CN109265162A - 一种高性能巨介电常数介质材料 - Google Patents
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Abstract
本发明公开了一种高性能巨介电常数介质材料,以TiO2粉体为基料,在此基础上,按化学式(La0.5Ta0.5)xTi1‑xO2进行三价La3+、五价Ta5+元素共掺杂,其中x=0.01~0.05。先将La2O3、Ta2O5和TiO2按摩尔比x/4:x/4:1‑x,其中x=0.01~0.05进行配料,经球磨、烘干、过筛后进行造粒,再压制成坯体,坯体于1400~1425℃烧结,得到高性能巨介电常数介质材料。本发明相对于现有技术具有介电常数高,损耗低的特性,且制备工艺简单、重复性好,利于工业化大规模生产。
Description
技术领域
本发明属于一种以成分为特征的陶瓷组合物,特别涉及一种高性能巨介电常数介质材料及其制备方法。
背景技术
随着无线通讯技术的高速发展,在对电子元器件的微型化、高频化和高储能设备的迫切需求背景下,研发出具备良好的温度稳定性及频率特性的低介电损耗巨介电常数材料(ε>104),可使电子科技中众多领域实现突破性进展,例如有利于MLCC(Multi-layerCeramic Capacitors)器件的薄层化和小型化以及制备出超大容量MLCC;制备出单层高储能电容器,即单层可满足传统MLCC容量需求,节约电极成本。
介质在电场中受电场作用发生极化,介质的极化能力越强,其介电常数越大,实现大容量的同时所需材料的体积越小,实际生产应用中得以极大地缩减器件尺寸,实现集成电路的小型化和微型化。除此之外,介电损耗、介电常数频率与温度特性等指标也是衡量材料体系的重要指标参数,与元器件的低损耗、环境稳定性密切相关,其指标参数的优异性是得以实际生产应用的关键,目前,研究较多的巨介电常数材料体系并不能同时满足上述要求,如BaTiO3类钙钛矿体系,通过A、B位离子掺杂方式如(Ba0.9Nd0.1)TiO3、 Ba(Ti0.86Zr0.14)O3、(Ba0.87Ca0.09Sr0.04)(Ti0.90Zr0.04Sn0.06)O3等体系,以使居里峰左移至室温附近使其具有位移型扩散转变的弛豫铁电体特征,然而这种体系的巨介电常数仅仅体现在室温附近,具有严重的温度依赖性;另外一种常见的巨介电常数CCTO体系,其在低频下可表现出>105的介电常数,但因凭借内部阻挡层电容(IBLC)机理引起强烈的界面极化以贡献介电常数,但也恰因为界面极化的是一种慢极化的表现方式,导致介电常数随着频率的增加严重下降,以至于1Khz或1MHz下介电常数<10000,且具有相对较高的介电损耗 (>0.2)。
三五价共掺TiO2体系于2013年被报道,凭借其优良的介电性能,高频下仍具有巨介性质,并拥有良好的温度稳定性,被寄予新一代高储能电容器的制备材料,目前大多拓宽此体系均基于电子钉扎效应(EPDD)以同时实现巨介电常数和低损耗特性,但采用大半径离子掺杂引起晶格畸变,使得缺陷簇的产生以及对电子的束缚更加稳固,另外大半径离子掺杂会引起第二相的产生,同晶粒之间的一直界面会造成IBLC的产生,通过改善掺杂比例以实现EPDD同IBLC之间的最优组合,以达到进一步提高介电常数和降低介电损耗的目的。
发明内容
本发明的目的,在于克服现有巨介电常数体系损耗高、频段窄等缺点,制备出宽频范围低介电损耗、具有优良的温度稳定特性的巨介电常数材料。
本发明通过如下技术方案予以实现。
一种高性能巨介电常数介质材料,以TiO2粉体为基料,在此基础上,按化学式(La0.5Ta0.5)xTi1-xO2进行三价La3+、五价Ta5+元素共掺杂,其中x=0.01~0.05;
该高性能巨介电常数介质材料的制备方法,具有如下步骤:
(1)将La2O3、Ta2O5和TiO2按摩尔比x/4:x/4:1-x,其中x=0.01~0.05进行配料,混合球磨10小时后烘干、过40目分样筛;
(2)造粒:将步骤(1)过筛后的粉料,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,坯体于1400~1425℃烧结得到高性能巨介电常数介质材料。
所述步骤(2)的坯体为Ф10×1.5~2.1mm的圆片坯体。
所述步骤(2)的坯体经3.5小时升温至550℃进行排胶,再经2℃/min升温速率至1400~ 1425℃烧结,保温10小时。
本发明公开的高性能巨介电常数介质材料,相对于现有技术具有介电常数高,损耗低的特性,且制备工艺简单、重复性好,有利于工业化大规模生产。
具体实施方式
下面将结合具体实施例对本发明作进一步的详细描述。
首先,按照摩尔比例(La0.5Ta0.5)xTi1-xO2(x=0.01~0.05),用电子天平称量分析纯级 (≥99%)的La2O3、Ta2O5和TiO2,并进行混合,以去离子水作为球磨介质,球磨10小时后烘干、过40目筛,再外加质量百分比为7%的石蜡,过80目分样筛进行造粒。
再将造粒后的粉料取0.5g~0.8g在4MPa下压制成Ф10×1.5~2.1mm的圆片坯体,坯体经3.5小时升温至550℃排胶,再经15小时升至1400~1425℃烧结(2℃/min升温速率),保温10小时,制得巨介电常数、低损耗介质材料。
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。
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1kHz,电压为1V)
使用HEWLETT PACKARD 4278A型电容量测试仪测试样品的电容量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原料配比详见表1,实施例1~15的不同组分及其介电性能详见表2,其他制作工艺完全相同。
表1
表2
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 (3)
1.一种高性能巨介电常数介质材料,以TiO2粉体为基料,在此基础上,按化学式(La0.5Ta0.5)xTi1-xO2进行三价La3+、五价Ta5+元素共掺杂,其中x=0.01~0.05。
该高性能巨介电常数介质材料的制备方法,具有如下步骤:
(1)将La2O3、Ta2O5和TiO2按摩尔比x/4:x/4:1-x,其中x=0.01~0.05进行配料,混合球磨10小时后烘干、过40目分样筛;
(2)造粒:将步骤(1)过筛后的粉料,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,坯体于1400~1425℃烧结,得到高性能巨介电常数介质材料。
2.根据权利要求1所述的一种高性能巨介电常数介质材料,其特征在于,所述步骤(2)的坯体为Ф10×1.5~2.1mm的圆片坯体。
3.根据权利要求1所述的一种高性能巨介电常数介质材料,其特征在于,所述步骤(2)的坯体经3.5小时升温至550℃进行排胶,再经2℃/min升温速率至1400~1425℃烧结,保温10小时。
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CN110407575A (zh) * | 2019-06-28 | 2019-11-05 | 天津大学 | 一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法 |
CN110451950A (zh) * | 2019-08-14 | 2019-11-15 | 天津大学 | 一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法 |
CN110577401A (zh) * | 2019-08-14 | 2019-12-17 | 天津大学 | 一种二氧化钛基介质材料的制备方法 |
CN111410527A (zh) * | 2020-03-20 | 2020-07-14 | 广东风华高新科技股份有限公司 | 一种复相巨介电陶瓷材料及其制备方法 |
CN116063849A (zh) * | 2023-02-15 | 2023-05-05 | 哈尔滨理工大学 | 一种高介电复合材料及其制备方法和应用 |
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Cited By (7)
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CN110407575A (zh) * | 2019-06-28 | 2019-11-05 | 天津大学 | 一种施受主共掺二氧化钛基电介质陶瓷材料的制备方法 |
CN110451950A (zh) * | 2019-08-14 | 2019-11-15 | 天津大学 | 一种二氧化钛基巨介电常数电介质陶瓷材料的改性方法 |
CN110577401A (zh) * | 2019-08-14 | 2019-12-17 | 天津大学 | 一种二氧化钛基介质材料的制备方法 |
CN111410527A (zh) * | 2020-03-20 | 2020-07-14 | 广东风华高新科技股份有限公司 | 一种复相巨介电陶瓷材料及其制备方法 |
CN111410527B (zh) * | 2020-03-20 | 2021-06-22 | 广东风华高新科技股份有限公司 | 一种复相巨介电陶瓷材料及其制备方法 |
CN116063849A (zh) * | 2023-02-15 | 2023-05-05 | 哈尔滨理工大学 | 一种高介电复合材料及其制备方法和应用 |
CN116063849B (zh) * | 2023-02-15 | 2023-08-15 | 哈尔滨理工大学 | 一种高介电复合材料及其制备方法和应用 |
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