CN114031398A - 一种复合体系高压电、低损耗的压电陶瓷及其制备方法 - Google Patents

一种复合体系高压电、低损耗的压电陶瓷及其制备方法 Download PDF

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CN114031398A
CN114031398A CN202111370621.5A CN202111370621A CN114031398A CN 114031398 A CN114031398 A CN 114031398A CN 202111370621 A CN202111370621 A CN 202111370621A CN 114031398 A CN114031398 A CN 114031398A
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piezoelectric ceramic
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姜旭宇
余洋
王海圣
刘瑞林
柯银鸿
翁新全
许静玲
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Xiamen Niell Electronics Co ltd
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Abstract

本发明公开了一种复合体系高压电、低损耗的压电陶瓷及其制备方法，它涉及压电陶瓷技术领域，在锆钛酸铅体系中引入具有钙钛矿结构锆镍酸铋Bi(Ni1/2Zr1/2)O3和铌锌酸铅Pb(Zn1/ 3Nb2/3)O3与锆钛酸铅形成复合体系的钙钛矿结构的固溶体；其配方分子式为：xBi(Zr1/2Ni1/2)O3‑(0.1‑x)Pb(Zn1/3Nb2/3)O3‑0.9Pb(Zr0.51Ti0.49)O3+y％CeO2。采用上述技术方案后，本发明能够降低介电损耗、具有优异的压电常数，压电性能优异，在低噪音要求领域具有高实用价值。

Description

一种复合体系高压电、低损耗的压电陶瓷及其制备方法
技术领域
本发明涉及压电陶瓷技术领域，具体涉及一种复合体系高压电、低损耗的压电陶瓷及其制备方法。
背景技术
压电陶瓷是实现机械能与电能相互耦合和转化(换能)的一类功能性材料。在先进制造、电子信息、能源探测和国防等领域有着非常广泛的应用，比如，压电驱动器、超声马达、深井下声波探测、换能器和振动传感器等，压电陶瓷材料是整个系统的敏感元件和核心部件。因此，压电陶瓷材料的性能参数，特别是材料的压电性能和介电损耗，直接决定了系统性能的优劣。更高的压电常数，一般意味着系统或器件的主要功能更为优异；而低的介电损耗，意味着器件或系统在长期工作的性能稳定性。陶瓷作为传感器应用，高压电性能意味着传感器具有高灵敏度，低的介电损耗意味着具有更低的噪音信号，因此传感器具有更高的灵敏度。
目前压电材料中应用最广泛的是锆钛酸铅基(PZT)压电陶瓷，分为软性PZT压电陶瓷和硬性PZT压电陶瓷两大类。软性PZT压电陶瓷虽然具有较高的压电常数，但是其损耗也较大；硬性PZT压电陶瓷虽然损耗很低，但是其压电常数也较低。因此，传统的PZT压电陶瓷材料不能满足许多低噪音要求下的应用需要。
有鉴于此，本发明针对上述压电陶瓷未臻完善所导致的诸多缺失及不便，而深入构思，且积极研究改良试做而开发设计出本发明。
发明内容
本发明的目的在于针对现有技术的缺陷和不足，提供一种能够降低介电损耗、具有优异的压电常数，在低噪音要求领域具有高实用价值的复合体系高压电、低损耗的压电陶瓷及其制备方法。
为实现上述目的，本发明采用以下技术方案是：
一种复合体系高压电、低损耗的压电陶瓷，在锆钛酸铅体系中引入具有钙钛矿结构锆镍酸铋Bi(Ni1/2Zr1/2)O3和铌锌酸铅Pb(Zn1/3Nb2/3)O3与锆钛酸铅形成复合体系的钙钛矿结构的固溶体；
其配方分子式为：
xBi(Zr1/2Ni1/2)O3-(0.1-x)Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3+y％CeO2
x＝0.01～0.05，y＝0～0.3。
本发明的另一目的在于提供一种复合体系高压电性能、低损耗的压电陶瓷的制备方法，其包括以下步骤：
步骤一：以NiO、Bi2O3、ZrO2、ZnO、Nb2O5、Pb3O4、TiO2、CeO2为原料，按照配方分子式中Ni、Bi、Zr、Zn、Nb、Pb、Ti、Ce的化学计量比进行配料；
步骤二：将配好的粉料放入行星式球磨机的球磨罐中混合球磨，得到球磨后的粉料；
步骤三：对球磨后的粉料进行预烧，得到预烧后的粉料；
步骤四：对预烧后的粉料进行二次球磨，然后取料烘干，得到烘干后的粉料；
步骤五：向烘干后的粉料中加入PVA溶液，并研磨压制成薄圆坯，对薄圆坯进行排塑处理，得到排塑处理后的薄圆坯；
步骤六：将排塑后的薄圆坯进行烧结，得到烧结后的陶瓷圆片；
步骤七：将烧结后的陶瓷圆片的两面进行抛光，并在陶瓷圆片的两面被上Ag电极，再进行烧银，然后对烧银后的陶瓷圆片进行极化处理，得到压电陶瓷。
进一步，所述步骤二中，球磨时间为13h，行星式球磨机的转速为250r/min。
进一步，所述步骤三中，预烧的温度为850℃，预烧的时间为3h。
进一步，所述步骤四中，二次球磨的时间为24h。
进一步，所述步骤五中，薄圆坯的直径为11mm，排塑温度为650℃。
进一步，所述步骤六中，烧结温度为1180℃，烧结时间为3h。
进一步，所述步骤七中，在140℃硅油中施加3kV/mm的直流电场保持20min进行极化处理。
采用上述技术方案后，本发明复合体系高压电、低损耗的压电陶瓷，通过引入具有钙钛矿结构锆镍酸铋Bi(Ni1/2Zr1/2)O3和铌锌酸铅Pb(Zn1/3Nb2/3)O3与锆钛酸铅形成复合体系的钙钛矿结构的固溶体，获得了一种新的锆镍酸铋-铌锌酸铅-锆钛酸铅系压电陶瓷材料，能够急剧降低介电损耗，同时保证了其具有优异的压电常数，该材料在低噪音要求领域具有很高的实用价值，可以满足许多低噪音要求下的应用需要。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动性的前提下，还可以根据这些附图获得其他的附图。
图1是本发明实施例3中制备得到的锆镍酸铋-铌锌酸铅-锆钛酸铅系压电陶瓷材料的XRD衍射图谱。
图2是本发明实施例3中制备得到的锆镍酸铋-铌锌酸铅-锆钛酸铅系压电陶瓷材料的介电温谱图。
具体实施方式
为了进一步解释本发明的技术方案，下面通过具体实施例来对本发明进行详细阐述。
在本发明的描述中，需要理解的是，术语“中心”、“纵向”、“横向”、“上”、“下”、“前”、“后”、“左”、“右”“竖直”、“水平”、“顶”、“底”、“内”、“外”等指示方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。在本发明的描述中，除非另有说明，“多个”的含义是两个或两个以上。
一种复合体系高压电、低损耗的压电陶瓷，在锆钛酸铅体系中引入具有钙钛矿结构锆镍酸铋Bi(Ni1/2Zr1/2)O3和铌锌酸铅Pb(Zn1/3Nb2/3)O3与锆钛酸铅形成复合体系的钙钛矿结构的固溶体；
其配方分子式为：
xBi(Zr1/2Ni1/2)O3-(0.1-x)Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3+y％CeO2
x＝0.01～0.05，y＝0～0.3。
以下为本发明复合体系高压电、低损耗的压电陶瓷组分的几个具体示例：
实施例1
制备配方分子式为：
xBi(Zr1/2Ni1/2)O3-(0.1-x)Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3+y％CeO2，x＝0.01，y＝0的改性压电陶瓷。
即为：0.01Bi(Zr1/2Ni1/2)O3-0.09Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3
制备方法为：
步骤一：以NiO、Bi2O3、ZrO2、ZnO、Nb2O5、Pb3O4、TiO2、CeO2为原料，按照配方分子式中Ni、Bi、Zr、Zn、Nb、Pb、Ti、Ce的化学计量比进行配料；
步骤二：将配好的粉料放入行星式球磨机的球磨罐中混合球磨13h，行星式球磨机的转速为250r/min，得到球磨后的粉料；
步骤三：对球磨后的粉料在850℃下进行预烧3h，得到预烧后的粉料；
步骤四：对预烧后的粉料进行二次球磨24h，然后取料烘干，得到烘干后的粉料；
步骤五：向烘干后的粉料中加入PVA溶液，并研磨压制成直径11mm的薄圆坯，对薄圆坯在650℃下进行排塑处理，得到排塑处理后的薄圆坯；
步骤六：将排塑后的薄圆坯在1180℃下进行烧结3h，得到烧结后的陶瓷圆片；
步骤七：将烧结后的陶瓷圆片的两面进行抛光，并在陶瓷圆片的两面被上Ag电极，再进行烧银，在140℃硅油中施加3kV/mm的直流电场保持20min进行极化处理，得到配方分子式为：
0.01Bi(Zr1/2Ni1/2)O3-0.09Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3的压电陶瓷。
其性能参数为：d33＝455pC/N，εr＝2407，tanδ＝0.80％，TC＝342℃。
实施例2
制备配方分子式为：
xBi(Zr1/2Ni1/2)O3-(0.1-x)Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3+y％CeO2，x＝0.02，y＝0的改性压电陶瓷。
即为：0.02Bi(Zr1/2Ni1/2)O3-0.08Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3
制备方法为：
步骤一：以NiO、Bi2O3、ZrO2、ZnO、Nb2O5、Pb3O4、TiO2、CeO2为原料，按照配方分子式中Ni、Bi、Zr、Zn、Nb、Pb、Ti、Ce的化学计量比进行配料；
步骤二：将配好的粉料放入行星式球磨机的球磨罐中混合球磨13h，行星式球磨机的转速为250r/min，得到球磨后的粉料；
步骤三：对球磨后的粉料在850℃下进行预烧3h，得到预烧后的粉料；
步骤四：对预烧后的粉料进行二次球磨24h，然后取料烘干，得到烘干后的粉料；
步骤五：向烘干后的粉料中加入PVA溶液，并研磨压制成直径11mm的薄圆坯，对薄圆坯在650℃下进行排塑处理，得到排塑处理后的薄圆坯；
步骤六：将排塑后的薄圆坯在1180℃下进行烧结3h，得到烧结后的陶瓷圆片；
步骤七：将烧结后的陶瓷圆片的两面进行抛光，并在陶瓷圆片的两面被上Ag电极，再进行烧银，在140℃硅油中施加3kV/mm的直流电场保持20min进行极化处理，得到配方分子式为：
0.02Bi(Zr1/2Ni1/2)O3-0.08Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3的压电陶瓷。
其性能参数为：d33＝421pC/N，εr＝2274，tanδ＝0.76％，TC＝348℃。
实施例3：
制备配方分子式为：
xBi(Zr1/2Ni1/2)O3-(0.1-x)Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3+y％CeO2，x＝0.04，y＝0的改性压电陶瓷。
即为：0.04Bi(Zr1/2Ni1/2)O3-0.06Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3
制备方法为：
步骤一：以NiO、Bi2O3、ZrO2、ZnO、Nb2O5、Pb3O4、TiO2、CeO2为原料，按照配方分子式中Ni、Bi、Zr、Zn、Nb、Pb、Ti、Ce的化学计量比进行配料；
步骤二：将配好的粉料放入行星式球磨机的球磨罐中混合球磨13h，行星式球磨机的转速为250r/min，得到球磨后的粉料；
步骤三：对球磨后的粉料在850℃下进行预烧3h，得到预烧后的粉料；
步骤四：对预烧后的粉料进行二次球磨24h，然后取料烘干，得到烘干后的粉料；
步骤五：向烘干后的粉料中加入PVA溶液，并研磨压制成直径11mm的薄圆坯，对薄圆坯在650℃下进行排塑处理，得到排塑处理后的薄圆坯；
步骤六：将排塑后的薄圆坯在1180℃下进行烧结3h，得到烧结后的陶瓷圆片；
步骤七：将烧结后的陶瓷圆片的两面进行抛光，并在陶瓷圆片的两面被上Ag电极，再进行烧银，在140℃硅油中施加3kV/mm的直流电场保持20min进行极化处理，得到配方分子式为：
0.04Bi(Zr1/2Ni1/2)O3-0.06Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3的压电陶瓷。
其性能参数为：d33＝443pC/N，εr＝2388，tanδ＝0.55％，TC＝356℃。
如图1所示为实施例3中制备得到的锆镍酸铋-铌锌酸铅-锆钛酸铅系压电陶瓷材料的XRD衍射图谱。
如图2所示为实施例3中制备得到的锆镍酸铋-铌锌酸铅-锆钛酸铅系压电陶瓷材料的介电温谱图。
实施例4
制备配方分子式为：
xBi(Zr1/2Ni1/2)O3-(0.1-x)Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3+y％CeO2，x＝0.04，y＝0.1的改性压电陶瓷。
制备方法为：
步骤一：以NiO、Bi2O3、ZrO2、ZnO、Nb2O5、Pb3O4、TiO2、CeO2为原料，按照配方分子式中Ni、Bi、Zr、Zn、Nb、Pb、Ti、Ce的化学计量比进行配料；
步骤二：将配好的粉料放入行星式球磨机的球磨罐中混合球磨13h，行星式球磨机的转速为250r/min，得到球磨后的粉料；
步骤三：对球磨后的粉料在850℃下进行预烧3h，得到预烧后的粉料；
步骤四：对预烧后的粉料进行二次球磨24h，然后取料烘干，得到烘干后的粉料；
步骤五：向烘干后的粉料中加入PVA溶液，并研磨压制成直径11mm的薄圆坯，对薄圆坯在650℃下进行排塑处理，得到排塑处理后的薄圆坯；
步骤六：将排塑后的薄圆坯在1180℃下进行烧结3h，得到烧结后的陶瓷圆片；
步骤七：将烧结后的陶瓷圆片的两面进行抛光，并在陶瓷圆片的两面被上Ag电极，再进行烧银，在140℃硅油中施加3kV/mm的直流电场保持20min进行极化处理，得到配方分子式为：
0.04Bi(Zr1/2Ni1/2)O3-0.06Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3+0.1％CeO2的压电陶瓷。
其性能参数为：d33＝466pC/N，εr＝2392，tanδ＝0.97％，TC＝358℃。
实施例1-4中的性能参数测试结果具体见表1。
表1：
Figure BDA0003362326730000071
本发明提供的锆镍酸铋-铌锌酸铅-锆钛酸铅复合体系压电陶瓷材料具有较低的介电损耗(tanδ＝0.5％～0.8％)和优异的压电常数，与传统的软性PZT压电陶瓷材料相比，介电损耗显著降低，压电d33基本保持不变；而与传统的硬性压电陶瓷材料相比起来，介电损耗基本与其一致，压电d33显著提高，综合来说，本发明的压电陶瓷材料兼具软性陶瓷压电常数优异和硬性压电陶瓷材料介电损耗小的优点于一身，本发明的压电陶瓷材料可满足高电压致动、高频换能器、传感器等敏感元器件在低噪音要求下的服役使用，在低噪音电子器件中具有实际应用价值，可以满足许多低噪音要求下的应用需要。
本发明提供的高压电、低损耗的压电陶瓷材料制备工艺简单稳定，操作方便，适于大规模工业生产的推广，具有实际的应用价值和广泛的应用前景。
以上所述，仅用以说明本发明的技术方案而非限制，本领域普通技术人员对本发明的技术方案所做的其它修改或者等同替换，只要不脱离本发明技术方案的精神和范围，均应涵盖在本发明的权利要求范围当中。

Claims (10)

1.一种复合体系高压电、低损耗的压电陶瓷,其特征在于：在锆钛酸铅体系中引入具有钙钛矿结构锆镍酸铋Bi(Ni1/2Zr1/2)O3和铌锌酸铅Pb(Zn1/3Nb2/3)O3与锆钛酸铅形成复合体系的钙钛矿结构的固溶体；
其配方分子式为：
xBi(Zr1/2Ni1/2)O3-(0.1-x)Pb(Zn1/3Nb2/3)O3-0.9Pb(Zr0.51Ti0.49)O3+y％CeO2
2.根据权利要求1所述的一种复合体系高压电、低损耗的压电陶瓷，其特征在于：x＝0.01～0.05，y＝0～0.3。
3.一种复合体系高压电、低损耗的压电陶瓷的制备方法，其特征在于：其包括以下步骤：
步骤一：以NiO、Bi2O3、ZrO2、ZnO、Nb2O5、Pb3O4、TiO2、CeO2为原料，按照配方分子式中Ni、Bi、Zr、Zn、Nb、Pb、Ti、Ce的化学计量比进行配料；
步骤二：将配好的粉料放入行星式球磨机的球磨罐中混合球磨，得到球磨后的粉料；
步骤三：对球磨后的粉料进行预烧，得到预烧后的粉料；
步骤四：对预烧后的粉料进行二次球磨，然后取料烘干，得到烘干后的粉料；
步骤五：向烘干后的粉料中加入PVA溶液，并研磨压制成薄圆坯，对薄圆坯进行排塑处理，得到排塑处理后的薄圆坯；
步骤六：将排塑后的薄圆坯进行烧结，得到烧结后的陶瓷圆片；
步骤七：将烧结后的陶瓷圆片的两面进行抛光，并在陶瓷圆片的两面被上Ag电极，再进行烧银，然后对烧银后的陶瓷圆片进行极化处理，得到压电陶瓷。
4.根据权利要求3所述的一种复合体系高压电、低损耗的压电陶瓷的制备方法，其特征在于：所述步骤二中，球磨时间为13h，行星式球磨机的转速为250r/min。
5.根据权利要求3所述的一种复合体系高压电、低损耗的压电陶瓷的制备方法，其特征在于：所述步骤三中，预烧的温度为850℃，预烧的时间为3h。
6.根据权利要求3所述的一种复合体系高压电、低损耗的压电陶瓷的制备方法，其特征在于：所述步骤四中，二次球磨的时间为24h。
7.根据权利要求3所述的一种复合体系高压电、低损耗的压电陶瓷的制备方法，其特征在于：所述步骤五中，薄圆坯的直径为11mm，排塑温度为650℃。
8.根据权利要求3所述的一种复合体系高压电、低损耗的压电陶瓷的制备方法，其特征在于：所述步骤六中，烧结温度为1180℃，烧结时间为3h。
9.根据权利要求3所述的一种复合体系高压电、低损耗的压电陶瓷的制备方法，其特征在于：
10.根据权利要求3所述的一种复合体系高压电、低损耗的压电陶瓷的制备方法，其特征在于：所述步骤七中，在140℃硅油中施加3kV/mm的直流电场保持20min进行极化处理。
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Application publication date: 20220211