CN110577401A - 一种二氧化钛基介质材料的制备方法 - Google Patents

一种二氧化钛基介质材料的制备方法 Download PDF

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CN110577401A
CN110577401A CN201910752256.0A CN201910752256A CN110577401A CN 110577401 A CN110577401 A CN 110577401A CN 201910752256 A CN201910752256 A CN 201910752256A CN 110577401 A CN110577401 A CN 110577401A
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titanium dioxide
dielectric material
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李玲霞
王梦龙
王文波
张凯
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Tianjin University
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Abstract

本发明公开了一种二氧化钛基介质材料的制备方法，先按摩尔比TiO2：Ta2O5：Eu2O3＝97～99.5:0.125～0.75:0.125～0.75进行配料，经球磨、烘干、过筛、造粒、压制成坯体，坯体排胶后于1400～1450℃烧结，制成二氧化钛基介质材料。制品再于1100℃退火，制成巨介电常数、超低损耗的二氧化钛基介质材料。本发明具有优良的介电性能，介电常数ε25℃～65277，介电损耗tanσ～0.009。

Description

一种二氧化钛基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损耗、巨介电常数的二氧化钛基介质材料及其制备方法。
背景技术
目前，微型化、高集成化、低功耗正在成为微电子行业的重要发展方向。这需要电子元器件在实际应用过程中具有较小的体积、较高的存储能力、较低的能量损耗。电容器作为一种重要的电子元器件，其高储能、小型化主要依赖添加的介质材料是否具有高的介电常数，这对传统的高介电常数、高损耗的介质材料带来了巨大的挑战。
目前，电容器的小型化主要依赖于介质材料具有高的介电常数，但是研究发现介质材料在具有较高介电常数的同时很难兼具较低的介电损耗，这就对介电材料研究与制备形成了新的挑战。为了制备出满器件小型化要求的高介电常数、低损耗的介质瓷料，选择二氧化钛作为基体材料进行研究。
发明内容
本发明的目的，在于通过Eu元素掺杂克服TiO2基巨介电材料损耗高的现象，采用传统固相反应方法提供低损耗、巨介电常数的TiO2基电介质材料及其制备方法，以期望开发出能满足当今小型化多层陶瓷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。
一种二氧化钛基介质材料的制备方法，具体步骤如下：
(1)按摩尔比TiO2：Ta2O5：Eu2O3＝97～99.5:0.125～0.75:0.125～0.75进行配料，在去离子水中混合球磨12小时，再于120℃烘干，并过40目分样筛；
(2)造粒：将步骤(1)过筛后的粉料，外加8wt％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烧结炉中，烧结温度为1400℃～1450℃，保温10h，制成二氧化钛基电介质陶瓷材料。
(5)退火：将烧结后的陶瓷片状制品置于管式烧结炉中，退火温度为1100℃，保温1h，制成巨介电常数、超低损耗的二氧化钛基电介质陶瓷材料。
所述步骤(3)的坯体经3.5h由室温升温至550℃排胶。
所述步骤(4)的坯体由550℃再经10h升温至1400℃～1450℃进行烧结。
所述步骤(4)d的烧结温度为1440℃。
本发明的有益效果如下：
1.原料使用施/受主元素Ta5+/Eu3+掺杂二氧化钛基介质材料，可以使介质材料中产生氧空位，从而保证电介质具有高的介电常数；
2.使用Ta5+对二氧化钛材料的温度性能进行改善；
3.本发明公开的二氧化钛基电介质材料具有优良的介电性能，通过调节烧结温度，使得材料性能达到了介电常数ε25℃～65277，介电损耗tanσ～0.009。
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实施例。
实施例1
首先，用电子天平称量TiO2、Ta2O5、Eu2O3按摩尔比99.5︰0.125︰0.125进行配料，以去离子水：锆球：粉料质量比＝2︰1︰1掺入去离子水，混合后球磨12h，于120℃烘干，过40目筛，再外加质量百分比为8％的石蜡，过80目分样筛进行造粒。
将造粒后的粉料在2MPa下压制成Ф10×2mm的圆片生坯，经3.5h空气中由室温升温至550℃排胶，再经10h升温至1440℃烧结，保温10h。冷却至室温后，放入管式炉中升温至1100℃退火，保温1h，制得二氧化钛基电介质陶瓷材料。
在所得制品上下表面均匀涂覆银浆，经840℃烧渗制备电极，制得待测样品，测试介电性能及TC特性。测试结果详见表1。
实施例2
首先，用电子天平称量TiO2、Ta2O5、Eu2O3按摩尔比99:0.25:0.25进行配料，以去离子水：锆球：粉料质量比＝2:1:1掺入去离子水、锆球，混合后球磨12h，于120℃烘干，过40目筛，再外加质量百分比为8％的石蜡，过80目分样筛进行造粒。
将造粒后的粉料在2MPa下压制成Ф10×2.1mm的圆片生坯，经3.5h空气中由室温升温至550℃排胶，再经10h升温至1440℃烧结，保温10h。冷却至室温后，放入管式炉中升温至1100℃退火，保温1h，制得二氧化钛基电介质陶瓷材料。
在所得制品上下表面均匀涂覆银浆，经840℃烧渗制备电极，制得待测样品，测试介电性能及TC特性。测试结果详见表1。
实施例3
首先，用电子天平称量TiO2、Ta2O5、Eu2O3按摩尔比98:0.5:0.5进行配料，以去离子水：锆球：粉料＝2:1:1质量比掺入去离子水、锆球，混合后球磨12h，于120℃烘干，过40目筛，再外加质量百分比为8％的石蜡，过80目分样筛进行造粒。
将造粒后的粉料在2MPa下压制成Ф10×2.1mm的圆片生坯，经3.5h空气中由室温升温至550℃排胶，再经10h升温至1440℃烧结，保温10h，冷却至室温后，放入管式炉中升温至1100℃退火，保温1h，制得二氧化钛基电介质陶瓷材料。
在所得制品上下表面均匀涂覆银浆，经840℃烧渗制备电极，制得待测样品，测试介电性能及TC特性。测试结果详见表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同惠精密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。
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)

1.一种二氧化钛基介质材料的制备方法，具体步骤如下：
(1)按摩尔比TiO2：Ta2O5：Eu2O3＝97～99.5:0.125～0.75:0.125～0.75进行配料，在去离子水中混合球磨12小时，再于120℃烘干，并过40目分样筛；
(2)造粒：将步骤(1)过筛后的粉料，外加8wt％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烧结炉中，烧结温度为1400℃～1450℃，保温10h，制成二氧化钛基电介质陶瓷材料。
(5)退火：将烧结后的陶瓷片状制品置于管式烧结炉中，退火温度为1100℃，保温1h，制成巨介电常数、超低损耗的二氧化钛基电介质陶瓷材料。
2.根据权利要求1所述的一种二氧化钛基介质材料的制备方法，其特征在于，所述步骤(3)的坯体经3.5h由室温升温至550℃排胶。
3.根据权利要求1所述的一种二氧化钛基介质材料的制备方法，其特征在于，所述步骤(4)的坯体由550℃再经10h升温至1400℃～1450℃进行烧结。
4.根据权利要求1所述的一种二氧化钛基介质材料的制备方法，其特征在于，所述步骤(4)的烧结温度为1440℃。
CN201910752256.0A 2019-08-14 2019-08-14 一种二氧化钛基介质材料的制备方法 Pending CN110577401A (zh)

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CN109231981A (zh) * 2018-09-19 2019-01-18 天津大学 一种三、五价异质元素共掺的巨介电常数介质材料
CN109265162A (zh) * 2018-09-19 2019-01-25 天津大学 一种高性能巨介电常数介质材料

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US20220127197A1 (en) * 2020-03-20 2022-04-28 Guangdong Fenghua Advanced Technology Holding Co., Ltd. Multiphase ceramic material with giant dielectric constant, and preparation method thereof
CN113248253A (zh) * 2021-06-11 2021-08-13 天津大学 一种巨介电常数钛酸锶介质陶瓷及其制备方法

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