CN114621007B - 一种低温制备的高性能pzt基多元改性压电陶瓷 - Google Patents

一种低温制备的高性能pzt基多元改性压电陶瓷 Download PDF

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CN114621007B
CN114621007B CN202011466431.9A CN202011466431A CN114621007B CN 114621007 B CN114621007 B CN 114621007B CN 202011466431 A CN202011466431 A CN 202011466431A CN 114621007 B CN114621007 B CN 114621007B
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piezoelectric ceramic
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CN114621007A (zh
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刘洪�
陈浩
朱建国
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Abstract

本发明公开了一种低温制备的高性能PZT基多元改性压电陶瓷材料及其制备方法，该压电陶瓷的通式为Pb1‑x‑yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1‑u‑v‑ wO3表示，0.01≤x≤0.5，0≤y≤1.0,0.01≤u≤0.10,0.01≤v≤0.10,0.01≤w≤0.10。采用固相反应法制备850～960℃低温烧结的PZT改性压电陶瓷粉体，再经过造粒、压片、排胶、烧结、烧银、极化等工艺制备陶瓷材料。结果表明，在850～960℃的烧结温度下制备得到了PZT改性陶瓷材料，其液相烧结特征明显，晶粒均匀、晶粒致密、结晶充分，压电性能大大提高。

Description

一种低温制备的高性能PZT基多元改性压电陶瓷
技术领域
本发明领域属于压电陶瓷材料领域，具体涉及一种低温制备的高性能PZT基多元改性压电陶瓷。
背景技术
PZT是传统的压电陶瓷，具有良好的介电、铁电、压电、热释电、电卡等效应，其原料价格低廉，适于工厂化生产，对其多元改性可以得到适用于多种用途的陶瓷材料。多层压电陶瓷有交替陶瓷层和内部金属电极层。随着科学技术的高速发展，多层压电陶瓷得到了越来越广泛的研究，广泛应用于制动器、转换器、传感器。一般将Ag-Pd电极用于多层陶瓷的内电极，其共烧温度范围为920～980℃。传统PZT压电陶瓷在约1200℃高温下烧结，因此内部电极不能在这么高的温度下使用Ag-Pd电极，而Ag-Pd电极层也会扩散到陶瓷层，导致陶瓷电学性能的恶化，从而影响多层器件的可靠性。
发明内容
本发明的目的在于针对现有技术的不足，本发明的第一个目的是提供一种低温制备的高性能PZT基多元改性压电陶瓷材料配方，该压电陶瓷烧结温度低，并且兼具良好的压电性能；本发明的第二个目的是提供上述低温制备的高性能PZT基多元改性压电陶瓷的制备方法，以降低PZT基多元改性压电陶瓷的烧结温度，同时提高压电性能。
针对本发明的第一个发明目的，本发明提供一种低温制备的高性能PZT基多元改性压电陶瓷，该压电陶瓷的化学通式为Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，0.01≤x≤0.5，0≤y≤1.0,0.01≤u≤0.10,0.01≤v≤0.10,0.01≤w≤0.10。
针对本发明的第二个发明目的，通过在PZT基多元改性压电陶瓷中引入多种元素Li、Cu、W、Mg、Sb、Yb、Ni、Zn、Nb进入A或B位，在850～960℃的烧结温度下，制备得到兼具良好压电性能的PZT基多元改性压电陶瓷，具体工艺步骤如下：
(1)PZT基多元改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，0.01≤x≤0.5，0≤y≤1.0,0.01≤u≤0.10,0.01≤v≤0.10,0.01≤w≤0.10，计算称量各原料，将各原料通过球磨破碎并混合均匀后，在750～850℃下保温2～4h，保温结束后冷却至室温并再次球磨破碎，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入5～10wt％的聚乙烯醇溶液进行造粒，然后将所得粒料压制成片，得到PZT基多元改性陶瓷片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片排胶后在850～950℃下保温烧结2～4h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得得到烧结PZT基多元改性压电陶瓷圆片表面涂覆5～15wt％的银浆后，在650～750℃下保温烧结10～20min，保温结束后冷却至室温，然后在硅油中进行极化，得到高性能PZT基多元改性压电陶瓷。
上述方法中，步骤(1)中两次球磨的具体工艺优选为：以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以100～450rmp的转速球磨10～24h，球磨后进行干燥。所述干燥可以是在烤灯下烘烤2～3小时。
上述方法中，将所得粒料压制成片的具体工艺优选为：在10～20MPa的压力下压制成直径约为10～15mm，厚度约为0.8～1.2mm的高性能PZT基多元改性压电陶瓷片。
上述方法中，步骤(2)中所述聚乙烯醇溶液的浓度为最好为5～10wt％。
上述方法中，步骤(3)中排胶的具体工艺优选为：将步骤(2)所得PZT基多元改性陶瓷片在450～550℃下保温4～10h。
上述方法中，步骤(4)中在硅油中进行极化的具体工艺为：在60～120℃的硅油中，极化场强为2～5kV/mm条件下保持电场强度15～30min。
与现有技术相比，本发明具有以下有益效果：
1、本发明提供的高性能PZT基多元改性压电陶瓷，烧结温度低，为850～950℃并具有良好的压电性能，d33高达623pC/N，在室温下利用安捷伦4294A精密阻抗仪在1kHz的频率下测得介电损耗不大于千分之三，且居里温度大于290℃，如图3所示。
2、本发明提供的低温制备的高性能PZT基多元改性压电陶瓷，其物相为纯钙钛矿相，如图1所示，加入的Li、Cu、W、Mg、Sb、Yb、Ni、Zn、Nb元素提高了烧结活性降低了烧结温度使晶粒致密均匀且生长充分，致密。
附图说明
图1是实施例1～5制备得到的压电陶瓷材料的X射线衍射(XRD)图谱。
图2是实施例1～5制备得到的压电陶瓷材料的压电性能图。
图3是实施例1～5制备得到的压电陶瓷材料的介电常数随温度的变化。
图4是实施例4制备得到的压电陶瓷材料的电声器件示意图。
具体实施方式
下面通过具体实施方式对本发明所述低温制备的高性能PZT基多元改性压电陶瓷作进一步说明。
实施例1
(1)PZT基多元改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3，(x＝0.01,y＝0,u＝0.01,v＝0.01,w＝0.01)计算称量各原料，以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以100rmp的转速球磨24h，球磨后烤灯下烘烤2小时进行干燥得到混合粉料，将所得混合粉料在800℃下保温3h，保温结束后冷却至室温并再次按照相同方法进行第二次球磨，球磨后烤灯下烘烤3小时进行干燥，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入浓度为10wt％的聚乙烯醇溶液进行造粒，然后在10MPa的压力下压制成直径约为10mm，厚度约为1.2mm的PZT基多元改性压电陶瓷圆片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片在550℃下保温4h进行排胶后，在850℃下保温烧结4h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT基多元改性压电陶瓷圆片表面涂覆10wt％的银浆后，在650℃下保温烧结20min，保温结束后冷却至室温，然后在在60℃的硅油中，极化场强为5kV/mm条件下保持电场强度15min进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷。
制得的低温制备的高性能PZT基多元改性压电陶瓷的XRD图谱见图1，图1表明PZT压电陶瓷为纯钙钛矿相；采用中科院声学所的ZJ-3型准静态d33仪，测得的压电系数的d33见图2，为556pC/N；利用安捷伦4980A精密阻抗仪连接温控炉测得介电常数随温度的变化，可从图3得到样品的居里温度为301℃。
实施例2
(1)PZT基多元改性陶瓷粉体的制备
按照通式按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/ 2W1/2]w(Ti,Zr)1-u-v-wO3表示，(x＝0.05,y＝0.2,u＝0.02,v＝0.03,w＝0.02)计算称量各原料，以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以450rmp的转速球磨10h，球磨后烤灯下烘烤3小时进行干燥得到混合粉料，将所得混合粉料在750℃下保温4h，保温结束后冷却至室温并再次按照相同方法进行第二次球磨，球磨后烤灯下烘烤3小时进行干燥，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入浓度为8wt％的聚乙烯醇溶液进行造粒，然后在20MPa的压力下压制成直径约为14mm，厚度约为0.9mm的PZT基多元改性压电陶瓷圆片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片在550℃下保温4h进行排胶后，在900℃下保温烧结3h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT基多元改性压电陶瓷圆片表面涂覆12wt％的银浆后，在700℃下保温烧结10min，保温结束后冷却至室温，然后在在60℃的硅油中，极化场强为2kV/mm条件下保持电场强度30min进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷。
制得的低温制备的高性能PZT基多元改性压电陶瓷的XRD图谱见图1，图1表明PZT压电陶瓷为纯钙钛矿相；采用中科院声学所的ZJ-3型准静态d33仪，测得的压电系数的d33见图2，为583pC/N；利用安捷伦4980A精密阻抗仪连接温控炉测得介电常数随温度的变化，可从图3得到样品的居里温度为298℃。
实施例3
(1)PZT基多元改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，(x＝0.15,y＝0.4,u＝0.03,v＝0.05,w＝0.03)计算称量各原料，以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以300rmp的转速球磨18h，球磨后烤灯下烘烤3小时进行干燥得到混合粉料，将所得混合粉料在850℃下保温2h，保温结束后冷却至室温并再次按照相同方法进行第二次球磨，球磨后烤灯下烘烤2小时进行干燥，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入浓度为10wt％的聚乙烯醇溶液进行造粒，然后在15MPa的压力下压制成直径约为13mm，厚度约为1mm的PZT基多元改性压电陶瓷圆片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片在450℃下保温10h进行排胶后，在950℃下保温烧结2h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT基多元改性压电陶瓷圆片表面涂覆5wt％的银浆后，在750℃下保温烧结10min，保温结束后冷却至室温，然后在在60℃的硅油中，极化场强为4kV/mm条件下保持电场强度16min进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷。
制得的低温制备的高性能PZT基多元改性压电陶瓷的XRD图谱见图1，图1表明PZT压电陶瓷为纯钙钛矿相；采用中科院声学所的ZJ-3型准静态d33仪，测得的压电系数的d33见图2，为601pC/N；利用安捷伦4980A精密阻抗仪连接温控炉测得介电常数随温度的变化，可从图3得到样品的居里温度为301℃。
实施例4
(1)PZT基多元改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，(x＝0.2,y＝0.6,u＝0.04,v＝0.07,w＝0.04)计算称量各原料，以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以200rmp的转速球磨20h，球磨后烤灯下烘烤3小时进行干燥得到混合粉料，将所得混合粉料在800℃下保温3h，保温结束后冷却至室温并再次按照相同方法进行第二次球磨，球磨后烤灯下烘烤3小时进行干燥，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入浓度为10wt％的聚乙烯醇溶液进行造粒，然后在20MPa的压力下压制成直径约为15mm，厚度约为0.8mm的PZT基多元改性压电陶瓷圆片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片在500℃下保温8h进行排胶后，在900℃下保温烧结4h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT基多元改性压电陶瓷圆片表面涂覆15wt％的银浆后，在650℃下保温烧结15min，保温结束后冷却至室温，然后在在60℃的硅油中，极化场强为5kV/mm条件下保持电场强度25min进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷。
制得的低温制备的高性能PZT基多元改性压电陶瓷的XRD图谱见图1，图1表明PZT压电陶瓷为纯钙钛矿相；采用中科院声学所的ZJ-3型准静态d33仪，测得的压电系数的d33见图2，为623pC/N；利用安捷伦4980A精密阻抗仪连接温控炉测得介电常数随温度的变化，可从图3得到样品的居里温度为293℃。
实施例5
(1)PZT基多元改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，(x＝0.25,y＝0.8,u＝0.05,v＝0.08,w＝0.05)计算称量各原料，以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以400rmp的转速球磨11h，球磨后烤灯下烘烤2小时进行干燥得到混合粉料，将所得混合粉料在750℃下保温4h，保温结束后冷却至室温并再次按照相同方法进行第二次球磨，球磨后烤灯下烘烤3小时进行干燥，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入浓度为6wt％的聚乙烯醇溶液进行造粒，然后在18MPa的压力下压制成直径约为10mm，厚度约为1.2mm的PZT基多元改性压电陶瓷圆片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片在500℃下保温7h进行排胶后，在900℃下保温烧结4h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT基多元改性压电陶瓷圆片表面涂覆10wt％的银浆后，在750℃下保温烧结12min，保温结束后冷却至室温，然后在在60℃的硅油中，极化场强为3kV/mm条件下保持电场强度30min进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷。
制得的低温制备的高性能PZT基多元改性压电陶瓷的XRD图谱见图1，图1表明PZT压电陶瓷为纯钙钛矿相；采用中科院声学所的ZJ-3型准静态d33仪，测得的压电系数的d33见图2，为588pC/N；利用安捷伦4980A精密阻抗仪连接温控炉测得介电常数随温度的变化，可从图3得到样品的居里温度为288℃。
实施例6
(1)PZT基多元改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，(x＝0.3,y＝0.1,u＝0.06,v＝0.02,w＝0.06)计算称量各原料，以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以100rmp的转速球磨24h，球磨后烤灯下烘烤2小时进行干燥得到混合粉料，将所得混合粉料在800℃下保温3h，保温结束后冷却至室温并再次按照相同方法进行第二次球磨，球磨后烤灯下烘烤3小时进行干燥，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入浓度为10wt％的聚乙烯醇溶液进行造粒，然后在10MPa的压力下压制成直径约为10mm，厚度约为1.2mm的PZT基多元改性压电陶瓷圆片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片在550℃下保温4h进行排胶后，在850℃下保温烧结4h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT基多元改性压电陶瓷圆片表面涂覆10wt％的银浆后，在650℃下保温烧结20min，保温结束后冷却至室温，然后在在60℃的硅油中，极化场强为5kV/mm条件下保持电场强度15min进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷。
实施例7
(1)PZT基多元改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，(x＝0.35,y＝0.3,u＝0.07,v＝0.04,w＝0.07)计算称量各原料，以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以100rmp的转速球磨24h，球磨后烤灯下烘烤2小时进行干燥得到混合粉料，将所得混合粉料在800℃下保温3h，保温结束后冷却至室温并再次按照相同方法进行第二次球磨，球磨后烤灯下烘烤3小时进行干燥，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入浓度为10wt％的聚乙烯醇溶液进行造粒，然后在10MPa的压力下压制成直径约为10mm，厚度约为1.2mm的PZT基多元改性压电陶瓷圆片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片在550℃下保温4h进行排胶后，在850℃下保温烧结4h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT基多元改性压电陶瓷圆片表面涂覆10wt％的银浆后，在650℃下保温烧结20min，保温结束后冷却至室温，然后在在60℃的硅油中，极化场强为5kV/mm条件下保持电场强度15min进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷。
实施例8
(1)PZT基多元改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，(x＝0.4,y＝0.5,u＝0.08,v＝0.06,w＝0.08)计算称量各原料，以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以100rmp的转速球磨24h，球磨后烤灯下烘烤2小时进行干燥得到混合粉料，将所得混合粉料在800℃下保温3h，保温结束后冷却至室温并再次按照相同方法进行第二次球磨，球磨后烤灯下烘烤3小时进行干燥，得到PZT基多元改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT基多元改性陶瓷粉体中加入浓度为10wt％的聚乙烯醇溶液进行造粒，然后在10MPa的压力下压制成直径约为10mm，厚度约为1.2mm的PZT基多元改性压电陶瓷圆片；
(3)排胶烧结
将步骤(2)所得PZT基多元改性陶瓷片在550℃下保温4h进行排胶后，在850℃下保温烧结4h，得到烧结PZT基多元改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT基多元改性压电陶瓷圆片表面涂覆10wt％的银浆后，在650℃下保温烧结20min，保温结束后冷却至室温，然后在在60℃的硅油中，极化场强为5kV/mm条件下保持电场强度15min进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷
应用例1
将实施例4制备得到的低温制备的高性能PZT基多元改性压电陶瓷材料制备成厚度0.2毫米，直径12毫米的圆片，加上电极、引线、膜片、外壳等做成电声器件，如图4所示。

Claims (8)

1.一种低温制备的高性能PZT基多元改性压电陶瓷，其特征在于该压电陶瓷的化学通式为Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，0.01≤x≤0.5，0≤y≤1.0,0.01≤u≤0.10,0.01≤v≤0.10,0.01≤w≤0.10。
2.权利要求1所述低温制备的高性能PZT基多元改性压电陶瓷的制备方法，其特征在于工艺步骤如下：
(1)PZT改性陶瓷粉体的制备
按照通式Pb1-x-yLixSry(Sb1/2Nb1/2)u[(Ni,Zn)1/3Nb2/3]v[(Cu,Mg,Yb)1/2W1/2]w(Ti,Zr)1-u-v-wO3表示，0.01≤x≤0.5，0≤y≤1.0,0.01≤u≤0.10,0.01≤v≤0.10,0.01≤w≤0.10，计算称量各原料，将各原料通过球磨破碎并混合均匀后，在750～850℃下保温2～4h，保温结束后冷却至室温并再次球磨破碎，得到PZT改性陶瓷粉体；
(2)造粒压片
向步骤(1)所得PZT改性陶瓷粉体中加入聚乙烯醇溶液进行造粒，然后将所得粒料压制成片，得到PZT改性陶瓷片；
(3)排胶烧结
将步骤(2)所得PZT改性陶瓷片排胶后在850～960℃下保温烧结2～4h，得到烧结PZT改性压电陶瓷片；
(4)极化
将步骤(3)所得烧结PZT改性压电陶瓷圆片表面涂覆5～15wt％的银浆后，在650～750℃下保温烧结10～20min，保温结束后冷却至室温，然后在硅油中进行极化，得到低温制备的高性能PZT基多元改性压电陶瓷。
3.根据权利要求2所述低温制备的高性能PZT基多元改性压电陶瓷的制备方法，其特征在于步骤(1)中两次球磨的具体工艺为：以无水乙醇为分散介质，按照各原料总量与无水乙醇的质量比为1:1.5将各原料和无水乙醇加入球磨罐中，在行星球磨机上以100～450rmp的转速球磨10～24h，球磨后进行干燥。
4.根据权利要求3所述低温制备的高性能PZT基多元改性压电陶瓷的制备方法，其特征在于所述干燥是在烤灯下烘烤2～3小时。
5.根据权利要求2～4中任一权利要求所述低温制备的高性能PZT基多元改性压电陶瓷的制备方法，其特征在于步骤(2)中将所得粒料压制成片的具体工艺为：在10～20MPa的压力下压制成直径为10～15mm，厚度为0.8～1.2mm的低温制备的高性能PZT基多元改性压电陶瓷片。
6.根据权利要求2～4中任一权利要求所述低温制备的高性能PZT基多元改性压电陶瓷的制备方法，其特征在于步骤(2)中所述聚乙烯醇溶液的浓度为5～10wt％。
7.根据权利要求2～4中任一权利要求所述低温制备的高性能PZT基多元改性压电陶瓷的制备方法，其特征在于步骤(3)中排胶的具体工艺为：将步骤(2)所得PZT改性陶瓷片在450～550℃下保温4～10h。
8.根据权利要求2～4中任一权利要求所述低温制备的高性能PZT基多元改性压电陶瓷的制备方法，其特征在于步骤(4)中在硅油中进行极化的具体工艺为：在50～120℃的硅油中，极化场强为2～5kV/mm条件下保持电场强度15～30min。
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