CN110240478B - 一种具有优异压电性能材料的制备方法 - Google Patents

一种具有优异压电性能材料的制备方法 Download PDF

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CN110240478B
CN110240478B CN201910510659.4A CN201910510659A CN110240478B CN 110240478 B CN110240478 B CN 110240478B CN 201910510659 A CN201910510659 A CN 201910510659A CN 110240478 B CN110240478 B CN 110240478B
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陈骏
张月云
孙胜东
朱观宇
高柏涛
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Abstract

本发明是一种具有优异压电性能的材料，属于压电功能材料领域。其特征是以PbO、NiO、In2O3、Nb2O5、TiO2为前驱体，采用传统固相法制备xPb(In1/2Nb1/2)O3‑yPb(Ni1/3Nb2/3)O3‑(1‑x‑y)PbTiO3压电陶瓷，要求0.15≤x≤0.25且0.45≤y≤0.55。按照xPb(In1/2Nb1/2)O3‑yPb(Ni1/3Nb2/3)O3‑(1‑x‑y)PbTiO3称取符合化学剂量比的PbO、NiO、In2O3、Nb2O5、TiO2，将称量好的样品在乙醇溶液中进行球磨1～24小时使其充分混匀，球磨后的粉体烘干后放到密封的坩埚中，在600～900℃温度范围内煅烧1‑12小时，煅烧后的产物在乙醇溶液中进行二次球磨1‑12小时，得到的粉体烘干后压制成片，最后在1100‑1300℃温度范围内烧结1‑15小时，冷却后即可得到优异压电性能的材料。该材料制备简单，成本低廉，易于大批量生产，因此具有更为宽广的科学研究与实用价值。

Description

一种具有优异压电性能材料的制备方法
技术领域
本发明涉及一种具有优异压电性能材料的制备方法，属于压电功能材料领域。
背景技术
压电陶瓷由于其优异的铁电、压电性能，广泛的应用在执行器、传感器、超声换能器及多层电容器等多个方面。其中铅基压电陶瓷具有比无铅更高的压电性能，成为目前不可替代的独特材料。近年来，国内外学者一直致力于研究开发更高性能的压电材料，并研究其高性能的机理，使其更好地应用在国防工业及民用企业中。铅基三元系钙钛矿型铁电陶瓷由于其中两种组成成分可以随意与PbTiO3组合形成固溶体，并且有望得到比二元系更高的压电性能，一直是研究的热点方向。Chen Y[1]等人发现Pb(Mg1/3Nb2/3)O3-Pb(Ni1/3Nb2/3)O3-PbTiO3三元体系，其压电系数d33达780pC/N，Zhang SJ[2]等又报道了Pb(Ni1/3Nb2/3)O3-PbHfO3-PbTiO3三元体系，其d33高达970pC/N。本发明采用传统固相合成法制备了一种具有优异压电性能的三元系陶瓷材料(Pb(In1/2Nb1/2)O3-Pb(Ni1/3Nb2/3)O3-PbTiO3),其d33可高达920pC/N，超过了已经报道的绝大多数压电材料的性能，并且该三元系的压电性能远远高于其组成的两个二元系Pb(In1/2Nb1/2)O3-PbTiO3(d33＝322pC/N)和Pb(Ni1/3Nb2/3)O3-PbTiO3(d33＝560pC/N)。本发明专利制作成本低廉，合成工艺简单，易于大批量生产，因而具有更广泛的实用价值和科学研究。到目前为止，本专利体系的优异性能压电材料尚未见报道。
[1]Chen Y,Zhang X,Pan J,et al.Study of the structure and electricalproperties of PMN-PNN-PT ceramics near the morphotropic phase boundary[J].Journal of electroceramics,2006,16(2):109-114.
[2]Tang H,Zhang M F,Zhang S J,et al.Investigation of dielectric andpiezoelectric properties in Pb(Ni1/3Nb2/3)O3–PbHfO3–PbTiO3ternary system[J].Journal of the European Ceramic Society,2013,33(13-14):2491-2497.
发明内容
本发明的目的在于获得一种具有优异压电性能的三元系陶瓷材料(Pb(In1/2Nb1/2)O3-Pb(Ni1/3Nb2/3)O3-PbTiO3)，从而广泛的应用于工业生产与科学研究中。
一种具有优异压电性能材料的制备方法,其特征在于以PbO、NiO、In2O3、Nb2O5、TiO2为前驱体，采用传统固相法制备xPb(In1/2Nb1/2)O3-yPb(Ni1/3Nb2/3)O3-(1-x-y)PbTiO3(0.15≤x≤0.25且0.45≤y≤0.55)三元系高性能压电陶瓷；按照xPb(In1/2Nb1/2)O3-yPb(Ni1/ 3Nb2/3)O3-(1-x-y)PbTiO3称取符合化学剂量比的PbO、NiO、In2O3、Nb2O5、TiO2，将称量好的样品与乙醇溶液进行球磨1～24小时使其充分混匀，球磨后的粉体烘干后放到密封的坩埚中煅烧，煅烧后的产物在乙醇溶液中进行二次球磨1-12小时，得到的粉体烘干后压制成片，烧结冷却后即可得到优异压电性能的材料。
进一步地，所述煅烧温度范围为600～900℃，煅烧时间1-12小时。
进一步地，所述烧结温度范围为1100-1300℃，烧结时间1-15小时。
本发明三元系压电陶瓷材料具有优异的压电性能(d33＝920pC/N)，超过了绝大部分已知的压电材料，并且生产成本低廉，合成工艺简单易行，适合大规模生产，能够广泛的应用于生产研究中。
附图说明
图1为0.23Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.31PbTiO3的粉末x射线衍射图。
图2为0.23Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.31PbTiO3的扫描电子显微镜图。
图3为0.23Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.31PbTiO3在电场下的极化与应变曲线图。
图4为0.2Pb(In1/2Nb1/2)O3-0.49Pb(Ni1/3Nb2/3)O3-0.31PbTiO3的粉末x射线衍射图。
图5为0.2Pb(In1/2Nb1/2)O3-0.49Pb(Ni1/3Nb2/3)O3-0.31PbTiO3的扫描电子显微镜图。
图6为0.2Pb(In1/2Nb1/2)O3-0.49Pb(Ni1/3Nb2/3)O3-0.31PbTiO3在电场下的极化与应变曲线图。
图7为0.17Pb(In1/2Nb1/2)O3-0.52Pb(Ni1/3Nb2/3)O3-0.31PbTiO3的粉末x射线衍射图。
图8为0.17Pb(In1/2Nb1/2)O3-0.52Pb(Ni1/3Nb2/3)O3-0.31PbTiO3在电场下的极化与应变曲线图。
图9为0.19Pb(In1/2Nb1/2)O3-0.5Pb(Ni1/3Nb2/3)O3-0.31PbTiO3的粉末x射线衍射图。
图10为0.19Pb(In1/2Nb1/2)O3-0.5Pb(Ni1/3Nb2/3)O3-0.31PbTiO3在电场下的极化与应变曲线图。
图11为0.22Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.32PbTiO3的粉末x射线衍射图。
图12为0.22Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.32PbTiO3在电场下的极化与应变曲线图。
具体实施方式
实施例一：
利用此发明制备0.23Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.31PbTiO3。按照化学剂量比称取13.6041克PbO，0.6911克NiO，0.9634克In2O3，3.3819克Nb2O5，和1.4941克TiO2。将以上原料与乙醇溶液球磨1-24小时，得到的粉体经烘干后在密封坩埚中600-900℃煅烧1-12小时，煅烧后的粉体加入乙醇溶液继续球磨1-12小时，得到的粉体烘干后压制成片，在1100-1300℃烧结1-15小时，冷却后即可得到致密的优异压电性能的陶瓷材料，压电系数d33为920pC/N。
图1说明0.23Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.31PbTiO3材料是单一的钙钛矿相，图2是该材料的SEM图像，说明其材料致密且晶粒尺寸在10μm以下，图3为电场作用下的极化与应变曲线，其最大极化为36.05μC/cm2，总应变为0.282％。
实施例二：
利用此发明制备0.2Pb(In1/2Nb1/2)O3-0.49Pb(Ni1/3Nb2/3)O3-0.31PbTiO3。按照化学剂量比称取13.6317克PbO，0.7377克NiO，0.8394克In2O3，3.4289克Nb2O5，和1.4971克TiO2。将以上原料与乙醇溶液球磨1-24小时，得到的粉体经烘干后在密封坩埚中600-900℃煅烧1-12小时，煅烧后的粉体加入乙醇溶液继续球磨1-12小时，得到的粉体烘干后压制成片，在1100-1300℃烧结1-15小时，冷却后即可得到致密的优异压电性能的陶瓷材料，压电系数d33为920pC/N。
图4说明0.2Pb(In1/2Nb1/2)O3-0.49Pb(Ni1/3Nb2/3)O3-0.31PbTiO3材料主要是钙钛矿相，其微量的烧绿石相可以忽略，图5是该材料的SEM图像，说明其材料致密且晶粒尺寸在10μm以下，图6为电场作用下的极化与应变曲线，最大极化为35.71μC/cm2，总应变为0.275％。
实施例三：
利用此发明制备0.17Pb(In1/2Nb1/2)O3-0.52Pb(Ni1/3Nb2/3)O3-0.31PbTiO3。按照化学剂量比称取13.6594克PbO，0.7845克NiO，0.7149克In2O3，3.4762克Nb2O5，和1.5002克TiO2。将以上原料与乙醇溶液球磨1-24小时，得到的粉体经烘干后在密封坩埚中600-900℃煅烧1-12小时，煅烧后的粉体加入乙醇溶液继续球磨1-12小时，得到的粉体烘干后压制成片，在1100-1300℃烧结1-15小时，冷却后即可得到致密的优异压电性能的陶瓷材料，压电系数d33为840pC/N。
图7说明0.17Pb(In1/2Nb1/2)O3-0.52Pb(Ni1/3Nb2/3)O3-0.31PbTiO3材料是单一的钙钛矿相，图8为电场作用下的极化与应变曲线，最大极化为34.62μC/cm2，总应变为0.248％。
实施例四：
利用此发明制备0.19Pb(In1/2Nb1/2)O3-0.50Pb(Ni1/3Nb2/3)O3-0.31PbTiO3。按照化学剂量比称取13.6409克PbO，0.7533克NiO，0.7979克In2O3，3.4447克Nb2O5，和1.4981克TiO2。将以上原料与乙醇溶液球磨1-24小时，得到的粉体经烘干后在密封坩埚中600-900℃煅烧1-12小时，煅烧后的粉体加入乙醇溶液继续球磨1-12小时，得到的粉体烘干后压制成片，在1100-1300℃烧结1-15小时，冷却后即可得到致密的优异压电性能的陶瓷材料，压电系数d33为840pC/N。
图9说明0.19Pb(In1/2Nb1/2)O3-0.50Pb(Ni1/3Nb2/3)O3-0.31PbTiO3材料主要为钙钛矿相，其微量的烧绿石相可以忽略。图10为电场作用下的极化与应变曲线，最大极化为34.85μC/cm2，总应变为0.249％。
实施例五：
利用此发明制备0.22Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.32PbTiO3。按照化学剂量比称取13.6271克PbO，0.6923克NiO，0.9231克In2O3，3.3475克Nb2O5，和1.5449克TiO2。将以上原料与乙醇溶液球磨1-24小时，得到的粉体经烘干后在密封坩埚中600-900℃煅烧1-12小时，煅烧后的粉体加入乙醇溶液继续球磨1-12小时，得到的粉体烘干后压制成片，在1100-1300℃烧结1-15小时，冷却后即可得到致密的优异压电性能的陶瓷材料，压电系数d33为840pC/N。
图11说明0.22Pb(In1/2Nb1/2)O3-0.46Pb(Ni1/3Nb2/3)O3-0.32PbTiO3材料是单一的钙钛矿相，图12为电场作用下的极化与应变曲线，最大极化为35.92μC/cm2，总应变为0.286％。

Claims (1)

1.一种具有优异压电性能材料的制备方法,其特征在于以PbO、NiO、In2O3、Nb2O5、TiO2为前驱体，采用传统固相法制备xPb(In1/2Nb1/2)O3-yPb(Ni1/3Nb2/3)O3-(1-x-y)PbTiO3(0.15≤x≤0.25且0.45≤y≤0.55)三元系高性能压电陶瓷；按照xPb(In1/2Nb1/2)O3-yPb(Ni1/3Nb2/3)O3-(1-x-y)PbTiO3称取符合化学剂量比的PbO、NiO、In2O3、Nb2O5、TiO2，将称量好的样品与乙醇溶液进行球磨1～24小时使其充分混匀，球磨后的粉体烘干后放到密封的坩埚中煅烧，煅烧后的产物在乙醇溶液中进行二次球磨1-12小时，得到的粉体烘干后压制成片，烧结冷却后即可得到优异压电性能的材料；
所述煅烧温度范围为600～900℃，煅烧时间1-12小时；
所述烧结温度范围为1100-1300℃，烧结时间1-15小时；
压电系数d33为920pC/N或840pC/N。
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