的M2选自Na、Li、Ag、Cu、Fe、Cr、Mn、Sb、Ni、Ce、Nd、Sm金属的氧化物中的一种或多种；选多种时，其摩尔分数之和为1。
一种铌酸钠基无铅无钾大功率压电陶瓷的制备方法，其特征在于，具体包括以下步骤：
a、将原料按照通式(1-z)[(1-x-y)NaNbO3+xM1+yABO3]+zM2所示化学组成的化学计量比进行称量化学纯或分析纯的碳酸盐或金属氧化物进行配料；
b、将步骤a配好的原料以酒精或者水为介质，经4-12小时的球磨混料；湿粉经烘干后得到混合粉料；
c、将步骤b得到的混合粉料放置于氧化铝坩埚中煅烧合成，合成温度为850-1000℃，保温2-4小时；重复球磨混料和煅烧工艺一次，完成预煅烧合成；
d、将步骤c得到的预合成粉体经过研碎后仍以酒精或者水为介质球磨6-12小时，干燥后的粉体过100-130目筛后在50-200 MPa的压力下冷压成型直径10 mm、厚度0.5-2 mm的圆片，得到陶瓷坯体；
e、将步骤d得到的陶瓷坯体在空气中常压下采用埋粉末法提供保护气氛烧结，并置于倒放的双坩埚中，烧结温度为1200-1400 oC，烧结时间为1-4小时、升温速率为1-3 oC/min，得到陶瓷样品；
f、将步骤e得到的陶瓷样品经过抛光处理后在两端面涂上银电极，然后置于25-120 oC的硅油中，在2-6 kV/mm的直流电场下保温保压5-30分钟得到铌酸钠基无铅无钾大功率压电陶瓷。
与已有技术相比，本发明的特点以及有益效果体现在：
1、本发明的陶瓷组成同时具有高压电性能和高机械品质因数，可采用传统压电陶瓷的制备技术和工业用原料获得，具有实用性。
2、本发明的无铅压电陶瓷不含钾元素，因此原料不需要易潮解的碳酸钾，制备工艺简单，性能稳定性好。
3、少量的金属氧化物添加剂能够有效降低压电陶瓷烧结温度得到更加致密的陶瓷，且可进一步优化铌酸钠基无铅无钾压电陶瓷的压电性能和机械品质因数。
附图说明
图1为实施例1中组成的介电－温度特性曲线。
图2为实施例1中组成陶瓷样品的X射线衍射图谱。
图3为实施例2中当z=0.005时的样品在1300 oC下烧结2小时后自然表面的扫描电镜照片。
图4为实施例3中当x=0.04时的样品的导纳曲线。
图5为实施例3中当x=0.04时的样品的电滞回线。
具体实施方式
实施例1
a、原料：5.8506g Na2CO3、1.1840g BaCO3、0.3603g CaCO3、14.6727g Nb2O5、0.4793gTiO2、0.4436g ZrO2、0.0522g MnO2；
b、将上述配好的原料以酒精为介质，经6小时的球磨混料；湿粉经烘干后得到混合粉料；
c、将得到的混合粉料放置于氧化铝坩埚中煅烧合成，合成温度为900 oC，保温4小时；重复球磨混料和煅烧工艺一次，完成预煅烧合成；
d、将得到的预合成粉体经过研碎后仍以酒精为介质球磨12小时，干燥后的粉体过100目筛后在100 MPa的压力下冷压成型直径10 mm、厚度1 mm的圆片，得到陶瓷坯体；
e、将得到的陶瓷坯体在空气中常压下采用埋粉末法提供保护气氛烧结，并置于倒放的双坩埚中，烧结温度为1320 oC，烧结时间为2小时、升温速率为3 oC/min，得到陶瓷样品；
f、将得到的陶瓷样品经过抛光处理后在两端面涂上银电极，然后置于120 oC的硅油中，在6 kV/mm的直流电场下保温保压30分钟。
由此得到0.92NaNbO3+0.05BaTiO3+0.03CaZrO3-0.005MnO2的铌酸钠基无铅无钾压电陶瓷。其介电-温度特性曲线如图1，X射线衍射图谱如图2。
测得样品的其它物理性能：居里温度为 192 oC，介电常数为388（1kHz）,介质损耗1%（1 kHz），压电常数为150 pC/N，平面机电耦合系数为15％，机械品质因数480。
实施例2
按上述实施方式依次进行各步骤，其中采用(1-z)[0.9NaNbO3+0.07LiNbO3+0.03BaZrO3]+zCuO为组成的压电陶瓷，预煅烧温度为900 oC、时间为4小时。两次煅烧后以无水乙醇为球磨介质再次球磨24小时。而后成型的坯体在1250-1350 oC的范围内烧结2小时。两端面被银后置于120 oC的硅油中，在6 kV/mm的直流电场下保温保压30分钟。
当z=0.005时的样品在1300 oC下烧结2小时后自然表面的扫描电镜照片如图3所示。测得样品的其它物理性能：居里温度为300 oC，介电常数为190 （1 kHz），介质损耗0.5%（1 kHz），压电常数为55 pC/N，平面机电耦合系数为14％，机械品质因数1000。
实施例3
按上述实施方式依次进行各步骤，其中采用0.99[(0.98-x)NaNbO3+xBaTiO3+0.02CaZrO3]+0.01CuO为组成的压电陶瓷，预煅烧温度为900 oC、时间为4小时。两次煅烧后以无水乙醇为球磨介质再次球磨24小时。而后成型的坯体在1280-1380 oC的范围内烧结2小时。两端面被银后置于120 oC的硅油中，在6 kV/mm的直流电场下保温保压30分钟。
当x=0.04时的样品的导纳曲线如图4所示，电滞回线如图5所示。测得x=0.04样品的其它物理性能：居里温度为235 oC，介电常数为330 （1kHz），介质损耗0.8%（1kHz），压电常数为90 pC/N，平面机电耦合系数为15％，机械品质因数740。

Claims (2)

1.一种铌酸钠基无铅无钾大功率压电陶瓷，其特征在于：所述的压电陶瓷的组成由以下通式表示：
(1-z)[(1-x-y)NaNbO3+xM1+yABO3]+zM2；
所述的通式中x，y，z为各元素在材料组分中所占的原子百分比，0<x<0.08，0<y<0.08，0<z<0.06;
所述的通式中的M1选自BaTiO3和LiNbO3中的一种或选为两种时，其摩尔分数之和为1;
所述的通式中的ABO3的A选自Ba2+、Ca2+、Sr2+、La3+、Bi3+、Na+、Li+中的至少一种；B选自Zr4 +、Ti4+、Sn4+、Hf4+、Mg2+、Zn2+、Al3+、Nb5+、Ta5+、Sb5+、W6+中的至少一种；
所述的通式中的ABO3为不同于M1的一种钙钛矿化合物；
所述的通式中的M2选自Na、Li、Ag、Cu、Fe、Cr、Mn、Sb、Ni、Ce、Nd、Sm金属的氧化物中的一种或多种；选多种时，其摩尔分数之和为1。
2.一种铌酸钠基无铅无钾大功率压电陶瓷的制备方法，其特征在于具体包括以下步骤：
a、将原料按照通式(1-z)[(1-x-y)NaNbO3+xM1+yABO3]+zM2所示化学组成的化学计量比进行称量化学纯或分析纯的碳酸盐或金属氧化物进行配料；
b、将步骤a配好的原料以酒精或者水为介质，经4-12小时的球磨混料；湿粉经烘干后得到混合粉料；
c、将步骤b得到的混合粉料放置于氧化铝坩埚中煅烧合成，合成温度为850-1000℃，保温2-4小时；重复球磨混料和煅烧工艺一次，完成预煅烧合成；
d、将步骤c得到的预合成粉体经过研碎后仍以酒精或者水为介质球磨6-12小时，干燥后的粉体过100-130目筛后在50-200 MPa的压力下冷压成型直径10 mm、厚度0.5-2 mm的圆片，得到陶瓷坯体；
e、将步骤d得到的陶瓷坯体在空气中常压下采用埋粉末法提供保护气氛烧结，并置于倒放的双坩埚中，烧结温度为1200-1400 oC，烧结时间为1-4小时、升温速率为1-3 oC/min，得到陶瓷样品；
f、将步骤e得到的陶瓷样品经过抛光处理后在两端面涂上银电极，然后置于25-120 oC的硅油中，在2-6 kV/mm的直流电场下保温保压5-30分钟得到铌酸钠基无铅无钾大功率压电陶瓷。
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