CN109231985A - 一种低损耗x8r型电介质材料的制备方法 - Google Patents

一种低损耗x8r型电介质材料的制备方法 Download PDF

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CN109231985A
CN109231985A CN201811245120.2A CN201811245120A CN109231985A CN 109231985 A CN109231985 A CN 109231985A CN 201811245120 A CN201811245120 A CN 201811245120A CN 109231985 A CN109231985 A CN 109231985A
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李玲霞
王文波
张宁
卢特
王瑞杰
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Abstract

本发明公开了一种低损耗X8R型电介质材料的制备方法，先按质量比BaTiO3：MnCO3：MgO：CaZrO3：SiO2：Al2O3：BaCO3＝100：0.5～2.0：0.1～2.0：1.0～3.0：0.5～1.5：0.25～1.5：0.5～1.5进行配料，经球磨、烘干、过筛、造粒后，压制成坯体，坯体经过排胶后于还原气氛炉1250～1350℃烧结，制得低损耗X8R型电介质材料。本发明的材料性能达到了介电常数ε25℃～2461，介电损耗tanσ～0.0096，绝缘电阻率ρν～3.68×1011Ω·cm。

Description

一种低损耗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、满足X8R特性的抗还原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；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。为了满足大容量、小型化的发展趋势，MLCC向着单层薄层化和多层化发展，这就导致内电极的占比持续上升，为了缩小成本，目前大多民用MLCC多采用贱金属(Cu，Ni)作为内电极。但贱金属在高温下烧结时容易被氧化而使得导电性急剧下降，因此，为了防止电极被氧化，需要在还原气氛下进行烧结。BaTiO3中的Ti4+在还原气氛下易被还原为Ti3+，同时产生大量弱束缚电子从而导致材料整体半导化，绝缘特性严重恶化，为了保证器件的正常使用，需要对还原气氛下烧结MLCC用介质材料进行掺杂改性从而抑制大量电子的产生，常用的方法是通过掺杂Mn2+、Mg2+等受主离子来对材料性能进行改善。
传统MLCC用介质材料多为X7R(-55～125℃，△C/C25℃≤15％)型，随着MLCC工作环境愈加恶劣，对MLCC的温度稳定性要求愈加严格，X7R型介质材料125℃的工作上限已经难以满足很多领域的实际应用需求，因此亟需开发出具有更高温度上限的MLCC用介质材料。X8R(-55～150℃，△C/C25℃≤15％)型MLCC用介质材料具有更好的温度稳定性，能够满足更多恶劣环境下的应用，其相关研究一直广受关注。
发明内容
本发明的目的，在于克服还原气氛下烧结时，BaTiO3基电介质材料半导化的问题，提供一种兼具低介电损耗和良好温度稳定性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贱金属电极MLCC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X8R型电介质材料的制备方法，具体步骤如下：
(1)按质量比BaTiO3：MnCO3：MgO：CaZrO3：SiO2：Al2O3：BaCO3＝100：0.5～2.0：0.1～2.0：1.0～3.0：0.5～1.5：0.25～1.5：0.5～1.5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：采用粉末压片机将造粒后的原料压制成坯体；
(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50sccmN2，烧结温度为1250～1350℃，保温3h，制成低损耗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)的坯体再经5℃/min升温速率至1000℃，再以2℃/min升温速率至1250～1350℃烧结。
本发明在原料中使用受主元素Mn2+、Mg2+以抑制钛酸钡基介质材料中Ti4+的变价，从而保证电介质具有良好的绝缘特性；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；通过调节烧结温度，使得材料性能达到了介电常数ε25℃～2461，介电损耗tanσ～0.0096，绝缘电阻率ρν～3.68×1011Ω·cm。
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、MnCO3、MgO、CaZrO3、SiO2、Al2O3、BaCO3按质量比100:1.0:1.5:1.5:1.0:0.5:1.0进行配料，以去离子水：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，生坯经3.5h空气中升温至600℃排胶，再在流速为50sccm N2气流中，以5℃/min升温速率至1000℃，再经2℃/min升至1300℃烧结，保温3h，制得低介电损耗X8R型抗还原电容器介质材料。
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与实施例1具有不同的烧结温度，其他制作工艺与实施例1完全相同。
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：
本发明具体实施例的主要工艺参数及其介电性能、TC特性详见表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X8R型电介质材料的制备方法，具体步骤如下：
(1)按质量比BaTiO3：MnCO3：MgO：CaZrO3：SiO2：Al2O3：BaCO3＝100：0.5～2.0：0.1～2.0：1.0～3.0：0.5～1.5：0.25～1.5：0.5～1.5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：采用粉末压片机将造粒后的原料压制成坯体；
(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50sccmN2，烧结温度为1250～1350℃，保温3h，制成低损耗X8R型电介质材料。
2.根据权利要求1所述的一种低损耗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)的坯体再经5℃/min升温速率至1000℃，再以2℃/min升温速率至1250～1350℃烧结。
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Cited By (5)

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CN110002864A (zh) * 2019-02-23 2019-07-12 天津大学 一种高绝缘抗还原型电介质材料的制备方法
CN110183224A (zh) * 2019-06-19 2019-08-30 天津大学 一种施受主共掺高介电常数低损耗电介质材料的制备方法
CN113248252A (zh) * 2021-06-10 2021-08-13 天津大学 一种稳定型mlcc用介质材料及其制备方法
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
CN113307622A (zh) * 2021-07-07 2021-08-27 天津大学 高性能抗还原钛酸钡基介质陶瓷及其制备方法

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CN110183224A (zh) * 2019-06-19 2019-08-30 天津大学 一种施受主共掺高介电常数低损耗电介质材料的制备方法
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