CN109437888A - 一种低损耗巨介电常数x8r型电介质材料的制备方法 - Google Patents

一种低损耗巨介电常数x8r型电介质材料的制备方法 Download PDF

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CN109437888A
CN109437888A CN201811254091.6A CN201811254091A CN109437888A CN 109437888 A CN109437888 A CN 109437888A CN 201811254091 A CN201811254091 A CN 201811254091A CN 109437888 A CN109437888 A CN 109437888A
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李玲霞
王文波
张宁
卢特
王瑞杰
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Tianjin University
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Abstract

本发明公开了一种低损耗巨介电常数X8R型电介质材料的制备方法，先按BaTiO3:Nb2O5:MgO:CaZrO3＝100:0.5～3.0:0.1～2.0:1.0～3.0的质量比进行配料，经球磨、烘干、过筛、造粒后压制成坯体，坯体经排胶后置于还原气氛炉中于1300～1350℃烧结，制成钛酸钡基低损耗巨介电常数X8R型电介质材料。本发明的介电常数ε25℃为4.23×104，介电损耗tanσ为0.0255。

Description

一种低损耗巨介电常数X8R型电介质材料的制备方法
技术领域
本发明属于一种以成分为特征的陶瓷组合物，具体涉及一种具有较低介电损耗、巨大介电常数同时满足X8R特性的钛酸钡基电介质陶瓷材料及其制备方法。
背景技术
随着电子设备集成化程度的提高，要求电子元器件具有更小的尺寸；另外，无源器件面临更高工作温度的挑战，特别是在高端民用领域及军用领域。例如：汽车的ABS(Anti-Block System,防抱死系统)的工作温度达150℃，卫星、军用飞机等武器装备发动机部位附近的工作温度更是高达300℃。多层陶瓷电容器(Multilayer ceramic capacitor，MLCC)作为应用最广泛的一类集成化无源器件，电子行业对具有更高温度上限的MLCC的需求一直居高不下。而传统的MLCC用电介质材料的工作温度上限大多集中在125℃，并且随着介质材料的温度稳定性的改善往往伴随着介电常数的降低，这导致目前很多MLCC用电介质材料难于满足拓宽器件工作温区的同时满足器件小型化的发展趋势，故而对兼具高介电常数和良好温度稳定性的电介质材料的研究具有重要意义。
发明内容
本发明的目的，在于克服大多数宽温电介质材料体系中存在的介电常数较低的问题，提供一种兼具X8R特性、巨介电常数与低损耗的钛酸钡基电介质材料及其制备方法，以期望开发出能满足当今大容量宽温稳定性电容器制备与应用要求的材料。
本发明通过如下技术方案予以实现。
一种低损耗巨介电常数X8R型电介质材料的制备方法，具体步骤如下：
(1)按质量比BaTiO3:Nb2O5:MgO:CaZrO3＝100:0.5～3.0:0.1～2.0:1.0～3.0进行配料，混合球磨4小时后于100℃烘干，并过40目分样筛；
(2)造粒：将步骤(1)粉料，添加7wt％石蜡作为粘结剂，过80目筛进行造粒；
(3)成型：采用粉末压片机压制成坯体；
(4)排胶：将制备好的坯体进行排胶；
(5)烧结：将排胶后的坯体置于还原气氛炉，通入N2或者N2/H2混合气体，烧结温度为1300～1350℃，保温3h，制成钛酸钡基低损耗巨介电常数X8R型电介质材料。
所述步骤(3)的坯体为Ф10×1.0～2.0mm的圆片坯体。
所述步骤(4)的坯体经3.5h升温至600℃排胶，并保温5h。
所述步骤(5)的坯体经5℃/min升温速率至1000℃烧结，再以2℃/min升温速率至1300～1350℃烧结。
本发明的原料使用施主元素Nb5+和受主元素Mg2+共同作用以促进钛酸钡基介质材料介电常数大幅度提升，并且使用CaZrO3对材料的温度稳定性进行改善从而使得材料满足X8R特性；本发明通过调节烧结气氛，使得材料性能达到了介电常数ε25℃为4.23×104，介电损耗tanσ为0.0255。
具体实施方式
以下将结合具体实施例对本发明作进一步的详细描述，本发明不局限于下列实施例：
实施例1
首先，用电子天平称量BaTiO3、Nb2O5、MgO、CaZrO3按质量比100:1.0:0.2:1.5进行配料，以去离子水：氧化锆球：粉料＝2:1:1混合后球磨4h，烘干后再外加质量百分比为7％的石蜡，过80目分样筛造粒。
将造粒后的粉料在3MPa下压制成Ф10×1.2mm的圆片生坯，经3.5h空气中升温至600℃排胶。在流速为50ml/min N2和5ml/min H2混合气流中，再经2℃/min升至1350℃烧结，保温3h，制得低损耗巨介电常数X8R型陶瓷电容器介质材料。
在所得制品上下表面均匀涂覆银浆，经850℃烧渗制备电极，制得待测样品，测试介电性能及TC特性。
实施例2～3
实施例2～3较之实施例1具有不同的通气及含量以及不同的烧结温度，其他制作工艺完全同于实施例1。
本发明的测试方法和检测设备如下：
(1)介电性能测试(交流测试信号：频率为20Hz～1MHz，电压为1V)
使用TH2828S 1MHz同辉精密LCR数字电桥测试样品的电容量C和损耗tanδ，并计算出样品的介电常数，计算公式为：
(2)TC特性测试
利用GZ-ESPEC MPC-710P型高低温循环温箱、HM27002型电容器C-T/V特性专用测试仪和HEWLETT PACKARD 4278A进行测试。测量样品在温区-55℃～150℃内的电容量，采用下述公式计算电容量变化率：
本发明的主要技术参数及其介电性能详见表1。
表1
本发明并不局限于上述实施例，很多细节的变化是可能的，但这并不因此违背本发明的范围和精神。

Claims (4)

1.一种低损耗巨介电常数X8R型电介质材料的制备方法，具体步骤如下：
(1)按质量比BaTiO3:Nb2O5:MgO:CaZrO3＝100:0.5～3.0:0.1～2.0:1.0～3.0进行配料，混合球磨4小时后于100℃烘干，并过40目分样筛；
(2)造粒：将步骤(1)粉料，添加7wt％石蜡作为粘结剂，过80目筛进行造粒；
(3)成型：采用粉末压片机压制成坯体；
(4)排胶：将制备好的坯体进行排胶；
(5)烧结：将排胶后的坯体置于还原气氛炉，通入N2或者N2/H2混合气体，烧结温度为1300～1350℃，保温3h，制成钛酸钡基低损耗巨介电常数X8R型电介质材料。
2.根据权利要求1所述的一种低损耗巨介电常数X8R型电介质材料的制备方法，其特征在于，所述步骤(3)的坯体为Ф10×1.0～2.0mm的圆片坯体。
3.根据权利要求1所述的一种低损耗巨介电常数X8R型电介质材料的制备方法，其特征在于，所述步骤(4)的坯体经3.5h升温至600℃排胶，并保温5h。
4.根据权利要求1所述的一种低损耗巨介电常数X8R型电介质材料的制备方法，其特征在于，所述步骤(5)的坯体经5℃/min升温速率至1000℃烧结，再以2℃/min升温速率至1300～1350℃烧结。
CN201811254091.6A 2018-10-24 2018-10-24 一种低损耗巨介电常数x8r型电介质材料的制备方法 Pending CN109437888A (zh)

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Cited By (1)

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Publication number Priority date Publication date Assignee Title
CN113277847A (zh) * 2021-06-10 2021-08-20 天津大学 一种抗还原X8R型BaTiO3基介质陶瓷材料及其制备方法

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JPH06243721A (ja) * 1991-03-07 1994-09-02 Tdk Corp 高誘電率誘電体磁器組成物
CN104177083A (zh) * 2014-08-07 2014-12-03 北京元六鸿远电子技术有限公司 用于中温烧结具有偏压特性的温度稳定x8r型mlcc介质材料
CN107226696A (zh) * 2017-05-19 2017-10-03 淄博高新技术产业开发区先进陶瓷研究院 X7R型BaTiO3基电容器陶瓷材料及其制备方法
CN107399970A (zh) * 2017-07-13 2017-11-28 天津大学 一种具有优异绝缘特性的多层陶瓷电容器介质材料
CN108610042A (zh) * 2018-04-27 2018-10-02 天津大学 具有巨介电常数高绝缘特性的介质材料及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06243721A (ja) * 1991-03-07 1994-09-02 Tdk Corp 高誘電率誘電体磁器組成物
CN104177083A (zh) * 2014-08-07 2014-12-03 北京元六鸿远电子技术有限公司 用于中温烧结具有偏压特性的温度稳定x8r型mlcc介质材料
CN107226696A (zh) * 2017-05-19 2017-10-03 淄博高新技术产业开发区先进陶瓷研究院 X7R型BaTiO3基电容器陶瓷材料及其制备方法
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113277847A (zh) * 2021-06-10 2021-08-20 天津大学 一种抗还原X8R型BaTiO3基介质陶瓷材料及其制备方法

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Application publication date: 20190308