CN108275995A - 一种提升SrTiO3基巨介电常数电介质材料介电常数的方法 - Google Patents

一种提升SrTiO3基巨介电常数电介质材料介电常数的方法 Download PDF

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CN108275995A
CN108275995A CN201810070130.0A CN201810070130A CN108275995A CN 108275995 A CN108275995 A CN 108275995A CN 201810070130 A CN201810070130 A CN 201810070130A CN 108275995 A CN108275995 A CN 108275995A
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李玲霞
王文波
张宁
卢特
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Tianjin University
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Abstract

本发明公开了一种提升SrTiO3基巨介电常数电介质材料介电常数的方法，先将SrTiO3、Nb2O5、Li2O3、SiO2、La2O3、CuO、MnO和玻璃粉，按质量百分比94％、1.1737％、0.32627％，0.40％、1％、1％、0.7％、1.6％进行配料，再外加SrTiO3：SrCO3＝0.987～0.990：0.010～0.020摩尔比的SrCO3，经球磨、烘干、过筛后进行造粒，再压制成型为坯体，坯体排胶后于1300～1350℃进行还原气氛烧结，制成SrTiO3基巨介电常数电介质材料。本发明通过调节Sr/Ti的值，显著提升了介电常数(ε25℃～2.30×105)，并保证了较低的介电损耗(tanσ～0.050)。

Description

一种提升SrTiO3基巨介电常数电介质材料介电常数的方法
技术领域
本发明属于一种以成分为特征的陶瓷组合物，特别涉及一种在SrTiO3基巨介电常数电介质陶瓷材料的基础上进一步提升其介电常数的方法.
背景技术
电子元器件的微小型化是实现电子产品小型化过程中至关重要的一步，而电容器作为各类电路和器件组成中不可或缺的一类元器件，其微小型化的实现也广受关注，国内外众多学者也相继开展了相关的研究工作。电容器储存电荷的能力主要取决于其尺寸和所使用的介质材料的介电常数，介电常数大的介质材料能在保证相同储存能力的前提下大大缩小电容器尺寸。所以研发出具备优良性能巨介电常数材料(ε＞104)，可使电子科技中众多领域实现突破性进展。除此之外，介电损耗也是衡量材料体系的重要指标参数之一，与元器件的低损耗密切相关，低介电损耗的实现是实现材料在电子元器件行业生产应用的关键。
目前，正在研究的高介电常数材料大部分基于晶界阻挡层效应(internalbarrier layer capacitor(IBLC))，这些材料的巨介电常数通常由空间电荷所贡献。SrTiO3基陶瓷材料体系在空气中烧结时，Sr/Ti的值对于其介电性能有很大的影响，多余的Sr由于半径较大，会同晶界物质如玻璃相和SiO2等形成第二相，有利于介电性能的提升。
在还原气氛(N2/H2)下烧结，有利于SrTiO3基陶瓷材料氧空位的产生，在这个过程中，为保证电荷平衡会产生电子。根据晶界特性，氧空位以及一些缺陷主要聚集于晶界处，产生的电子于晶粒内部引起半导化效应，晶粒与晶界处的介电常数和电导率不同会造成晶粒晶界界面处聚集大量的空间电荷，形成界面极化从而引起巨介电常数。通过改变N2/H2通气时间、通气含量、烧结温度等以获得性能最优的SrTiO3基晶界层巨介电常数陶瓷。
发明内容
本发明的目的，是在一种新型SrTiO3基巨介电常数体系配方的基础上，调节Sr/Ti的值，实现该体系介电常数的进一步突破，并兼具低损耗(＜0.1)特性，使其能够有望成为制备大容量电容器的材料。
本发明通过如下技术方案予以实现。
一种提升SrTiO3基巨介电常数电介质材料介电常数的方法，具体步骤如下：
(1)将SrTiO3、Nb2O5、Li2O3、SiO2、La2O3、CuO、MnO和玻璃粉，按质量百分比94％、1.1737％、0.32627％，0.40％、1％、1％、0.7％、1.6％进行配料，在该配方的基础上分别再按照SrTiO3：SrCO3＝0.987～0.990：0.010～0.020的摩尔比添加SrCO3，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，再用粉末压片机压制成坯体；
(3)排胶：将制备好的坯体进行排胶；
(4)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，进行还原气氛烧结，烧结温度为1300～1350℃，保温3～3.5h，制成SrTiO3基巨介电常数电介质材料。
所述步骤(1)的玻璃粉的原料为Bi2O3、TiO2、ZnO和H3BO3，所占质量百分比分别为27.28％、23.15％、31.92％和17.65％。
所述步骤(2)的坯体为Ф10×1.5～2.1mm的圆片坯体。
所述步骤(3)的坯体经5小时升温至600℃排胶，升温速率为5℃/min，并保温5h。
所述步骤(4)的坯体在排胶结束后，再经5℃/min升温速率至1000℃烧结，再以2℃/min升温速率至1300～1350℃。
所述步骤(4)通入的气氛分别为N2＝50SCCM或者N2/H2＝64/4ml/min。
本发明的有益效果是
(1)原料使用施主元素Nb5+以促进介电常数大幅度提升，并以受主元素La3+和Mn2+和添加晶界滞留物等控制电子迁移过程以降低损耗。
(2)本发明公开的巨介电常数SrTiO3基介质材料具有优良的介电性能，通过调节Sr/Ti的值，显著提升了介电常数，达到了ε25℃～2.30×105。
(3)在显著提升介电常数的同时保证了较低的介电损耗(tanζ～0.050)。
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，本发明不局限于下述具体实施例。
实施例1
首先，用电子天平称量SrTiO3、Nb2O5、Li2O3、SiO2、La2O3、CuO、MnO和玻璃粉，按质量比94％、1.1737％、0.32627％，0.40％、1％、1％、0.7％、1.6％进行配料进行配料，共20g。在该配方的基础上按照SrTiO3：SrCO3＝0.987～0.990：0.010～0.020的摩尔比添加SrCO3。球磨4h，原料与去离子水与球石的混合比例为1:1:1，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Ф15×1.2mm的圆片生坯，经3.5h空气中升温至600℃排胶。在流速为N2＝50SCCM或者64ml/min N2和4ml/min H2混合气流中，再经2℃/min升至1350℃烧结，保温3～3.5h，制得巨介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。
实施例2-7
实施例2-7相对于实施例1具有不同的烧结温度、保温时间、通气含量和不同的Sr/Ti值，其它工艺条件与实施例1完全相同，本发明的主要工艺参数及其介电性能详见表1。
本发明的测试方法和检测设备如下：
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：
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 (6)

1.一种提升SrTiO3基巨介电常数电介质材料介电常数的方法，具体步骤如下：
(1)将SrTiO3、Nb2O5、Li2O3、SiO2、La2O3、CuO、MnO和玻璃粉，按质量百分比94％、1.1737％、0.32627％，0.40％、1％、1％、0.7％、1.6％进行配料，在该配方的基础上分别再按照SrTiO3：SrCO3＝0.987～0.990：0.010～0.020的摩尔比添加SrCO3，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，再用粉末压片机压制成坯体；
(3)排胶：将制备好的坯体进行排胶；
(4)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，进行还原气氛烧结，烧结温度为1300～1350℃，保温3～3.5h，制成SrTiO3基巨介电常数电介质材料。
2.根据权利要求1所述的一种提升SrTiO3基巨介电常数电介质材料介电常数的方法，其特征在于，所述步骤(1)的玻璃粉的原料为Bi2O3、TiO2、ZnO和H3BO3，所占质量百分比分别为27.28％、23.15％、31.92％和17.65％。
3.根据权利要求1所述的一种提升SrTiO3基巨介电常数电介质材料介电常数的方法，其特征在于，所述步骤(2)的坯体为Ф10×1.5～2.1mm的圆片坯体。
4.根据权利要求1所述的一种提升SrTiO3基巨介电常数电介质材料介电常数的方法，其特征在于，所述步骤(3)的坯体经5小时升温至600℃排胶，升温速率为5℃/min，并保温5h。
5.根据权利要求1所述的一种提升SrTiO3基巨介电常数电介质材料介电常数的方法，其特征在于，所述步骤(4)的坯体在排胶结束后，再经5℃/min升温速率至1000℃烧结，再以2℃/min升温速率至1300～1350℃。
6.根据权利要求1所述的一种提升SrTiO3基巨介电常数电介质材料介电常数的方法，其特征在于，所述步骤(4)通入的气氛分别为N2＝50SCCM或者N2/H2＝64/4ml/min。
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