CN108191428A - 一种制备SrTiO3基巨介电常数介质陶瓷材料的方法 - Google Patents
一种制备SrTiO3基巨介电常数介质陶瓷材料的方法 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 15
- 238000000034 method Methods 0.000 title claims abstract description 14
- 229910002367 SrTiO Inorganic materials 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 10
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 8
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910002370 SrTiO3 Inorganic materials 0.000 claims abstract description 7
- 239000011521 glass Substances 0.000 claims abstract description 7
- 239000000428 dust Substances 0.000 claims abstract description 6
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 5
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 5
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 5
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 5
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 5
- 238000000498 ball milling Methods 0.000 claims abstract description 4
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims abstract description 4
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 4
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 239000011230 binding agent Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000009413 insulation Methods 0.000 abstract description 9
- 239000003990 capacitor Substances 0.000 abstract description 4
- 238000005469 granulation Methods 0.000 abstract description 2
- 230000003179 granulation Effects 0.000 abstract description 2
- 238000007873 sieving Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000001967 indiganyl group Chemical group [H][In]([H])[*] 0.000 description 1
- 230000008595 infiltration Effects 0.000 description 1
- 238000001764 infiltration Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 210000003739 neck Anatomy 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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Abstract
本发明公开了一种制备SrTiO3基巨介电常数介质陶瓷材料的方法，先将SrTiO3、Nb2O5、Li2CO3、SiO2、In2O3、MnO2、CuO和玻璃粉，按质量百分比94.000％、1.174％、0.326％、0.400％、1.000％、0.700％、1.000％、1.600％进行配料，经球磨、过筛、造粒，再压制成坯体，排胶后坯体于还原气氛中1300～1350℃烧结保温。本发明具有较高的绝缘电阻率(RΩ～9.38×108)和巨介电常数(ε25℃～1.55×105)，实现了介电常数大于105的突破，有望成为制备大容量电容器的介质陶瓷材料。
Description
技术领域
本发明属于一种以成分为特征的陶瓷组合物，特别涉及一种优化气氛烧结工艺以获得巨介电常数和高绝缘特性的SrTiO3基巨介电常数介质陶瓷材料。
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、高储能、低损耗设备的迫切需求背景下，研发出具备优良性能巨介电常数材料(ε＞103)，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 Ceramic 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。
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、绝缘电阻率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、可靠性密切相关，其指标参数的优异性是得以实现生产应用于电子元器件行业的关键。
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internal barrierlayer capacitor(IBLC)，这些材料由于内部存在半导化，通常具有较低的绝缘电阻率。故常通过掺杂的方式提高晶界电阻，以提高材料的绝缘电阻率。
还原气氛(N2/H2)烧结，造成烧结制品内部部分晶格氧同还原气体结合，以氧空位形式出现，电子随着产生以使电荷达到平衡，根据晶界特性，氧空位以及一些缺陷聚集于晶界处，电子于晶粒内部引起半导化效应，彼此具有不同介电常数不同电导率会造成晶粒晶界界面处形成大量的空间电荷聚集，形成界面极化从而引起巨介电常数。通过改变N2/H2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介质陶瓷材料。
发明内容
本发明的目的，是在现有技术的基础上进一步提高SrTiO3基晶界层巨介电常数介质陶瓷材料的绝缘电阻率，获得巨介电常数，提供一种新型SrTiO3基巨介电常数体系配方，优化还原气氛烧结工艺，实现介电常数大于105的突破，并兼具高绝缘(>108)特性，使其能够有望成为制备大容量电容器的介质陶瓷材料。
本发明通过如下技术方案予以实现。
一种制备SrTiO3基巨介电常数介质陶瓷材料的方法，具有如下步骤：
(1)将SrTiO3、Nb2O5、Li2CO3、SiO2、In2O3、MnO2、CuO和玻璃粉，按质量百分比94.000％、1.174％、0.326％、0.400％、1.000％、0.700％、1.000％、1.600％进行配料，混合球磨12小时后于100℃烘干，并过40目分样筛；
(2)造粒：将步骤(1)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；
(3)排胶：将上述坯体进行排胶；
(4)烧结：将排胶后的坯体置于还原气氛炉，通入N2/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。
所述步骤(1)的玻璃粉的原料组成及其质量百分比含量为Bi2O3︰TiO2︰ZnO︰H3BO3＝27.28％︰23.15％︰31.92％︰17.65％。
所述步骤(2)的坯体为Ф10×1.5～2.1mm的圆片生坯。
所述步骤(3)的坯体经5小时升温至600℃排胶，升温速率为2℃/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℃，再以2℃/min升温速率至1300～1350℃烧结。
所述步骤(4)N2/H2混合气体的流速为64～50ml/min N2和1～4ml/min H2。
本发明的有益效果如下：
(1)本发明的原料使用CuO、SiO2、玻璃等物质，提高了晶界电阻，绝缘电阻率得到明显提高。
(2)本发明公开的巨介电常数SrTiO3基介质陶瓷材料具有优良的介电性能：具有较高的绝缘电阻率(RΩ～9.38×108)，和巨介电常数(ε25℃～1.55×105)。
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SrTiO3、Nb2O5、Li2CO3、SiO2、In2O3、MnO2、CuO和玻璃粉，按质量比94％、1.1737％、0.32627％、0.4％、1％、0.7％、1％、1.6％进行配料，共25g。原料与去离子水与球石的混合比例为1:30:15，球磨12h，烘干后外加质量百分比为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Ф10×1.2mm的圆片坯体，经3.5h空气中升温至600℃排胶。在流速为64ml/min N2和4ml/min H2混合气流中，再经2℃/min升至1350℃烧结，保温3.5h，制得SrTiO3基巨介电常数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2～5
实施例2～5与实施例1具有不同烧结温度及不同通气含量以及不同的保温时间，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)
1.一种制备SrTiO3基巨介电常数介质陶瓷材料的方法，具有如下步骤：
(1)将SrTiO3、Nb2O5、Li2CO3、SiO2、In2O3、MnO2、CuO和玻璃粉，按质量百分比94.000％、1.174％、0.326％、0.400％、1.000％、0.700％、1.000％、1.600％进行配料，混合球磨12小时后于100℃烘干，并过40目分样筛；
(2)造粒：将步骤(1)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；
(3)排胶：将上述坯体进行排胶；
(4)烧结：将排胶后的坯体置于还原气氛炉，通入N2/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。
2.根据权利要求1所述的一种制备SrTiO3基巨介电常数介质陶瓷材料的方法，所述步骤(1)的玻璃粉的原料组成及其质量百分比含量为Bi2O3︰TiO2︰ZnO︰H3BO3＝27.28％︰23.15％︰31.92％︰17.65％。
3.根据权利要求1所述的一种制备SrTiO3基巨介电常数介质陶瓷材料的方法，所述步骤(2)的坯体为Ф10×1.5～2.1mm的圆片生坯。
4.根据权利要求1所述的一种制备SrTiO3基巨介电常数介质陶瓷材料的方法，所述步骤(3)的坯体经5小时升温至600℃排胶，升温速率为2℃/min，并保温5h。
5.根据权利要求1所述的一种制备SrTiO3基巨介电常数介质陶瓷材料的方法，所述步骤(4)的坯体在排胶结束后，再经5℃/min升温速率至1000℃，再以2℃/min升温速率至1300～1350℃烧结。
6.根据权利要求1所述的一种制备SrTiO3基巨介电常数介质陶瓷材料的方法，所述步骤(4)N2/H2混合气体的流速为64～50ml/min N2和1～4ml/min H2。
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341192A (zh) * | 2020-11-20 | 2021-02-09 | 西安合容新能源科技有限公司 | 一种高储能密度钛酸铋钠基无铅介质材料及其制备方法 |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60107803A (ja) * | 1983-11-17 | 1985-06-13 | 松下電器産業株式会社 | 電圧依存性非直線抵抗体磁器組成物 |
| CN102557672A (zh) * | 2012-01-05 | 2012-07-11 | 江苏大学 | 一种添加物及其降低钛酸钡锶电容器陶瓷烧结温度的用途 |
| CN103508732A (zh) * | 2013-10-08 | 2014-01-15 | 江苏大学 | 一种低温度系数晶界层陶瓷电容器介质及其制备方法 |
| CN105130421A (zh) * | 2015-09-07 | 2015-12-09 | 武汉理工大学 | 一种Ti位高价取代SrTiO3基巨介电陶瓷及其制备方法 |
| CN106673644A (zh) * | 2017-01-10 | 2017-05-17 | 北京元六鸿远电子科技股份有限公司 | 一种用于中温烧结的钛酸锶基储能介质材料 |
-
2018
- 2018-02-02 CN CN201810107739.0A patent/CN108191428A/zh active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60107803A (ja) * | 1983-11-17 | 1985-06-13 | 松下電器産業株式会社 | 電圧依存性非直線抵抗体磁器組成物 |
| CN102557672A (zh) * | 2012-01-05 | 2012-07-11 | 江苏大学 | 一种添加物及其降低钛酸钡锶电容器陶瓷烧结温度的用途 |
| CN103508732A (zh) * | 2013-10-08 | 2014-01-15 | 江苏大学 | 一种低温度系数晶界层陶瓷电容器介质及其制备方法 |
| CN105130421A (zh) * | 2015-09-07 | 2015-12-09 | 武汉理工大学 | 一种Ti位高价取代SrTiO3基巨介电陶瓷及其制备方法 |
| CN106673644A (zh) * | 2017-01-10 | 2017-05-17 | 北京元六鸿远电子科技股份有限公司 | 一种用于中温烧结的钛酸锶基储能介质材料 |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112341192A (zh) * | 2020-11-20 | 2021-02-09 | 西安合容新能源科技有限公司 | 一种高储能密度钛酸铋钠基无铅介质材料及其制备方法 |
| CN112341192B (zh) * | 2020-11-20 | 2022-07-22 | 西安合容新能源科技有限公司 | 一种高储能密度钛酸铋钠基无铅介质材料及其制备方法 |
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