CN105622097A - 耐高温压电陶瓷及其制备方法 - Google Patents

耐高温压电陶瓷及其制备方法 Download PDF

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CN105622097A
CN105622097A CN201510961673.8A CN201510961673A CN105622097A CN 105622097 A CN105622097 A CN 105622097A CN 201510961673 A CN201510961673 A CN 201510961673A CN 105622097 A CN105622097 A CN 105622097A
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褚涛
吴康和
张田才
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GUIZHOU ZHENHUA HONGYUN ELECTRONICS CO Ltd
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Abstract

本发明涉及耐高温压电陶瓷及其制备方法。该压电陶瓷的结构通式为：Pb(Zr1/2Ti1/2)x(Ni1/3Nb2/3)y(Sb1/3Nb2/3)z(Mg1/3Nb2/3)1-x-y-zO3+wmol%A，x的取值范围为0.85-0.97，y的取值范围为0.01-0.10，z的取值范围为0.01-0.05，w的取值范围为0.05-2.0，A为碱金属或碱土金属的改性元素。其制备方法包括配料混合；预烧；球磨；干燥；过筛；造粒、成型、冲片、排胶、烧结；被银电极；极化等步骤。本发明解决了现有的压电陶瓷使用温度低且电学性能无法满足要求的问题；可以在200℃以上使用，具有高压电常数、高介电常数。

Description

耐高温压电陶瓷及其制备方法
技术领域
本发明涉及压电陶瓷，尤其涉及耐高温压电陶瓷及其制备方法，属于压电陶瓷生产技术领域。
背景技术
高温压电陶瓷材料被广泛应用于航天、核能、汽车、石化、冶金、发电、地质勘探等众多科研与工业部门。进十年来，随着科学技术的迅猛发展，许多电子设备对所选的压电器件要求越来越高，适用范围和适应环境要求压电材料具有更大的适应性。现有压电陶瓷使用温度一般在-40℃~+120℃，采用压电陶瓷制作蜂鸣片，在高于120℃使用时会使蜂鸣片的性能出现严重恶化，甚至在高于200℃时完全不能使用。因此，研究制造能在高温下使用的压电陶瓷具有十分重要的意义。一般而言，具有较高居里温度的同时，其压电性能就较差，综合电学性能也较差；尤其对于电声器件，要求其具有较高使用温度（耐高温，能在高温条件下正常工作）的同时，还要求具有较高的压电常数d33、介电常数ε和机电耦合系数Kp。研究表示，一种铋层状压电陶瓷，其居里温度Tc大于600℃，但其压电常数d33只有20pC/N；一种BiScO3-PbTiO3体系压电陶瓷有优异的压电特性（Tc≈450℃，d33≈460pC/N），但其综合电学性能较差、Sc2O3的价格昂贵，也不适宜工业生产。因此，开发具有高使用温度（耐高温、能在200℃的高温环境下正常工作），高压电常数（d33≥500pC/N），高机电耦合系数（Kp≥70%），高介电常数（ε≥2000），综合电学性能优异的压电材料，是该领域的一个难题。
发明内容
为了克服现有技术中存在的压电陶瓷材料无法在获得高使用温度的同时具有较高的综合电学性能，不能满足压电器件的使用要求的缺陷，本发明旨在提供一种具有高使用温度、高压电常数、高机电耦合系数和介电常数的耐高温压电陶瓷及其制备方法。
为了实现上述目的，本发明采用以下技术方案，其结构通式为：Pb(Zr1/2Ti1/2)x(Ni1/3Nb2/3)y(Sb1/3Nb2/3)z(Mg1/3Nb2/3)1-x-y-zO3+wmol%A，结构通式中x的取值范围为0.85-0.97，y的取值范围为0.01-0.10，z的取值范围为0.01-0.05，w的取值范围为0.05-2.0，A为碱金属或碱土金属的改性元素。
所述碱金属或碱土金属的改性元素A为K、Li、Ba、Ca中的一种或几种。
上述耐高温压电陶瓷的制备方法，包括以下步骤：
（1）配料混合：将Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、Sb2O3、MgO和改性元素的氧化物或盐按上述通式摩尔比称量，倒入振磨机中振磨6h，得到混合均匀的粉体；
（2）预烧：在遂道炉中将粉体于900~1000℃预烧1.5-3小时；
（3）球磨：用超细球磨机球磨，使平均粒度小于2μm；
（4）干燥：将球磨料放入120℃~150℃的烘箱烘烤20h~24h，使其充分干燥；
（5）过筛：将已烘干的料粉降至常温，过200目筛，制备成成型料粉；
（6）造粒、成型、冲片、排胶、烧结：在料粉中加入质量比10%的胶合剂，混合、陈腐后挤压成型，冲片，排胶，在1180℃～1250℃遂道炉中烧结成陶瓷片；
（7）被银电极：将制备的陶瓷片两表面用丝网印刷上所需直径、厚度0.01mm的银浆，在260～350℃的遂道炉中烘干，放在垫板上于750~800℃的遂道炉中烧银，制成被银陶瓷片；
（8）极化：将被银陶瓷片放入80℃~140℃的极化装置中在1.5kv/mm~4kv/mm电压下极化20~30min，制成通式为Pb(Zr1/2Ti1/2)x(Ni1/3Nb2/3)y(Sb1/3Nb2/3)z(Mg1/3Nb2/3)1-x-y-zO3+wmol%A的耐高温压电陶瓷。
优选地，步骤（3）中粉体﹕球﹕水约为1﹕（2~3）﹕（0.5~1.5），球磨时间为6~12h。
优选地，步骤（6）中胶合剂为羟丙基甲基纤维素、聚乙烯醇、酒精和水的混合物，其比例为羟丙基甲基纤维素：聚乙烯醇：酒精：水=1:1:0.5:5。
与现有技术比较，本发明由于采用了上述技术方案，解决了现有的压电陶瓷使用温度低且电学性能无法满足要求的问题；本发明可以在200℃以上使用，具有较高压电常数，较大机电耦合系数，较高介电常数，能满足蜂鸣片等高温压电器件的需求；本发明生产过程相对简单、生产成本低，适合大规模工业生产。
具体实施方式
下面结合具体的实施例对本发明作进一步说明：
实施例1
将Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、Sb2O3、MgO和Li2CO3按Pb(Zr1/2Ti1/2)0.85(Ni1/3Nb2/3)0.10(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+0.1mol%Li摩尔比称量，倒入振磨机中振磨6h，得到混合均匀的粉体；过筛后于950℃预烧2h，将预烧后的粉体球磨6~12h，使平均粒度小于2μm，粉体﹕球﹕水约为1﹕（2~3）﹕（0.5~1.5）；将球磨粉体烘干并加入10%的胶合剂（羟丙基甲基纤维素：聚乙烯醇：酒精：水=1:1:0.5:5）造粒，陈腐后挤压成型，冲片，排胶，并在1210℃的温度下保温2h烧结，得到陶瓷片；将陶瓷片两表面用丝网印刷上所需直径、厚度0.01mm的银浆，在260～350℃的遂道炉中烘干，放在垫板上于750~800℃的遂道炉中烧银，制成被银陶瓷片；将被银陶瓷片放入120℃的极化装置在2kV/mm的电压下极化25min，得到耐高温压电陶瓷片。老化24h后测得耐高温压电陶瓷片综合电性能为：d33=622pC/N，Tc=320℃，ε=2700，tanδ=0.016，Kp=83.68%。
实施例2
将Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、Sb2O3、MgO和Li2CO3按Pb(Zr1/2Ti1/2)0.87(Ni1/3Nb2/3)0.08(Sb1/3Nb2/3)0.015(Mg1/3Nb2/3)0.035O3+0.1mol%Li摩尔比称量，倒入振磨机中振磨6h，得到混合均匀的粉体；过筛后于950℃预烧2h，将预烧后的粉体球磨6~12h，使平均粒度小于2μm，粉体﹕球﹕水约为1﹕（2~3）﹕（0.5~1.5）；将球磨粉体烘干并加入10%的胶合剂（羟丙基甲基纤维素：聚乙烯醇：酒精：水=1:1:0.5:5）造粒，陈腐后挤压成型，冲片，排胶，并在1220℃的温度下保温2h烧结，得到陶瓷片；将陶瓷片两表面用丝网印刷上所需直径、厚度0.01mm的银浆，在260～350℃的遂道炉中烘干，放在垫板上于750~800℃的遂道炉中烧银，制成被银陶瓷片；将被银陶瓷片放入120℃的极化装置在2kV/mm的电压下极化25min，得到耐高温压电陶瓷片。老化24h后测得耐高温压电陶瓷片综合电性能为：d33=583pC/N，Tc=325℃，ε=2500，tanδ=0.014，Kp=78.98%。
实施例3
将Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、Sb2O3、MgO和Li2CO3按Pb(Zr1/2Ti1/2)0.90(Ni1/3Nb2/3)0.03(Sb1/3Nb2/3)0.02(Mg1/3Nb2/3)0.05O3+0.1mol%Ba摩尔比称量，倒入振磨机中振磨6h，得到混合均匀的粉体；过筛后于980℃预烧2h，将预烧后的粉体球磨6~12h，使平均粒度小于2μm，粉体﹕球﹕水约为1﹕（2~3）﹕（0.5~1.5）；将球磨粉体烘干并加入10%的胶合剂（羟丙基甲基纤维素：聚乙烯醇：酒精：水=1:1:0.5:5）造粒，陈腐后挤压成型，冲片，排胶，并在1230℃的温度下保温2h烧结，得到陶瓷片；将陶瓷片两表面用丝网印刷上所需直径、厚度0.01mm的银浆，在260～350℃的遂道炉中烘干，放在垫板上于750~800℃的遂道炉中烧银，制成被银陶瓷片；将被银陶瓷片放入120℃的极化装置在2.5kV/mm的电压下极化25min，得到耐高温压电陶瓷片。老化24h后测得耐高温压电陶瓷片综合电性能为：d33=543pC/N，Tc=335℃，ε=2000，tanδ=0.012，Kp=72.35%。

Claims (5)

1.一种耐高温压电陶瓷，其特征在于：该压电陶瓷的结构通式为：Pb(Zr1/2Ti1/2)x(Ni1/3Nb2/3)y(Sb1/3Nb2/3)z(Mg1/3Nb2/3)1-x-y-zO3+wmol%A，结构通式中x的取值范围为0.85-0.97，y的取值范围为0.01-0.10，z的取值范围为0.01-0.05，w的取值范围为0.05-2.0，A为碱金属或碱土金属的改性元素。
2.根据权利要求1所述的耐高温压电陶瓷，其特征在于：所述碱金属或碱土金属的改性元素A为K、Li、Ba、Ca中的一种或几种。
3.一种权利要求1或2所述的耐高温压电陶瓷的制备方法，其特征在于：包括以下步骤：
（1）配料混合：将Pb3O4、ZrO2、TiO2、Ni2O3、Nb2O5、Sb2O3、MgO和改性元素的氧化物或盐按上述通式摩尔比称量，倒入振磨机中振磨6h，得到混合均匀的粉体；
（2）预烧：在遂道炉中将粉体于900~1000℃预烧1.5-3小时；
（3）球磨：用超细球磨机球磨，使平均粒度小于2μm；
（4）干燥：将球磨料放入120℃~150℃的烘箱烘烤20h~24h，使其充分干燥；
（5）过筛：将已烘干的料粉降至常温，过200目筛，制备成成型料粉；
（6）造粒、成型、冲片、排胶、烧结：在料粉中加入质量比10%的胶合剂，混合、陈腐后挤压成型，冲片，排胶，在1180℃～1250℃遂道炉中烧结成陶瓷片；
（7）被银电极：将制备的陶瓷片两表面用丝网印刷上所需直径、厚度0.01mm的银浆，在260～350℃的遂道炉中烘干，放在垫板上于750~800℃的遂道炉中烧银，制成被银陶瓷片；
（8）极化：将被银陶瓷片放入80℃~140℃的极化装置中在1.5kv/mm~4kv/mm电压下极化20~30min，制成通式为Pb(Zr1/2Ti1/2)x(Ni1/3Nb2/3)y(Sb1/3Nb2/3)z(Mg1/3Nb2/3)1-x-y-zO3+wmol%A的耐高温压电陶瓷。
4.根据权利要求3所述的耐高温压电陶瓷的制备方法，其特征在于：步骤（3）中粉体﹕球﹕水约为1﹕（2~3）﹕（0.5~1.5），球磨时间为6~12h。
5.根据权利要求3所述的耐高温压电陶瓷的制备方法，其特征在于：步骤（6）中胶合剂为羟丙基甲基纤维素、聚乙烯醇、酒精和水的混合物，其比例为羟丙基甲基纤维素：聚乙烯醇：酒精：水=1:1:0.5:5。
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