CN106587986B - 具备储能、应变与宽介电温区的多功能无铅陶瓷及制备方法 - Google Patents

具备储能、应变与宽介电温区的多功能无铅陶瓷及制备方法 Download PDF

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CN106587986B
CN106587986B CN201611201458.9A CN201611201458A CN106587986B CN 106587986 B CN106587986 B CN 106587986B CN 201611201458 A CN201611201458 A CN 201611201458A CN 106587986 B CN106587986 B CN 106587986B
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刘国保
许积文
王�华
周昌荣
袁昌来
饶光辉
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Guilin University of Electronic Technology
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Abstract

本发明公开了一种同时具备储能、应变及宽介电温区多功能共存的三元体系无铅陶瓷及其制备方法，所述多功能无铅陶瓷组份的化学通式可以用(1‑x)[(1‑y)BiAO3‑yMeTiO3]‑x(Bi0.5Na0.5)TiO3所表示。其中：A为Sc、Y、In中的一种或两种；Me为Ca、Sr、Ba中的一种或两种；x、y表示摩尔分数；0.05≤x≤0.30；0.50≤y≤0.80。这种多功能无铅陶瓷除了低污染外，还具备储能、应变及宽介电温区等多功能特性，相比于传统的多组分集成方式具有更好的质量和体积效率，是一种新型的智能性材料。

Description

具备储能、应变与宽介电温区的多功能无铅陶瓷及制备方法
技术领域
本发明属于电子陶瓷材料领域，具体涉及一种同时具备储能、应变与宽介电温区的多功能无铅陶瓷及其制备方法。
背景技术
高储能密度电容器在脉冲功率电源、航空航天、新能源发电等领域应用非常广泛。储能陶瓷具有储能密度高、充放电速度快(短至纳秒)、抗循环老化、适用于高温高压等极端环境以及具有性能稳定的优点。通常的压电材料因离子在电场中微动而产生场致应变，但这种普通压电效应的电致变形很小，制约了该材料的实际应用。在200V/mm的电场下，一般的PZT系压电陶瓷的应变不到0.02％。而且由于铅对人体健康的不利影响，这些如今仍然广泛使用的含铅压电材料，已经开始受到越来越多的限制。
宽介电温区型的陶瓷电容器介电材料是重要的电子材料，几乎可以应用于所有的电子工业中。在一些特殊的行业，常常会提出严格的温度需求，特别是高达200℃以上的应用。普通产品可能不适合额定125℃以上的应用，基于Y5R，Y7R或Y8R电介质的电容，尽管可在200℃的高温下应用，但其性能可能会有一定的衰减。目前公开的BaTiO3基Y9R电容器陶瓷介电材料也难满足这么高的工作温度。
随着功能材料和器件的不断发展，期待在一种材料或器件中可以实现越来越多的功能，成为智能材料和器件。对于同时具备较好高储能密度、高储能效率，良好的电致应变，以及高稳定介电性能等多功能无铅电子陶瓷，电子工业中存在广泛的需求。
发明内容
针对上述背景，本发明提供一种同时具备储能、应变及宽介电温区多功能共存的三元体系无铅陶瓷及其制备方法。这种多功能无铅陶瓷除了低污染外，还具备储能、应变及宽介电温区等多功能特性，相比于传统的多组分集成方式具有更好的质量和体积效率，是一种新型的智能性材料。
本发明中所述多功能无铅陶瓷组份的化学通式可以用
(1-x)[(1-y)BiAO3-yMeTiO3]-x(Bi0.5Na0.5)TiO3所表示。其中：A为Sc、Y、In中的一种或两种；Me为Ca、Sr、Ba中的一种或两种；x、y表示摩尔分数；0.05≤x≤0.30；0.50≤y≤0.80。
本发明中所述多功能无铅陶瓷的制备方法，除了现有工艺步骤外，至少还包括将粉体原料按照化学通式(1-x)[(1-y)BiAO3-yMeTiO3]-x(Bi0.5Na0.5)TiO3进行配料的步骤。其它后续步骤如加入分散剂球磨、球磨浆料干燥、过筛、煅烧、保温合成粉体等皆可以采用现有工艺。
具体实施方式
为了详细介绍本发明，在此给出一些具体的实施例，并提供了一些优选的工艺参数。
实施例1：成分为(1-x)[(1-y)BiScO3-yBaTiO3]-x(Bi0.5Na0.5)TiO3，其中x＝0.05，y＝0.50。主要制备步骤：
(1)以分析纯粉末Bi2O3、Sc2O3、TiO2、BaCO3和Na2CO3为原料，按照化学式(1-x)[(1-y)BiScO3-yBaTiO3)]-x(Bi0.5Na0.5)TiO3进行配料，以无水乙醇为介质球磨24小时，干燥后过100目筛，再在坩埚中以800℃预烧保温2小时合成粉体。
(2)获得的干燥粉体，加入5％(重量百分比)浓度的PVA溶液造粒，烘干后过100目筛，在40MPa压力下压制成型圆片。
(3)将成型后的圆片在600℃保温2小时排除PVA。
(4)将步骤(3)获得的圆片在空气氛围中烧结，烧结温度1150℃，保温2小时，随炉降温至室温。
将烧结后的样品加工成两面光滑、厚度约0.25mm的薄片，披银电极，然后测试储能密度和介电温谱等，测试性能如表1所示。
实施例2：成分为(1-x)[(1-y)BiScO3-yBaTiO3]-x(Bi0.5Na0.5)TiO3，其中x＝0.10，y＝0.55。制备方法同实施例1，测试性能如表1所示。
实施例3：成分为(1-x)[(1-y)BiScO3-yBaTiO3]-x(Bi0.5Na0.5)TiO3，其中x＝0.15，y＝0.60。制备方法同实施例1，测试性能如表1所示。
实施例4：成分为(1-x)[(1-y)BiScO3-yBaTiO3]-x(Bi0.5Na0.5)TiO3，其中x＝0.20，y＝0.65。制备方法同实施例1，测试性能如表1所示。
实施例5：成分为(1-x)[(1-y)BiScO3-yBaTiO3]-x(Bi0.5Na0.5)TiO3，其中x＝0.25，y＝0.70。制备方法同实施例1，测试性能如表1所示。
实施例6：成分为(1-x)[(1-y)BiScO3-yBaTiO3]-x(Bi0.5Na0.5)TiO3，其中x＝0.30，y＝0.80。制备方法同实施例1，测试性能如表1所示。
实施例7：以Y2O3替代实施例1-6中的Sc2O3，其他参数保持不变，制备方法同实施例1，成功制备出成分为(1-x)[(1-y)BiYO3-yBaTiO3]-x(Bi0.5Na0.5)TiO3的多功能陶瓷,测试性能如表1所示。
实施例8：以In2O3替代实施例1-6中的Sc2O3，其他参数保持不变，制备方法同实施例1，成功制备出成分为(1-x)[(1-y)BiInO3-yBaTiO3]-x(Bi0.5Na0.5)TiO3的多功能陶瓷,测试性能如表1所示。
实施例9：以CaCO3替代实施例1-6中的BaCO3，其他参数保持不变，制备方法同实施例1，成功制备出成分为(1-x)[(1-y)BiInO3-yCaTiO3]-x(Bi0.5Na0.5)TiO3的多功能陶瓷,测试性能如表1所示。
实施例10：以SrCO3替代实施例1-6中的BaCO3，其他参数保持不变，制备方法同实施例1，成功制备出成分为(1-x)[(1-y)BiInO3-ySrTiO3]-x(Bi0.5Na0.5)TiO3的多功能陶瓷,测试性能如表1所示。
实施例11：分别以Sc2O3、Y2O3、In2O3中的两两混合物替代实施例1-6中的Sc2O3，分别以BaCO3、CaCO3、SrCO3中的两两混合物替代实施例1-6中的BaCO3，并进行交叉组合，其他参数保持不变，制备方法同实施例1，均成功制备出成分为(1-x)[(1-y)BiAO3-yMeTiO3]-x(Bi0.5Na0.5)TiO3(其中：A为Sc、Y、In中的两种；Me为Ca、Sr、Ba中的两种；0.05≤x≤0.30；0.50≤y≤0.80)的多功能陶瓷,测试性能如表1所示。上述各实施例制出的多功能陶瓷，经测试，都能达到相近的预期效果。
表1实施例样品的电性能

Claims (6)

1.一种具备储能、应变与宽介电温区的多功能无铅陶瓷，其特征在于所述多功能无铅陶瓷的组成用化学通式(1-x)[(1-y)BiAO3-yMeTiO3]-x(Bi0.5Na0.5)TiO3所表示；其中：A为In；Me为Ca、Sr、Ba中的一种或两种；x、y表示摩尔分数；0.05≤x≤0.30；0.50≤y≤0.80；
所述具备储能、应变与宽介电温区的多功能无铅陶瓷的制备方法由如下步骤组成：
将粉体原料按照化学式(1-x)[(1-y)BiAO3-yMeTiO3]-x(Bi0.5Na0.5)TiO3进行配料，加入分散剂后球磨，球磨浆料干燥后过筛，然后加以煅烧、保温合成粉体；将煅烧合成的粉体加入临时粘胶进行造粒、造粒粉体过筛后压制成片状生坯；将片状生坯排胶，排胶后的生坯进行高温烧结。
2.一种如权利要求1所述的具备储能、应变与宽介电温区的多功能无铅陶瓷的制备方法，由如下步骤组成：
将粉体原料按照化学式(1-x)[(1-y)BiAO3-yMeTiO3]-x(Bi0.5Na0.5)TiO3进行配料，加入分散剂后球磨，球磨浆料干燥后过筛，然后加以煅烧、保温合成粉体；其中：A为In；Me为Ca、Sr、Ba中的一种或两种；x、y表示摩尔分数；0.05≤x≤0.30；0.50≤y≤0.80；将煅烧合成的粉体加入临时粘胶进行造粒、造粒粉体过筛后压制成片状生坯；将片状生坯排胶，排胶后的生坯进行高温烧结。
3.根据权利要求2所述的方法，其中所述分散剂为无水乙醇；所述煅烧、保温的过程为在坩埚中以800-900℃煅烧、保温2-6小时。
4.根据权利要求2所述的方法，其中所述临时粘胶为5wt％-7wt％浓度的聚乙烯醇溶液。
5.根据权利要求2所述的方法，其中所述排胶步骤，是将片状生坯放在氧化锆承烧板上，在600℃下保温2小时排除临时粘胶。
6.根据权利要求2所述的方法，其中所述高温烧结步骤是以5℃/min的速率升温至烧结温度1150℃，保温2小时，其后随炉自然降温至室温。
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