CN109592980B - 一种低温共烧压电多层陶瓷及其制备方法 - Google Patents

一种低温共烧压电多层陶瓷及其制备方法 Download PDF

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CN109592980B
CN109592980B CN201811538521.7A CN201811538521A CN109592980B CN 109592980 B CN109592980 B CN 109592980B CN 201811538521 A CN201811538521 A CN 201811538521A CN 109592980 B CN109592980 B CN 109592980B
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张田才
王兰花
徐民
李斌
李帮菊
李娅
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Guizhou Zhenhua Hongyun Electronics Co ltd
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Abstract

本发明公开了一种低温共烧压电多层陶瓷，该低温压电多层陶瓷的结构通式为PbxM3 1‑X〔(M4 1/3Nb 2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZr.Ti]O3+wmol%Cuo，其x=0.86‑0.96，e=0.01‑0.10，f=0.01‑0.5，g=0.01‑0.6，w=0.05‑2.5。本发明还提供了制备该压电多层陶瓷的方法，可利用该方法制备具有高压电常数、高品质因数、高机电耦合系数、高介电常数、高容量的低温烧结压电多层陶瓷，克服了现有普通压电陶瓷烧结温度高，无法制备高容量压电器件的问题。本发明所公开的制备方法具有工艺简单，无特殊设备要求，成本比较低，利于企业大规模生产等特点，可以用于压电蜂鸣器件等各种高容量压电器件产品。

Description

一种低温共烧压电多层陶瓷及其制备方法
技术领域
本发明涉及多层压电陶瓷技术，具体涉及一种能实现低温共烧的压电陶瓷材料及其制备方法。
背景技术
现有压电陶瓷材料烧结温度为1250～1300℃，在温度900～950℃很难烧结成瓷；而银电极材料在1250～1300℃烧结时又会挥发，因而必须使用昂贵的银钯浆料作为电极才能实现多层叠片烧结，从而大大提高了压电多层陶瓷元件的成本。因此，研究制造可低温共烧的压电陶瓷元件具有十分重要的意义。
一般而言，当压电陶瓷材料具有较高居里温度时，其静态电容较低，介质损耗也较大，综合性能较差；而对于压电器件而言，其要求具有高电容量的同时，还需要具有较高的介电常数和机电耦合系数。研究表明，铋层状压电陶瓷，其烧结温度大于1250℃，但其压电系数只有30pC/N；而BiScO3-PbTiO3体系压电陶瓷有最优压电特性（Tc≈430℃，d33≈400pC/N），但其综合电学性能较差。因此，开发具有烧结温度低，使用温度高（≥220℃），高压电常数（d33≥450pC/N），高机电耦合系数（Kp≥75%），较高介电常数（ε≥2600），综合电学性能优异且容量高的压电材料，是压电陶瓷领域的一个难题。
发明内容
针对现有压电陶瓷材料无法在烧结温度低的同时具有较高的综合压电性能，不能满足压电器件的使用要求的现状，本发明提供了一种具有烧结温度低，电容量高，且综合压电性能好，并在一定范围内可以调节的高性能压电陶瓷材料，为了解决上述技术问题，所采用的技术方案为：
一种低温共烧压电多层陶瓷材料，该低温烧结压电多层陶瓷的结构通式为PbxM3 1-X［(M4 1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZrTi］O3+wmol%CuO，其中M3为3价金属的改性元素、M4为4价金属元素，所述改性元素M为La、K、Er、Yb中的一种或几种；所述结构通式中x的取值范围为0.86～0.96，e的取值范围为0.01～0.10，f的取值范围为0.01～0.5，g的取值范围为0.01～0.6，w的取值范围为0.05～2.5。
这种低温共烧压电多层陶瓷的制备方法包括以下步骤：
（1）将PbO、ZrO2、TiO2、Ni2O3、Nb2O5、Co2O3、ZnO、CuO和改性元素的氧化物或盐按摩尔比称量，然后混合得到粉体；
（2）第一次磨料 用水磨搅拌机搅拌2.5～3.5h，其中料:球:水的重量比例为1:2:0.6；将混合均匀的粉体在150～170℃烘箱中烘10h使其烘干，然后在隧 道炉中将烘干的粉料于800～850℃煅烧合成；
（3）第二次磨料 用砂磨机砂磨5.5～6.5h，其中料:球:水的重量比例为1:2:0.6，使粒度D50达到1.0～1.4μm；将砂磨料放入150～170℃的烘箱烘烤19～21h，将已烘干的料自然冷却至常温，过120目振动筛网，制备成待成型料粉；
（4）料粉中按一定比例加入粘合剂、分散剂、消泡剂和水，混合球磨均匀后23～25h在流延机上流延成型，将成型的膜片裁剪成一定的尺寸并印刷银电极后再按所需的层数进行叠层；将叠层好的膜片在等静压机中进行等静压35～45分钟，然后放在含量99％氧化铝板上，在900～950℃隧 道炉中进行烧结，烧结后进行剥离；
（5）将制备好的叠层陶瓷片的上下两面用丝网印刷上所需直径、厚度0.003～0.007㎜的银浆，在200～300℃的隧 道烘干炉中烘干，放在氧化锆垫板上于780～820℃的隧 道炉中烧银，制成多层被银陶瓷片；将多层被银陶瓷片放入95～105℃的极化装置中在2～3.6kV/mm 电压下极化25～35分钟，制成通式为PbxM3 1-X［(Ni1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/ 3Nb2/3)gZrTi］O3+wmol%CuO的多层压电陶瓷被银片。
本发明的有益效果体现在：这种材料具有低烧结温度，高电容量，综合性能优异的复合钙钛矿结构PbxM3 1-X［(Ni1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZrTi］O3+wmol%CuO新型压电陶瓷材料，解决了现有的压电陶瓷材料无法低温烧结，性能好且电学性能满足使用要求的问题。该压电材料可以满足多层压电陶瓷的低温共烧需求，提高压电陶瓷的电容量，大幅降低成本，同时具有较高的压电常数（450～600pC/N）、机电耦合系数75～85%和介电常数2600～3300，可以满足压电蜂鸣器件等各种高容量压电器件产品的需求。
具体实施方式
实施例1
一种低温共烧压电多层陶瓷材料，该低温烧结压电多层陶瓷的结构通式为PbxM3 1-X［(M4 1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZr.Ti］O3+wmol%CuO，其中M3为3价金属的改性元素，M4为4价金属元素；所述压电材料的结构通式中x的取值范围为0.86，e的取值范围为0.10，f的取值范围为0.01，g的取值范围为0.6，w的取值范围为0.05。其中低温共烧压电多层陶瓷材料中改性元素M为La。
这种低温共烧压电多层陶瓷的制备方法包括以下步骤：
（1）将PbO、ZrO2、TiO2、Ni2O3、Nb2O5、Co2O3、ZnO、CuO和改性元素的氧化物或盐按摩尔比称量，然后混合得到粉体；
（2）第一次磨料 用水磨搅拌机中搅拌2.5h，其中料:球:水的重量比例为1:2:0.6，使其混合均匀；混合均匀的粉体在170℃烘箱中烘10h使其烘干；在隧 道炉中将烘干的粉料于800℃煅烧合成；
（3）第二次磨料 用砂磨机砂磨6.5h，其中料:球:水的重量比例为1:2:0.6，使粒度D50达到1.0μm；将砂磨料放入170℃的烘箱烘烤19h，使其充分干燥；将已烘干的料自然冷却至常温，过120目振动筛网，制备成待成型料粉；
（4）将料粉中按一定比例加入粘合剂、分散剂、消泡剂和水，混合球磨均匀后24h在流延机上流延成型，将成型的膜片裁剪成一定的尺寸并印刷银电极后再按所需的层数进行叠层；将叠层好的膜片在等静压机中进行等静压45分钟，然后放在含量99％氧化铝板上，在900℃隧 道炉中进行烧结，烧结后进行剥离；
（5）将制备好的叠层陶瓷片的上下两面用丝网印刷上所需直径、厚度0.007㎜的银浆，在200℃的隧 道烘干炉中烘干，放在氧化锆垫板上于820℃的隧 道炉中烧银，制成多层被银陶瓷片；将多层被银陶瓷片放入95℃的极化装置中在3.6kV/mm 电压下极化25分钟，制成通式为PbxM3 1-X［(Ni1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZrTi］O3+wmol%CuO的多层压电陶瓷被银片。
实施例2
一种低温共烧压电多层陶瓷材料，该低温烧结压电多层陶瓷的结构通式为PbxM3 1-X［(M4 1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZrTi］O3+wmol%CuO，其中M3为3价金属的改性元素，M4为4价金属元素；所述压电材料的结构通式中x的取值范围为0.96，e的取值范围为0.01，f的取值范围为0.5，g的取值范围为0.01，w的取值范围为2.5。其中低温共烧压电多层陶瓷材料中改性元素M为Er。
这种低温共烧压电多层陶瓷的制备方法包括以下步骤：
（1）将PbO、ZrO2、TiO2、Ni2O3、Nb2O5、Co2O3、ZnO、CuO和改性元素的氧化物或盐按摩尔比称量，然后混合得到粉体；
（2）第一次磨料 用水磨搅拌机搅拌3.5h，其中料:球:水的重量比例为1:2:0.6，使其混合均匀；混合均匀的粉体在150℃烘箱中烘10h使其烘干；在隧 道炉中将烘干的粉料于850℃煅烧合成；
（3）第二次磨料 用砂磨机砂磨5.5h，其中料:球:水的重量比例为1:2:0.6，使粒度D50达到1.2μm；将砂磨料放入170℃的烘箱烘烤19h，使其充分干燥；将已烘干的料自然冷却至常温，过120目振动筛网，制备成待成型料粉；
（4）将料粉中按一定比例加入粘合剂、分散剂、消泡剂和水，混合球磨均匀后24h在流延机上流延成型，将成型的膜片裁剪成一定的尺寸并印刷银电极后再按所需的层数进行叠层；将叠层好的膜片在等静压机中进行等静压35分钟，然后放在含量99％氧化铝板上，在950℃隧 道炉中进行烧结，烧结后进行剥离；
（5）将制备好的叠层陶瓷片的上下两面用丝网印刷上所需直径、厚度0.003㎜的银浆，在300℃的隧 道烘干炉中烘干，放在氧化锆垫板上于780℃的隧 道炉中烧银，制成多层被银陶瓷片；将多层被银陶瓷片放入105℃的极化装置中在2kV/mm 电压下极化35分钟，制成通式为PbxM3 1-X［(Ni1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZrTi］O3+wmol%CuO的多层压电陶瓷被银片。
实施例3
一种低温共烧压电多层陶瓷材料，该低温烧结压电多层陶瓷的结构通式为PbxM3 1-X［(M4 1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZrTi］O3+wmol%CuO，其中M3为3价金属的改性元素，M4为4价金属元素；所述压电材料的结构通式中x的取值范围为0.90，e的取值范围为0.08，f的取值范围为0.35，g的取值范围为0.4，w的取值范围为2.0。其中低温共烧压电多层陶瓷材料中改性元素M为Yb。
这种低温共烧压电多层陶瓷的制备方法包括以下步骤：
（1）将PbO、ZrO2、TiO2、Ni2O3、Nb2O5、Co2O3、ZnO、CuO和改性元素的氧化物或盐按摩尔比称量，然后混合得到粉体；
（2）第一次磨料 用水磨搅拌机搅拌3.0h，其中料:球:水的重量比例为1:2:0.6，使其混合均匀；混合均匀的粉体在160℃烘箱中烘10h使其烘干；在隧 道炉中将烘干的粉料于820℃煅烧合成；
（3）第二次磨料 用砂磨机砂磨6.0h，其中料:球:水的重量比例为1:2:0.6，使粒度D50达到1.4μm；将砂磨料放入160℃的烘箱烘烤20h，使其充分干燥；将已烘干的料自然冷却至常温，过120目振动筛网，制备成待成型料粉；
（4）将料粉中按一定比例加入粘合剂、分散剂、消泡剂和水，混合球磨均匀后23h在流延机上流延成型，将成型的膜片裁剪成一定的尺寸并印刷银电极后再按所需的层数进行叠层；将叠层好的膜片在等静压机中进行等静压40分钟；然后放在含量99％氧化铝板上，在920℃隧 道炉中进行烧结，烧结后进行剥离；
（5）将制备好的叠层陶瓷片的上下两面用丝网印刷上所需直径、厚度0.005㎜的银浆，在250℃的隧 道烘干炉中烘干，放在氧化锆垫板上于800℃的隧 道炉中烧银，制成多层被银陶瓷片；将多层被银陶瓷片放入100℃的极化装置中在2.6kV / mm 电压下极化30分钟，制成通式为PbxM3 1-X［(Ni1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZrTi］O3+wmol%CuO的多层压电陶瓷被银片。
以上所描述的实施例是本发明一部分实施例，而不是全部的实施例。本发明实施例的详细描述并非旨在限制要求保护的本发明的范围，而是仅仅表示本发明的选定实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。

Claims (2)

1.一种低温共烧压电多层陶瓷材料，其特征在于该低温烧结压电多层陶瓷的结构通式为：PbxM3 1-X［(M4 1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/3Nb2/3)gZrTi］O3+wmol%CuO，其中M3为3价金属的改性元素、M4为4价金属元素，所述改性元素M为La、K、Er、Yb中的一种或几种；所述结构通式中x的取值范围为0.86～0.96，e的取值范围为0.01～0.10，f的取值范围为0.01～0.5，g的取值范围为0.01～0.6，w的取值范围为0.05～2.5。
2.实现权利要求1所述的一种低温共烧压电多层陶瓷的制备方法，其特征在于包括以下步骤：
（1）将PbO、ZrO2、TiO2、Ni2O3、Nb2O5、Co2O3、ZnO、CuO和改性元素的氧化物或盐按摩尔比称量，然后混合得到粉体；
（2）第一次磨料 用水磨搅拌机搅拌2.5～3.5h，其中料:球:水的重量比例为1:2:0.6；将混合均匀的粉体在150～170℃烘箱中烘10h使其烘干，然后在隧 道炉中将烘干的粉料于800～850℃煅烧合成；
（3）第二次磨料 用砂磨机砂磨5.5～6.5h，其中料:球:水的重量比例为1:2:0.6，使粒度D50达到1.0～1.4μm；将砂磨料放入150～170℃的烘箱烘烤19～21h，将已烘干的料自然冷却至常温，过120目振动筛网，制备成待成型料粉；
（4）料粉中按一定比例加入粘合剂、分散剂、消泡剂和水，混合球磨均匀后23～25h在流延机上流延成型，将成型的膜片裁剪成一定的尺寸并印刷银电极后再按所需的层数进行叠层；将叠层好的膜片在等静压机中进行等静压35～45分钟，然后放在含量99％氧化铝板上，在900～950℃隧 道炉中进行烧结，烧结后进行剥离；
（5）将制备好的叠层陶瓷片的上下两面用丝网印刷上所需直径、厚度0.003～0.007㎜的银浆，在200～300℃的隧 道烘干炉中烘干，放在氧化锆垫板上于780～820℃的隧 道炉中烧银，制成多层被银陶瓷片；将多层被银陶瓷片放入95～105℃的极化装置中在2～3.6kV/mm 电压下极化25～35分钟，制成通式为PbxM3 1-X［(Ni1/3Nb2/3)e(Co1/3Nb2/3)f(Zn1/ 3Nb2/3)gZrTi］O3+wmol%CuO的多层压电陶瓷被银片。
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