CN107399967A - 一种超低损耗巨介电常数温度稳定型电容器介质材料 - Google Patents
一种超低损耗巨介电常数温度稳定型电容器介质材料 Download PDFInfo
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 16
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- 239000000463 material Substances 0.000 claims abstract description 14
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000126 substance Substances 0.000 claims abstract description 7
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010792 warming Methods 0.000 claims abstract description 6
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims abstract description 5
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Abstract
本发明公开了一种超低损耗巨介电常数温度稳定型电容器介质材料，以TiO2为基料，按化学式(La0.5Nb0.5)xTi1‑xO2进行三价La3+、五价Nb5+元素共掺杂，其中x＝0.005～0.10。先将La2O3、Nb2O5和TiO2按合化学式配料，经球磨、烘干、过筛，再外加质量百分比为7wt％石蜡作，进行造粒，压制为成型的坯体；坯体于1300℃～1400℃烧结，制得电容器介质材料。本发明在‑55℃～125℃温区内，电容量变化率在±8.9％以内，升温至150℃，电容量变化率最大为+14.8，满足且具有巨介电常数(最大值为100179)、低损耗(最低值为0.019)的性能要求，同时1MHz频率下介电常数达到89607，满足电子材料高频化的发展要求。工艺简单、重复性好且成本低廉，有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，特别涉及一种巨介电常数电容器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，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-layer CeramicCapacitors)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。
通常把介电常数实部超过104的材料称为巨介电常数材料。电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，但因其内阻挡层电容(IBLC)机理引起强烈的界面极化贡献介电常数，同时也恰因为界面极化的原因导致其随频率的变化严重下降，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)。
发明内容
本发明的目的，在于克服现有巨介电常数电容器介质体系损耗高、频段窄等缺点，提供有一种宽频范围、低介电损耗、具有优良的温度稳定特性的巨介电常数电容器介质材料。
本发明通过如下技术方案予以实现。
一种超低损耗巨介电常数温度稳定型电容器介质材料，以TiO2粉体为基料，在此基础上，按化学式(La0.5Nb0.5)xTi1-xO2进行三价La3+、五价Nb5+元素共掺杂，其中x＝0.005～0.10；
所述(La0.5Nb0.5)xTi1-xO2化合物，将原料La2O3、Nb2O5和TiO2按摩尔比x/4：x/4：1-x，其中x＝0.005～0.10合成；
上述电容器介质材料的制备方法，具有如下步骤：
(1)将La2O3、Nb2O5和TiO2按摩尔比x/4：x/4：1-x，其中x＝0.005～0.10进行配料，混合球磨10小时后烘干、过40目分样筛；
(2)将步骤(1)过筛后的粉料，外加质量百分比为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为成型的坯体；
(3)将步骤(2)的坯体于1300℃～1400℃烧结，升温速率为2～5℃/min，保温5～11小时，得到超低损耗巨介电常数温度稳定型电容器介质材料。
所述步骤(1)的化学式(La0.5Nb0.5)xTi1-xO2，其中x＝0.03。
所述步骤(2)的坯体为Ф10×1.5mm的圆片坯体。
所述步骤(3)的坯体经3.5小时升温至550℃排胶，再经2/min升温速率至1350℃烧结，保温10小时。
本发明的有益效果如下：
1.本发明公开的巨介电常数电容器介质材料，相对其它巨介电常数体系材料具有介电常数更高，损耗更低等特性。
2.工艺步骤简单、重复性好且成本低廉有利于工业化大规模生产。
3.本发明公开的多层陶瓷电容器介质材料具有优良的介电性能：在-55℃～125℃温区内，电容量变化率在±8.9％以内，温度稳定性较好，升温至150℃，电容量变化率最大为+14.8，满足且具有巨介电常数(最大值为100179)、低损耗(最低值为0.019)的性能要求，同时1MHz频率下介电常数达到89607，满足电子材料高频化的发展要求。
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。
本发明采用分析纯级试剂(≥99％)为原料。
实施例1
(1)以化学式(La0.5Nb0.5)xTi1-xO2进行配料，其中x＝0.03，用电子天平称量0.5967gLa2O3和0.4868g Nb2O5，18.9165g TiO2，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；
(2)将过筛后的粉料，外加质量百分比为7wt％石蜡作为粘结剂，过80目筛，进行造粒，再取造粒后的粉料0.5g～0.8g在4MPa下压制成型为坯体，坯体为Ф10×1.5mm的圆片生坯；
(3)坯体先经3.5小时升温至550℃排胶，再经7小时(2℃/min)升至1350℃烧结，保温10小时，制得超低损耗巨介电常数温度稳定型电容器介质材料。
(4)在所得制品上下表面均匀涂覆银浆，经820℃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2-14
实施例2-14的除具体原料配比及主要工艺参数之外，其他工艺方法与实施例1完全相同。
实施例1-14的具体原料配比及其主要工艺参数详见表1。
表1
在上述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：
实施例1-14的介电性能及TC特性的测试结果详见表2。
表2
坯体经3.5小时升温至550℃排胶，再经2/min升温速率至1350℃烧结，保温10小时，介电性能最优，即介电常数最大，损耗最小。
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)
1.一种超低损耗巨介电常数温度稳定型电容器介质材料，以TiO2粉体为基料，在此基础上，按化学式(La0.5Nb0.5)xTi1-xO2进行三价La3+、五价Nb5+元素共掺杂，其中x＝0.005～0.10；
所述(La0.5Nb0.5)xTi1-xO2化合物，将原料La2O3、Nb2O5和TiO2按摩尔比x/4：x/4：1-x，其中x＝0.005～0.10合成。
上述电容器介质材料的制备方法，具有如下步骤：
(1)将La2O3、Nb2O5和TiO2按摩尔比x/4：x/4：1-x，其中x＝0.005～0.10进行配料，混合球磨10小时后烘干、过40目分样筛；
(2)将步骤(1)过筛后的粉料，外加质量百分比为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为成型的坯体；
(3)将步骤(2)的坯体于1300℃～1400℃烧结，升温速率为2～5℃/min，保温5～11小时，得到超低损耗巨介电常数温度稳定型电容器介质材料。
2.根据权利要求1所述的一种超低损耗巨介电常数温度稳定型电容器介质材料，其特征在于，所述步骤(1)的化学式(La0.5Nb0.5)xTi1-xO2，其中x＝0.03。
3.根据权利要求1所述的一种超低损耗巨介电常数温度稳定型电容器介质材料，其特征在于，所述步骤(2)的坯体为Ф10×1.5mm的圆片坯体。
4.根据权利要求1所述的一种超低损耗巨介电常数温度稳定型电容器介质材料，其特征在于，所述步骤(3)的坯体经3.5小时升温至550℃排胶，再经2/min升温速率至1350℃烧结，保温10小时。
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