CN110407575A - 一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法 - Google Patents

一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法 Download PDF

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CN110407575A
CN110407575A CN201910579098.3A CN201910579098A CN110407575A CN 110407575 A CN110407575 A CN 110407575A CN 201910579098 A CN201910579098 A CN 201910579098A CN 110407575 A CN110407575 A CN 110407575A
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李玲霞
王梦龙
王文波
张凯
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Abstract

本发明公开了一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法，先按摩尔比TiO2：Ta2O5：Eu2O3＝97～99.5:0.125～0.75:0.125～0.75进行配料，再经球磨、过筛、造粒后压制成坯体，坯体排胶后于1400～1450℃烧结，制成超宽温度范围巨介电常数低损耗二氧化钛基电介质陶瓷材料。本发明达到了介电常数ε25℃～74357，介电损耗tanσ～0.0318，在‑150℃‑150℃满足ΔC/C<10％的需求。

Description

一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法
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超宽工作温度范围、较低损耗、巨介电常数的二氧化钛基电介质陶瓷材料及其制备方法。
背景技术
目前，全球微电子行业正向微型化、高集成化、大容量画、低功耗等方向发展。对电子元器件提出更小的体积空间、更好的存储能力、更低的功耗要求。高储能、微型化电容器的制备关键在于实现填充的介质材料具有非常高的介电常数，传统的介质材料已经不能满足对应的性能要求。
目前高介电常数瓷料在小型化方面具有广泛的应用，在获得高介电常数的同时还应满足低损耗以及宽的工作温度范围的要求，这就对材料的研发造成一定的难度。为了制备出满器件小型化要求的高介电常数、低损耗以及宽的工作温度范围的介质瓷料，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基巨介电材料温度稳定性差的现象，采用传统固相反应方法提供具有超宽工作温度范围、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。
一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法，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，添加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，制成超宽温度范围巨介电常数低损耗二氧化钛基电介质陶瓷材料。
所述步骤(2)的坯体为Ф10×2.0～3.0mm的圆片坯体。
所述步骤(3)是坯体经3.5h由室温升温至550℃排胶。
所述步骤(4)是坯体由550℃再经10h升温至1440℃进行烧结。
所述步骤(4)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℃～74357，介电损耗tanσ～0.0318，在-150℃-150℃满足ΔC/C<10％的需求。
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，本发明不局限于实例：
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，烘干后过40目筛，再外加质量百分比为8％的石蜡，过80目分样筛造粒。
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，制得超宽温度范围、低损耗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，烘干后过40目筛，再外加质量百分比为8％的石蜡，过80目分样筛造粒。
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，制得超宽温度范围、低损耗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，烘干后过40目筛，再外加质量百分比为8％的石蜡，过80目分样筛造粒。
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，制得超宽温度范围、低损耗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。测量样品在温区-150℃～150℃内的电容量，采用下述公式计算电容量变化率：
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 (5)

1.一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法，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，添加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，制成超宽温度范围巨介电常数低损耗二氧化钛基电介质陶瓷材料。
2.根据权利要求1所述的一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法，其特征在于，所述步骤(2)的坯体为Ф10×2.0～3.0mm的圆片坯体。
3.根据权利要求1所述的一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法，其特征在于，所述步骤(3)是坯体经3.5h由室温升温至550℃排胶。
4.根据权利要求1所述的一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法，其特征在于，所述步骤(4)是坯体由550℃再经10h升温至1440℃进行烧结。
5.根据权利要求1所述的一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法，其特征在于，所述步骤(4)的烧结温度为1440℃。
CN201910579098.3A 2019-06-28 2019-06-28 一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法 Pending CN110407575A (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
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