CN103214240B - 压电陶瓷材料、烧结体及其制备方法、压电陶瓷器件 - Google Patents

压电陶瓷材料、烧结体及其制备方法、压电陶瓷器件 Download PDF

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CN103214240B
CN103214240B CN201310091453.5A CN201310091453A CN103214240B CN 103214240 B CN103214240 B CN 103214240B CN 201310091453 A CN201310091453 A CN 201310091453A CN 103214240 B CN103214240 B CN 103214240B
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sintered compact
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piezoelectric ceramics
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CN103214240A (zh
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苏绍华
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AAC Precision Manufacturing Technology Changzhou Co Ltd
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Abstract

本发明提供一种压电陶瓷材料，所述压电陶瓷材料含有用化学通式：PbZraTib(Nb2/3Ni1/3)1-a-b O3+c%BaW0.5Cu0.5O3+d%SiO2表示且满足如下关系的主要组分：0.1≤a≤0.4，0.2≤b≤0.5，0.1≤c≤3，0.05≤d≤1。本发明采用的低温烧结可以降低能耗、减小PbO的挥发，既避免陶瓷组分的波动及偏离设计组成，也减轻了挥发对环境的污染，同时还减轻了对烧结设备的腐蚀、在多层器件中，一般用Ag/Pd合金做内电极，以防止电极在烧结过程中的氧化，如果降低烧结温度，可以降低Ag/Pd合金中Pd的比例甚至采用纯Ag电极，大大降低器件的成本。

Description

压电陶瓷材料、烧结体及其制备方法、压电陶瓷器件
技术领域
本发明涉及一种高压电性能的压电陶瓷材料、烧结体、压电陶瓷器件及采用所述压电陶瓷材料的烧结体的制备方法。
背景技术
自1954年人们发现了PZT锆钛酸铅压电陶瓷后，美国、日本、荷兰等许多国家对压电陶瓷系统进行了详尽的研究，并且随着研制的深入派生出了一系列性能优越的PZT压电陶瓷材料，压电陶瓷材料的应用范围也大大拓展。其中以锆钛酸铅为基础，用多种元素改进的三元系、四元系压电陶瓷也都应运而生。
为了得到为得到高性能的压电陶瓷，目前多采用对Pb(Zr，Ti)O3改性的A位（Pb）或B位（Zr,Ti）进行部分置换，并改变锆钛比以达到调整性能的目的。制备方法多采用普通固相烧结法，即通过对预烧后的粉末与一定的粘结剂等配比，干压成型后来进行烧结。这种烧结方法不但不能满足压电元器件日益多元化和复杂化的要求，同时需要较高的烧结温度(1200℃-1300℃)，也不利于成本的降低，而且在烧结过程中PbO挥发严重，不仅会损害人类的健康以及污染环境，还会导致实际成分的偏离，从而使性能改变，铅的挥发还会对烧结设备的加热棒造成腐蚀，降低了设备的使用寿命。
随着表面贴装技术（SMT）的发展，多层压电陶瓷以其高效率、小型化、功能集成化备受市场青睐，这就要求内电极和陶瓷必需共烧合成。银的熔点为961℃，在此温度之上一般采用钯银合金作为共烧电极，随着钯含量的升高，其价格将带动产品成本的大幅升高。
发明内容
因此，本发明采用的低温烧结可以降低能耗、减小PbO的挥发，既避免陶瓷组分的波动及偏离设计组成，也减轻了挥发对环境的污染，同时还减轻了对烧结设备的腐蚀、在多层器件中，一般用Ag/Pd合金做内电极，以防止电极在烧结过程中的氧化，如果降低烧结温度，可以降低Ag/Pd合金中Pd的比例甚至采用纯Ag电极，大大降低器件的成本。
为了解决上述问题，本发明提供了一种压电陶瓷材料，所述压电陶瓷材料含有用化学通式:
PbZraTib(Nb2/3Ni1/3)1-a-bO3+c%BaW0.5Cu0.5O3+d%SiO2表示且满足如下关系的主要组分：0.1≤a≤0.4，0.2≤b≤0.5，0.1≤c≤3，0.05≤d≤1。
优选的，所述压电陶瓷烧结体是通过烧制如权利要求1所述的压电陶瓷材料而得到的烧结体。
一种压电陶瓷烧结体的制备方法，所述制备方法包括如下步骤：
配料：按PbZraTib(Nb2/3Ni1/3)1-a-bO3化学式配比提供压电陶瓷材料的各组分并将所述组分制成粉末，所述组分包括Pb3O4、TiO2、ZrO2、Nb2O5、NiO、CuO、BaCO3、WO3、SiO2；混料：将上述配置好的粉末加1：1质量的蒸馏水混合8小时后烘干；煅烧：将上述烘干后的产物在780-850℃的环境中煅烧3h以合成得到煅烧产物；添加低温助剂和粉碎：按照c%BaW0.5Cu0.5O3+d%SiO2的质量百分比在所述煅烧产物中加入低温助剂，然后粉碎并烘干以形成混合物；制浆：向上述混合物中加入粘结剂、增塑剂、分散剂、溶剂并混合以形成陶瓷浆料；成型：将所述陶瓷浆料除泡后流延形成陶瓷薄膜；叠置：将上述陶瓷薄膜层叠设置形成层压产物；烧结：在900-950℃的环境中保温3h烧制所述层压产物形成压电陶瓷烧结体。
优选的，在配料步骤中，所述组分通过原料选择或球磨混合的方式制成粉末。
优选的，在配料步骤中，所述粉末的颗粒度中位数控制在2μm以下。
优选的，所述混料步骤中，配置好的粉末与蒸馏水在球磨机内进行混合。
优选的，在添加低温助剂和粉碎步骤中，所述BaW0.5Cu0.5O3是CuO、BaCO3、WO3按照化学式配比混合并在600-650℃温度中煅烧得到。
优选的，在添加低温助剂和粉碎步骤中，粉粹后的混合物的粒度分布在中位数1μm以下。
一种压电陶瓷器件，所述压电陶瓷器件通过电极极化上述的压电陶瓷烧结体形成的。
优选的，所述压电陶瓷器件在极化电场范围为2500‐3500V/mm的空气中极化5秒得到。
相较于相关技术，本发明采用的低温烧结可以降低能耗；减小PbO的挥发，即避免陶瓷组分的波动及偏离涉及组成，也减轻了挥发对环境的污染，同时还减轻了对烧结设备的腐蚀；在多层器件中，一般用Ag/Pd合金做内电极，以防止电极在烧结过程中的氧化，如果降低烧结温度，可以降低Ag/Pd合金中Pd的比例甚至采用纯Ag电极，大大降低器件的成本。
粒度控制与低熔点添加物在降低烧结温度的同时，保证了材料的压电性能而且成本低廉、工艺简单,便于工业化应用。
附图说明
为了更清楚地说明本发明实施例中的技术方案，下面将对实施例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的前提下，还可以根据这些附图获得其它的附图，其中：
图1是不同烧结温度的陶瓷性能对比；
图2是本发明压电陶瓷烧结体在920℃温度下烧结的陶瓷断面的显微形貌；
图3是在920℃温度下烧结的陶瓷断面的能谱。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
本发明提供本发明提供了一种压电陶瓷材料，所述压电陶瓷材料含有用化学通式:
PbZraTib(Nb2/3Ni1/3)1-a-bO3+c%BaW0.5Cu0.5O3+d%SiO2表示且满足如下关系的主要组分：0.1≤a≤0.4，0.2≤b≤0.5，0.1≤c≤3，0.05≤d≤1。通过调整a、b的配比，来调整其性能，最终使其达到高压电性能；通过调整c、d的量，并在煅烧后粉粹时添加来降低烧结温度。
本发明同时提供一种采用上述压电陶瓷材料加工形成压电陶瓷烧结体的制备方法，其通过控制原料和预烧后粉末的粒度，通过添加低温烧结助剂，使用流延成型法制备所需低温压电陶瓷烧结体，然后通过在极化电场范围为2500‐3500V/mm的空气中极化5秒得到所需要的压电陶瓷器件，具体包括如下步骤：
步骤S1，配料：按PbZraTib(Nb2/3Ni1/3)1-a-bO3化学式配比提供压电陶瓷材料的各组分并将所述组分制成粉末，所述组分包括Pb3O4、TiO2、ZrO2、Nb2O5、NiO、CuO、BaCO3、WO3、SiO2。
按照化学式的配比计算各原料组分的质量，用精密电子天平称量，通过原料选择或球磨等方法使上述各组分的颗粒度中位数控制在2μm以下，以提高原料的反应活性。
步骤S2，混料：将上述配置好的粉末加1：1质量的蒸馏水混合8小时后烘干。
配置好的粉末与蒸馏水在球磨机内进行混合使混合更加均匀。
步骤S3，煅烧：将上述烘干后的产物在780-850℃的环境中煅烧3h以合成得到煅烧产物；
步骤S4，添加低温助剂和粉碎：按照c%BaW0.5Cu0.5O3+d%SiO2的质量百分比在所述煅烧产物中加入低温助剂，然后粉碎并烘干以形成混合物。
其中，所述BaW0.5Cu0.5O3是CuO、BaCO3、WO3按照化学式配比混合并在600-650℃温度中煅烧得到。然后使用球磨粉碎上述混合物，使所述混合物的粒度分布在中位数1μm以下并烘干。微珠球磨提高了分体的比表面积，使粉末的活性增强，增大了烧结的驱动力，进而降低了陶瓷的烧结温度；低温助剂在烧结前期形成液相，促进了烧结，在烧结后期，玻璃料成分部分进入主晶相晶格，从而也起到了掺杂改性的作用。
另外，参照图1所示，在不同烧结温度下的性能对比，其中，1130℃的为未加低温助剂烧结的性能，880-1000℃的为加低温助剂后烧结的性能，可以看出，添加低温助剂后，在保持性能的前提下，烧结温度可降低约200℃。
步骤S5，制浆：向上述混合物中加入粘结剂、增塑剂、分散剂、溶剂并混合以形成陶瓷浆料。
其中，所述制浆所加入的粘结剂、增塑剂、分散剂、溶剂如下表1所示。
表1
步骤S6，成型：将所述陶瓷浆料除泡后流延形成陶瓷薄膜。
成型陶瓷薄膜的方法主要有四种；轧膜成型、流延成型、干压成型和静水压成型。轧膜成型适用于薄片元件；流延成型适合于更薄的元件，膜厚可以小于10μm；干压成型适合于块状元件；静水压成型适合于异形或块状元件。除了静水压成型外，其他成型方法都需要有粘合剂，粘合剂一般占原料重量的3％左右。成型以后需要排胶。粘合剂的作用只是利于成型，但它是一种还原性强的物质，成型后应将其排出以免影响烧结质量。
步骤S7，叠置：将上述陶瓷薄膜层叠设置形成层压产物；
步骤S8，烧结：在900-950℃的环境中保温3h烧制所述层压产物形成压电陶瓷烧结体
如图2所示，通过上述制备方法在920℃温度环境下形成的压电陶瓷烧结体的断面的显微形貌图，可以看出，陶瓷烧结致密，晶粒大小均匀，在2μm左右，晶界明显。另外，如图3所示，是该压电陶瓷烧结体的断面的能谱。
在所述压电陶瓷烧结体上形成电极层以实现压电陶瓷的被电极，其中可选用的电极材料有银、铜、金、铂等。形成所述电极层的方法有真空蒸发、化学沉积等多种。在本实施方式中采用的是，涂上银浆，在空气中烧制电极层。
将形成了电极层的压电陶瓷烧结体置于空气中，并在2500‐3500V/mm的极化电场中极化5秒得到，然后去除电场，如此获得上述压电陶瓷烧结体施行电极极化的压电陶瓷器件。
将所述压电陶瓷器件按照国标进行测试并计算压电性能，其中920℃具体样品测试结果详见表2。
表2
其中，通过测量样品尺寸和LCR来计算得到介电常数；
由此，可以看出本发明粒度控制与低熔点添加物在降低烧结温度的同时，保证了材料的压电性能而且成本低廉、工艺简单，便于工业化应用。
另外，本发明采用的低温烧结可以降低能耗、减小PbO的挥发，既避免陶瓷组分的波动及偏离设计组成，也减轻了挥发对环境的污染，同时还减轻了对烧结设备的腐蚀、在多层器件中，一般用Ag/Pd合金做内电极，以防止电极在烧结过程中的氧化，如果降低烧结温度，可以降低Ag/Pd合金中Pd的比例甚至采用纯Ag电极，大大降低器件的成本。
以上所述仅为本发明的实施例，并非因此限制本发明的专利范围，凡是利用本发明说明书及附图内容所作的等效结构或等效流程变换，或直接或间接运用在其它相关的技术领域，均同理包括在本发明的专利保护范围内。

Claims (8)

1.一种压电陶瓷烧结体的制备方法，其特征在于，所述制备方法包括如下步骤：
配料：按PbZraTib(Nb2/3Ni1/3)1-a-bO3化学式配比且满足0.1≤a≤0.4，0.2≤b≤0.5提供压电陶瓷材料的各组分并将所述组分制成粉末，所述组分包括Pb3O4、TiO2、ZrO2、Nb2O5、NiO、CuO、BaCO3、WO3、SiO2；
混料：将上述配置好的粉末加1：1质量的蒸馏水混合8小时后烘干；
煅烧：将上述烘干后的产物在780-850℃的环境中煅烧3h以合成得到煅烧产物；
添加低温助剂和粉碎：按照c％BaW0.5Cu0.5O3+d％SiO2的质量百分比且满足0.1≤c≤3，0.05≤d≤1在所述煅烧产物中加入低温助剂，然后粉碎并烘干以形成混合物；
制浆：向上述混合物中加入粘结剂、增塑剂、分散剂、溶剂并混合以形成陶瓷浆料；
成型：将所述陶瓷浆料除泡后流延形成陶瓷薄膜；
叠置：将上述陶瓷薄膜层叠设置形成层压产物；
烧结：在900-950℃的环境中保温3h烧制所述层压产物形成压电陶瓷烧结体。
2.根据权利要求1所述的压电陶瓷烧结体的制备方法，其特征在于，在配料步骤中，所述组分通过原料选择或球磨混合的方式制成粉末。
3.根据权利要求1所述的压电陶瓷烧结体的制备方法，其特征在于，在配料步骤中，所述粉末的颗粒度中位数控制在2μm以下。
4.根据权利要求1所述的压电陶瓷烧结体的制备方法，其特征在于，所述混料步骤中，配置好的粉末与蒸馏水在球磨机内进行混合。
5.根据权利要求1所述的压电陶瓷烧结体的制备方法，其特征在于，在添加低温助剂和粉碎步骤中，所述BaW0.5Cu0.5O3是CuO、BaCO3、WO3按照化学式配比混合并在600-650℃温度中煅烧得到。
6.根据权利要求1所述的压电陶瓷烧结体的制备方法，其特征在于，在添加低温助剂和粉碎步骤中，粉粹后的混合物的粒度分布在中位数1μm以下。
7.一种压电陶瓷器件，其特征在于，所述压电陶瓷器件通过电极极化如权利要求1至6任意一项所述方法制备的压电陶瓷烧结体形成的。
8.根据权利要求7所述的压电陶瓷器件，其特征在于，所述压电陶瓷器件在极化电场范围为2500-3500V/mm的空气中极化5秒得到。
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