CN106278258A - 一种mlcc用高介电常数陶瓷材料及其制备方法 - Google Patents
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 25
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Chemical compound O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000498 ball milling Methods 0.000 claims abstract description 13
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 8
- 238000005245 sintering Methods 0.000 claims abstract description 6
- 239000000126 substance Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 229920000728 polyester Polymers 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 6
- 239000003985 ceramic capacitor Substances 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 239000003989 dielectric material Substances 0.000 description 2
- VEAHHGDAQKXNNG-UHFFFAOYSA-H C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-].[Zr+4].[Ba+2].C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-].C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-] Chemical compound C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-].[Zr+4].[Ba+2].C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-].C(C=1C(C(=O)[O-])=CC=CC1)(=O)[O-] VEAHHGDAQKXNNG-UHFFFAOYSA-H 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 238000010295 mobile communication Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002365 multiple layer Substances 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/48—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates
- C04B35/49—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zirconium or hafnium oxides, zirconates, zircon or hafnates containing also titanium oxides or titanates
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/08—Inorganic dielectrics
- H01G4/12—Ceramic dielectrics
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3251—Niobium oxides, niobates, tantalum oxides, tantalates, or oxide-forming salts thereof
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Abstract
本发明公开了一种MLCC用高介电常数陶瓷材料，其化学式为：Ba(Zr0.2Ti0.8)O3+xmol％Nb2O5，其中外加的Nb2O5为x＝0.1～0.6mol％。先将BaCO3、TiO2、ZrO2按化学计量式Ba(Zr0.2Ti0.8)O3进行配料，经球磨、烘干、过筛后于1000～1200℃预烧；再与外加的Nb2O5混合，再经球磨、烘干、过筛后压制成型为坯体；坯体于1250℃～1270℃烧结，制成高介电常数陶瓷材料。本发明的室温介电常数εr为2944～38328，介电损耗为0.005～0.1。
Description
技术领域
本发明属于电子信息材料与元器件领域，特别涉及一种用于MLCC的高介电常数材料的制备方法
背景技术
多层片式陶瓷电容器(Multi-Layer Ceramic Capacitor，MLCC)是一种适用于SMT(Surface Mount Technology)表面贴装的片式电容器，几乎所有的电子整机都必须配套应用。特别是移动通信产品、计算机、数码相机、新一代数字化家电产品，而且随着电子整机产品趋向于轻、薄、短、小和表面贴装技术的日益普及，MLCC也逐渐向小型化、微型化的方向发展。
为了适应MLCC的小型化发展趋势，对MLCC用介质材料也提出了高介电常数、低介电损耗的要求。BaTiO3基铁电陶瓷是MLCC的核心材料，锆钛酸钡(Ba(Zr0.2Ti0.8)O3)是ZrO2掺杂BaTiO3所形成固溶体系。该体系具有高的介电常数(～20000)和适中的介电损耗(～0.08)。通过对其进行掺杂改性，可以进一步提高材料的介电常数，降低介电损耗。
发明内容
本发明的目的，是为进一步提高Ba(Zr0.2Ti0.8)O3介质材料的介电常数，并进一步降低材料的介电损耗，适应MLCC逐渐向小型化方向发展的需要。以BaCO3、TiO2、ZrO2、Nb2O5为原料，通过固相法制备MLCC用高介电常数陶瓷材料。
本发明通过如下技术方案予以实现。
一种MLCC用高介电常数陶瓷材料，其化学式为：Ba(Zr0.2Ti0.8)O3+xmol％Nb2O5，其中外加的Nb2O5为x＝0.05～0.6mol％；
该MLCC用高介电常数陶瓷材料的制备方法，具体步骤如下：
(1)将BaCO3、TiO2、ZrO2按化学计量式Ba(Zr0.2Ti0.8)O3进行配料，将原料放入聚酯罐中，加入去离子水和氧化锆球后，球磨4～8小时；
(2)将步骤(1)球磨后的原料放入干燥箱中，于100～120℃烘干，然后过40目筛；
(3)将步骤(2)过筛后的原料放入中温炉中，于1000～1200℃预烧，保温2～6小时；
(4)将步骤(3)预烧后的原料与外加的0.05～0.6mol％Nb2O5进行混合，放入球磨罐中，加入氧化锆球和去离子水，球磨10～14小时，烘干后过筛，再用粉末压片机压制成型为坯体；
(5)将步骤(4)的坯体于1250℃～1270℃烧结，保温2～6小时，制成MLCC用高介电常数陶瓷材料。
所述步骤(1)、步骤(4)球磨工艺的原料与去离子水和氧化锆球的质量比为1︰1︰1。
所述步骤(4)的坯体直径为10mm，厚度为1mm。
所述步骤(4)的坯体成型压力为2～8Mpa。
所述步骤(5)的烧结温度为1270℃。
所述步骤(4)外加Nb2O5的掺杂比例为0.2mol％。
本发明通过固相法制备了MLCC用高介电常数陶瓷材料Ba(Zr0.2Ti0.8)O3+xmol％Nb2O5。其室温介电常数εr为2944～38328，介电损耗为0.005～0.1。
具体实施方式
本发明以BaCO3(分析纯)、TiO2(分析纯)、ZrO2(分析纯)、Nb2O5(分析纯)为初始原料，通过简单固相法制备陶瓷电容器用介质陶瓷材料。
具体实施方案如下：
(1)将BaCO3、TiO2、ZrO2按化学计量式Ba(Zr0.2Ti0.8)O3进行配料,将混合原料放入聚酯罐中，加入去离子水和氧化锆球后，在行星式球磨机上球磨6小时，球磨机转速为400转/分；
(2)将球磨后的原料置于干燥箱中，于100℃烘干，而后过40目筛；
(3)将过筛后的原料放入中温炉，于1100℃预烧，保温4小时；
(4)将步骤(3)预烧后的原料按按化学计量式Ba(Zr0.2Ti0.8)O3+xmol％，外加Nb2O5为x＝0.05～0.6mol％进行混合，放入球磨罐中，加入氧化锆球和去离子水，球磨12小时，于100℃烘干，而后过40目筛，再用粉末压片机以4MPa的压力压制成型为坯体；
所述坯体的直径为10mm，厚度为1mm；
(5)将坯体于1250℃～1270℃烧结，保温4小时，制成MLCC用高介电常数的介质陶瓷材料。
通过HEWLETT PACKARD 4278A测试所得制品的介电性能。
具体实施例的主要工艺参数及其介电性能详见表1。
表1
Claims (6)
1.一种MLCC用高介电常数陶瓷材料，其化学式为：Ba(Zr0.2Ti0.8)O3+xmol％Nb2O5，其中外加的Nb2O5为x＝0.05～0.6mol％。
该MLCC用高介电常数陶瓷材料的制备方法，具体步骤如下：
(1)将BaCO3、TiO2、ZrO2按化学计量式Ba(Zr0.2Ti0.8)O3进行配料，将原料放入聚酯罐中，加入去离子水和氧化锆球后，球磨4～8小时；
(2)将步骤(1)球磨后的原料放入干燥箱中，于100～120℃烘干，然后过40目筛；
(3)将步骤(2)过筛后的原料放入中温炉中，于1000～1200℃预烧，保温2～6小时；
(4)将步骤(3)预烧后的原料与外加的0.05～0.6mol％Nb2O5进行混合，放入球磨罐中，加入氧化锆球和去离子水，球磨10～14小时，烘干后过筛，再用粉末压片机压制成型为坯体；
(5)将步骤(4)的坯体于1250℃～1270℃烧结，保温2～6小时，制成MLCC用高介电常数陶瓷材料。
2.根据权利要求1所述的一种MLCC用高介电常数陶瓷材料，其特征在于，所述步骤(1)、步骤(4)球磨工艺的原料与去离子水和氧化锆球的质量比为1︰1︰1。
3.根据权利要求1所述的一种MLCC用高介电常数陶瓷材料，其特征在于，所述步骤(4)的坯体直径为10mm，厚度为1mm。
4.根据权利要求1所述的一种MLCC用高介电常数陶瓷材料，其特征在于，所述步骤(4)的坯体成型压力为2～8Mpa。
5.根据权利要求1所述的一种MLCC用高介电常数陶瓷材料，其特征在于，所述步骤(5)的烧结温度为1270℃。
6.根据权利要求1所述的一种MLCC用高介电常数陶瓷材料，其特征在于，所述步骤(4)外加Nb2O5的掺杂比例为0.2mol％。
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| CN106927821A (zh) * | 2017-04-12 | 2017-07-07 | 湖南云平环保科技有限公司 | 高介电常数陶瓷电容器材料及其制造方法 |
| CN106966721A (zh) * | 2017-04-26 | 2017-07-21 | 天津大学 | 一种具有高介电常数的锆钛酸钡陶瓷材料及其制备方法 |
| CN108610042A (zh) * | 2018-04-27 | 2018-10-02 | 天津大学 | 具有巨介电常数高绝缘特性的介质材料及其制备方法 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106927821A (zh) * | 2017-04-12 | 2017-07-07 | 湖南云平环保科技有限公司 | 高介电常数陶瓷电容器材料及其制造方法 |
| CN106966721A (zh) * | 2017-04-26 | 2017-07-21 | 天津大学 | 一种具有高介电常数的锆钛酸钡陶瓷材料及其制备方法 |
| CN108610042A (zh) * | 2018-04-27 | 2018-10-02 | 天津大学 | 具有巨介电常数高绝缘特性的介质材料及其制备方法 |
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Application publication date: 20170104 |