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CN113149644A - 一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷及其制备方法 - Google Patents

一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷及其制备方法 Download PDF

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CN113149644A
CN113149644A CN202110313994.2A CN202110313994A CN113149644A CN 113149644 A CN113149644 A CN 113149644A CN 202110313994 A CN202110313994 A CN 202110313994A CN 113149644 A CN113149644 A CN 113149644A
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边浪
曹文武
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Harbin Institute of Technology
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Abstract

一种低温烧结的锑锰酸铅‑锆钛酸铅低介电损耗压电陶瓷及其制备方法。本发明属于压铁电材料领域。本发明是为了解决现有硬性陶瓷烧结温度高、压电性能较低的技术问题。本发明的一种低温烧结的锑锰酸铅‑锆钛酸铅低介电损耗压电陶瓷的化学通式为0.05Pb(Mn1/3Sb2/3)O3‑0.47PbZrO3‑0.48PbTiO3+x wt％Li2CO3，其中0<x≤1。制备方法：按陶瓷成分配比配料，然后依次经过预烧、压片、排胶然后在950℃烧结，再经烧银和极化后得到低温烧结的锑锰酸铅‑锆钛酸铅低介电损耗压电陶瓷。本发明通过引入合适含量的Li2CO3，使产品压电性能提高了27％～34％，显著降低了陶瓷的烧结温度。950℃左右的烧结温度，对于烧结炉的要求大大降低，同时降低了能源成本。

Description

一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷及 其制备方法
技术领域
本发明属于压铁电材料领域，具体涉及一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷及其制备方法。
背景技术
随着电子产品的不断微型化，电子元器件都逐渐在向小、轻、薄的方向发展。而多层陶瓷电容器(MLCC)作为片状的元器件中应用极广的一类，广泛应用在医疗、导航、通讯和致动系统等高新技术领域。对于多层陶瓷，需要降低烧结温度，以利于陶瓷与内部电极(如银钯合金)的共烧成型。此外，较低的烧结温度也将降低生产过程中的能耗和氧化铅的挥发，减少金属离子向陶瓷内部扩散。因此，研发新一代的低烧结温度、高电学性能的压电材料成具有重大社会意义和经济价值。
PZT基陶瓷因其制备工艺简单、成本较低、电性能优异等特点广泛应用于各种器件中。但一般的PZT基陶瓷其烧结温度在1200℃以上，这严重限制了其在多层陶瓷制备中电极的选择。一般地，能稳定在1200℃以上实现共烧的内电极浆料为纯铂电极，这极大的提高了多层制备的成本。而当烧结温度低于1000℃时，内电极浆料的选择便有了极大的拓展，比如镍内电极、铜内电极、银内电极等。无论是成本还是工艺难度都显著降低。因此，降低材料的烧结温度在1000℃以下对于制备多层压电陶瓷来讲非常关键。
发明内容
本发明是为了解决现有硬性陶瓷烧结温度高、压电性能较低的技术问题，而提供一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷及其制备方法。
本发明的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的化学通式为0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3，其中0<x≤1。
进一步限定，所述低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的化学式为0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+1wt％Li2CO3。
本发明的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法按以下步骤进行：
步骤一、配料：以MnO2、PbO、TiO2、ZrO2、Sb2O3、LiCO3作为原料，按照低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的化学计量比称取原料，其中PbO的物质的量过量1.5％，球磨烘干；
步骤二、预烧：将步骤一烘干的粉体置于坩埚中，然后在马弗炉中预烧粉体；
步骤三、压片：将步骤二得到的预烧粉体二次球磨烘干，然后加入聚乙烯醇溶液研磨均匀，过筛后压制成胚体；
步骤四、排胶：将步骤三得到的胚体放入马弗炉中进行排胶，得到排胶后胚件；
步骤五、烧结：将步骤四得到的排胶后胚件放于马弗炉中，以同组分粉料覆盖胚件进行埋烧，以3℃/min～10℃/min的升温速度升至930～970℃，并在该温度下保温1.5h～3h，保温结束自然冷却至室温，得到陶瓷片；
步骤六、烧银：将步骤五烧结好的陶瓷片表面打磨处理，然后在陶瓷片的上、下表面涂抹银浆，再置于马弗炉中进行烧银，自然冷却至室温，得到被银的陶瓷片；
步骤七、极化：将步骤六得到的被银的陶瓷片置于100～140℃的硅油中，施加电场进行极化，得到低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷。
进一步限定，步骤二中预烧的过程为：以3℃/min～10℃/min的升温速度升温至730～770℃，并在该温度下保温1.5h～3h，得到预烧粉体。
进一步限定，步骤三中所述聚乙烯醇溶液的加入量为步骤二得到的预烧粉体的5wt％～7wt％。
进一步限定，步骤三中所述过筛是过80～200目筛。
进一步限定，步骤三中所述压制的压力为150Mpa～300MPa。
进一步限定，步骤四中所述排胶的过程为：以，0.5℃/min～1.5℃/min的升温速度升至180～220℃，保温1.5h～2.5h，然后以0.2℃/min～0.4℃/min的升温速度升至580～620℃，保温1.5h～2.5h。
进一步限定，步骤六中所述烧银的过程为：以3℃/min～10℃/min的升温速度升温至630～670℃，并在该温度下保温20min～40min。
进一步限定，步骤七中所述极化的电场强度为3kV/mm～4kV/mm，极化时间为5min～15min。
本发明相比现有技术的优点如下：
本发明相比现有技术的优点如下：
1)Li2CO3的加入，在固相反应中提供了液相，提高了烧结驱动力，加快了固相反应的速率，同时晶粒间的液相膜起到一个润滑作用，促进晶粒重排向减少气孔的方向进行，减少了系统的表面自由能，明显降低陶瓷烧结温度的同时，提高了陶瓷的压电性能，极大的拓展了多层陶瓷制备中内电极的选择范围，降低了多层陶瓷的制备成本。
2)添加的Li2CO3过少，在烧结过程中可以提供的液相较少，对烧结温度的降低效果有限。当添加的Li2CO3过多时，陶瓷烧结过程中需要的液相趋于饱和，液相的继续增加并不会继续降低烧结温度，反而对陶瓷产生了掺杂效果，恶化其电学性能。
3)制备工艺中，低于800℃的预烧温度远离PbO的熔点，使得预烧粉中晶粒尺寸较小。最终烧结温度低于1000℃，限制了陶瓷中较大尺寸晶粒的形成，有利于陶瓷电学性能的提升。
4)本发明的产品，通过引入合适含量的Li2CO3，压电性能提高了27％～34％，显著降低了陶瓷的烧结温度。950℃左右的烧结温度，对于烧结炉的要求大大降低，同时降低了能源成本。此外，在多层陶瓷堆的制备中完全可以使用铜内电极、镍内电极等贱金属内电极，比起铂内电极、银钯内电极，成本降低了几百倍。
附图说明
图1为实施例1制备的0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+0.4wt％Li2CO3陶瓷的微观形貌图；
图2是实施例1制备的0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+0.6wt％Li2CO3陶瓷的介电温谱。
具体实施方式
实施例1：本实施例的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的化学式为0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3，其中x＝0.1、0.2、0.4、0.6、0.8、1。
制备实施例1的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的方法按以下步骤进行：
步骤一、配料：以MnO2、PbO、TiO2、ZrO2、Sb2O3、LiCO3作为原料，按照0.05Pb(Mn1/ 3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3的化学计量比称取原料，其中PbO的物质的量过量1.5％，球磨烘干；其中MnO2、PbO、TiO2、ZrO2、Sb2O3、LiCO3，均为市售的化学纯原料(纯度≥99％)；球磨烘干过程为：球磨介质为酒精，加入酒精的质量为原料总质量的80％，磨球直径8mm，磨球数目为覆盖球磨罐1/3处，球磨24h后烘干；
步骤二、预烧：将步骤一烘干的粉体置于坩埚中，然后在马弗炉中，以5℃/min的升温速度升温至750℃，并在该温度下保温2h，得到预烧粉体；
步骤三、压片：将步骤二得到的预烧粉体二次球磨24h烘干，然后加入聚乙烯醇溶液研磨均匀，过100目筛后于150MPa下压制成直径13mm，厚度1mm的圆片状胚体；所述聚乙烯醇溶液的加入量为步骤二得到的预烧粉体的5wt％；
步骤四、排胶：将步骤三得到的胚体放入马弗炉中，1℃/min的升温速度升至200℃，保温2h，然后以0.3℃/min的升温速度升至600℃，保温2h进行排胶，得到排胶后胚件；
步骤五、烧结：将步骤四得到的排胶后胚件放于马弗炉中，以同组分粉料覆盖胚件进行埋烧，以5℃/min的升温速度升至950℃，并在该温度下保温2.5h，保温结束自然冷却至室温，得到陶瓷片；
步骤六、烧银：将步骤五烧结好的陶瓷片表面打磨处理，然后在陶瓷片的上、下表面涂抹银浆，再置于马弗炉中，以5℃/min的升温速度升温至650℃，并在该温度下保温30min进行烧银，自然冷却至室温，得到被银的陶瓷片；
步骤七、极化：将步骤六得到的被银的陶瓷片置于120℃的硅油中，施加3.5kV/mm电场进行极化10min，得到0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3陶瓷，即低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷。
对比例：本实施例与实施例1不同的是：0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3中x＝0，烧结温度为1200℃，保温2.5h。其他步骤及参数与实施例1相同。
测试：将实施例1与对比例所制备的陶瓷室温静置24h测试其电学性能，电学性能测试结果列于表1。
表1电学性能测试结果
Figure BDA0002990385920000041

Claims (10)

1.一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷，其特征在于，该低介电损耗压电陶瓷的化学通式为0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+x wt％Li2CO3，其中0<x≤1。
2.根据权利要求1所述的所述低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷，其特征在于，该低介电损耗压电陶瓷的化学式为0.05Pb(Mn1/3Sb2/3)O3-0.47PbZrO3-0.48PbTiO3+1wt％Li2CO3。
3.如权利要求1或2所述的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法，其特征在于，该制备方法按以下步骤进行：
步骤一、配料：以MnO2、PbO、TiO2、ZrO2、Sb2O3、LiCO3作为原料，按照低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的化学计量比称取原料，其中PbO的物质的量过量1.5％，球磨烘干；
步骤二、预烧：将步骤一烘干的粉体置于坩埚中，然后在马弗炉中预烧粉体；
步骤三、压片：将步骤二得到的预烧粉体二次球磨烘干，然后加入聚乙烯醇溶液研磨均匀，过筛后压制成胚体；
步骤四、排胶：将步骤三得到的胚体放入马弗炉中进行排胶，得到排胶后胚件；
步骤五、烧结：将步骤四得到的排胶后胚件放于马弗炉中，以同组分粉料覆盖胚件进行埋烧，以3℃/min～10℃/min的升温速度升至930～970℃，并在该温度下保温1.5h～3h，保温结束自然冷却至室温，得到陶瓷片；
步骤六、烧银：将步骤五烧结好的陶瓷片表面打磨处理，然后在陶瓷片的上、下表面涂抹银浆，再置于马弗炉中进行烧银，自然冷却至室温，得到被银的陶瓷片；
步骤七、极化：将步骤六得到的被银的陶瓷片置于100～140℃的硅油中，施加电场进行极化，得到低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷。
4.根据权利要求3所述的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法，其特征在于，步骤二中预烧的过程为：以3℃/min～10℃/min的升温速度升温至730～770℃，并在该温度下保温1.5h～3h，得到预烧粉体。
5.根据权利要求3所述的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法，其特征在于，步骤三中所述聚乙烯醇溶液的加入量为步骤二得到的预烧粉体的5wt％～7wt％。
6.根据权利要求3所述的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法，其特征在于，步骤三中所述过筛是过80～200目筛。
7.根据权利要求3所述的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法，其特征在于，步骤三中所述压制的压力为150Mpa～300MPa。
8.根据权利要求3所述的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法，其特征在于，步骤四中所述排胶的过程为：以0.5℃/min～1.5℃/min的升温速度升至180～220℃，保温1.5h～2.5h，然后以0.2℃/min～0.4℃/min的升温速度升至580～620℃，保温1.5h～2.5h。
9.根据权利要求3所述的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法，其特征在于，步骤六中所述烧银的过程为：以3℃/min～7℃/min的升温速度升温至630～670℃，并在该温度下保温20min～40min。
10.根据权利要求3所述的一种低温烧结的锑锰酸铅-锆钛酸铅低介电损耗压电陶瓷的制备方法，其特征在于，步骤七中所述极化的电场强度为3kV/mm～4kV/mm，极化时间为5min～15min。
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