CN107840654A - 一种用于陶瓷电容器的介质材料及其制备方法 - Google Patents
一种用于陶瓷电容器的介质材料及其制备方法 Download PDFInfo
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- CN107840654A CN107840654A CN201710955223.7A CN201710955223A CN107840654A CN 107840654 A CN107840654 A CN 107840654A CN 201710955223 A CN201710955223 A CN 201710955223A CN 107840654 A CN107840654 A CN 107840654A
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- raw material
- dielectric
- barium titanate
- ceramic capacitor
- dielectric material
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 45
- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 143
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 36
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 16
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 3
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 3
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract description 3
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 3
- 229910052772 Samarium Inorganic materials 0.000 claims abstract description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 3
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 3
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 3
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 3
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 3
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 3
- 239000006185 dispersion Substances 0.000 claims description 40
- 239000000463 material Substances 0.000 claims description 32
- 238000001354 calcination Methods 0.000 claims description 31
- 238000002156 mixing Methods 0.000 claims description 29
- 238000012545 processing Methods 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 26
- 238000001035 drying Methods 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 5
- QDOXWKRWXJOMAK-UHFFFAOYSA-N dichromium trioxide Chemical compound O=[Cr]O[Cr]=O QDOXWKRWXJOMAK-UHFFFAOYSA-N 0.000 claims description 5
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 3
- 229910052681 coesite Inorganic materials 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 229910052906 cristobalite Inorganic materials 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229910052682 stishovite Inorganic materials 0.000 claims description 3
- 229910052905 tridymite Inorganic materials 0.000 claims description 3
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 2
- 239000002904 solvent Substances 0.000 description 11
- 239000010410 layer Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 239000002002 slurry Substances 0.000 description 6
- 238000005245 sintering Methods 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 4
- 239000004576 sand Substances 0.000 description 4
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 230000000996 additive effect Effects 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 description 3
- 238000003475 lamination Methods 0.000 description 3
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Inorganic materials O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 229910000990 Ni alloy Inorganic materials 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 238000005266 casting Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910019714 Nb2O3 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical group [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000005338 frosted glass Substances 0.000 description 1
- CMIHHWBVHJVIGI-UHFFFAOYSA-N gadolinium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Gd+3].[Gd+3] CMIHHWBVHJVIGI-UHFFFAOYSA-N 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- JYTUFVYWTIKZGR-UHFFFAOYSA-N holmium oxide Inorganic materials [O][Ho]O[Ho][O] JYTUFVYWTIKZGR-UHFFFAOYSA-N 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 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
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明提供的一种用于陶瓷电容器的介质材料及其制备方法，该介质材料包括：98‑105摩尔份的钛酸钡、0.5‑2.5摩尔份的原料A、0.2‑0.8摩尔份的原料B、0.1‑0.5摩尔份的原料C、0.2‑0.8摩尔份的原料D和0.2‑1.0摩尔份的原料E，其中A为选自Ho、Yb、Gd、Dy、Sm和Y中的至少一种元素的氧化物，B为选自W、Mo、V中的至少一种元素的氧化物，C为选自Mn、Cr、Co中的至少一种元素的氧化物，D为选自Mg、Ca、Ba中的至少一种元素的碳酸盐，E为选自Si、Li、Al和B中的至少一种元素的氧化物。该制备方法采用原料与钛酸钡分次加入的方式，能够使原料均匀分布于钛酸钡的表面。本发明的用于陶瓷电容器的介质材料及其制备方法，该介质材料的颗粒尺寸小，制作的MLCC具有高可靠性。
Description
技术领域
本发明涉及电容材料，更具体地，涉及一种用于陶瓷电容器的介质材料及其制备方法。
背景技术
多层片式陶瓷电容器(Multilayer Ceramic Capacitors)简称MLCC，是由印好电极的陶瓷介质膜片以错位的方式叠合起来，经过高温烧结形成陶瓷芯片，再在陶瓷芯片的两端封上金属层而形成。其具有高比容、高可靠性、高耐压、频率特性好等特点，是在电子信息、计算机、自动控制及通讯等领域应用十分广泛的电子器件。
随着电子设备及元器件向微型、薄层、混合集成等方向发展以及集成电路表面安装技术的迅速发展，对高性能MLCC的需求与日俱增。MLCC的介质单层厚度不断薄层化，要求即使薄层化也可以维持电容器的可靠性；特别是在介质层厚度小于2μm甚至小于0.5μm的超薄的MLCC，要求电容器非常高的可靠性，这对用于制备电容器的介质材料提出了更高的要求。
例如，公开号为CN101781115A的中国专利申请，其公开了一种X8R型多层陶瓷电容器介质材料及制备方法。该介质材料的主成分为钛酸钡，其摩尔含量为92％～96％；由Nb2O3与Co3O4组成的固溶物、R1的氧化物、R2的氧化物和Bi2O3组成的添加剂，其摩尔含量为4％～8％；R1和R2均为稀土族元素。
该介质材料的温度稳定性好、介电常数较高，并且，具有较好的可靠性。但是，由于介质材料的尺寸较大，难以满足陶瓷电容器的薄层化、大容量的需求。
发明内容
本发明提供一种克服上述问题或者至少部分地解决上述问题的用于陶瓷电容器的介质材料及其制备方法，以解决介质材料颗粒尺寸大、难以满足制作薄层化和高可靠性MLCC的技术问题。
根据本发明的一个方面，提供一种用于陶瓷电容器的介质材料，其包括钛酸钡及原料A、B、C、D和E。
其中，原料A为Ho、Yb、Gd、Dy、Sm和Y中的至少一种元素的氧化物；原料B为W、Mo和V中的至少一种元素的氧化物；原料C为Mn、Cr和Co中的至少一种元素的氧化物；原料D为Mg、Ca和Ba中的至少一种元素的碳酸盐；原料E为Si、Li、AL和B中的至少一种元素的氧化物。
在另一个具体的实施例中，所述介质材料中各组分的摩尔份含量如下：98-105份的钛酸钡、0.5-2.5份的原料A、0.2-0.8份的原料B、0.1-0.5份的原料C、0.2-0.8份的原料D和0.2-1.0份的原料E。
可以优选为：优选100份的钛酸钡、1-1.5份的原料A、0.3-0.6份的原料B、0.2-0.3份的原料C、0.5-0.7份的原料D和0.5-0.8份的原料E。
具体地，介质材料包含上述比例的各组分，既能实现介质材料良好的介电性能，又能够有效的抑制颗粒的生长。
原料A含量过少，抗还原性和寿命特性差；含量过多，烧结性能恶化，介电常数低。原料C含量过少，不能得到充分的效果；含量过多，不利于容量温度特性。原料B和D的含量保持在合适的范围，能够有效的提高材料的耐压性和容量温度特性，避免出现绝缘电阻导电性能不良或介电常数过低的问题。原料E为烧结助剂，其含量过少，烧结特性恶化，不利于绝缘电阻；含量过多，造成过烧，会引起介电常数的下降。
在另一个具体的实施例中，原料A为Ho2O3、Yb2O3、Gd2O3、Dy2O3、Sm2O3和Y2O3中的一种或多种；优选为Dy2O3和/或Y2O3。具体地，Y2O3为两性添加剂，可以平衡A位和B位的比例。而Dy2O3的抗还原性效果显著。
在另一个具体的实施例中，原料B为WO3、MoO3和V2O5中的一种或多种；优选为V2O5。
在另一个具体的实施例中，原料C为Mn3O4、Cr2O3和Co2O3中的一种或多种；优选为Mn3O4和/或Cr2O3。
在另一个具体的实施例中，原料D为MgCO3、CaCO3和BaCO3中的一种或多种；优选为MgCO3和CaCO3。
在另一个具体的实施例中，原料E为SiO2、Li2O、Al2O3和B2O3中的一种或几种；优选为SiO2和/或Al2O3。
在另一个具体的实施例中，以水热法制备的钛酸钡，其颗粒尺寸较小，通常在20-80nm。颗粒尺寸小、且粒径均匀的钛酸钡能够有利于减小介质材料的颗粒尺寸、提高介质材料的颗粒均匀性。
在另一个具体的实施例中，钛酸钡的颗粒尺寸优选为40-60nm。
根据本发明的另一个方面，还提供一种陶瓷电容器介质材料的制备方法，包括：
步骤S1、基于所述陶瓷电容器的规格要求，将原料A、原料B、原料C、原料D与钛酸钡分次湿式分散混合后，得到分散体系；
步骤S2、所述分散体系干燥处理后进行煅烧处理得到煅烧料，所述煅烧料与原料E混合后，再依次经湿式分散和干燥处理后得到所述介质材料。
具体地，对原料A、原料B、原料C、原料D和钛酸钡分次混合的方式可以有多种。
具体地，可以将对原料A、原料B、原料C、原料D和钛酸钡这五类物质，按照不同的混合次序混合，并采用湿式分散处理，使这五类物质充分混合均匀，得到分散体系。
具体地，对该分散体系进行干燥处理后，将所得的干料进行煅烧。煅烧后得到的煅烧料与原料E湿式分散混合，再经干燥处理，即得到介质材料。煅烧料与原料E采用湿式分散处理，以混合均匀，能够使原料E均匀的分布于煅烧料的外周，使所得的介质材料在后续制作陶瓷电容器时，不仅能够改善其烧结性能，还能够避免因原料E在局部区域的富集，从而提高介质材料以及陶瓷电容器的可靠性。
在另一个具体的实施例中，步骤S1中所述分次湿式分散混合具体包括：
步骤S11、将所述原料A、原料B、原料C、原料D与钛酸钡中的任意两类或两类以上的物质湿式分散混合后，经干燥、煅烧处理得到第一混合物；
步骤S12、所述原料A、原料B、原料C、原料D和钛酸钡中与所述第一混合物不同种类的物质中的一类或多类物质再与所述第一混合物湿式分散混合后，经干燥、煅烧处理，得到第二混合物；直至原料A、原料B、原料C、原料D和钛酸钡均混合均匀，得到所述分散体系。
具体地，可以先将原料A、原料B、原料C、原料D和钛酸钡中的任意一类、两类、三类物质或四类湿式分散混合，经干燥、煅烧处理后，再依次加入添加剂中剩余的其他四类、三类、两类或一类物质，继续湿式分散处理，并干燥、煅烧处理。
例如，先将原料A和原料B湿式分散混合，并经干燥、煅烧处理后得到第一混合物；第一混合物再与原料C湿式分散混合，经干燥、煅烧处理后，得到第二混合物；第二混合物再与原料D和钛酸钡湿式分散混合，得到分散体系。
再例如，先将原料A、原料B和原料D湿式分散混合，并经干燥、煅烧处理后得到第一混合物；第一混合物再与原料C湿式分散混合，经干燥、煅烧处理后，得到第二混合物；第二混合物再与钛酸钡湿式分散混合，得到分散体系。
再例如，先将原料D和钛酸钡湿式分散混合，并经干燥、煅烧处理后得到第一混合物；第一混合物再与原料B和原料C湿式分散混合，经干燥、煅烧处理后，得到第二混合物；第二混合物再与原料A湿式分散混合，得到分散体系。
按照上述方式进行混合，混合方式不一一列举，原料A、原料B、原料C、原料D和钛酸钡湿式分散的顺序不同，可根据介质材料所要求的性能选择不同的分散顺序。
上述过程中所涉及的湿式分散处理，其所选用的溶剂可以为水或乙醇。即将所需混合的物质混合后，加入溶剂，所得混合物由砂磨机研磨混合。具体地，砂磨机中可采用锆球为研磨介质，锆球直径可根据具体的研磨要求选取，例如采用0.1mm的锆球。具体地，湿式分散处理的时间可以根据实际情况调整。
具体地，对原料A、原料B、原料C、原料D和钛酸钡进行湿式分散处理后得到分散体系，由于该分散体系为浆料，再对该分散体系进行干燥处理。干燥处理采用离心式喷雾干燥机，对分散体系进行干燥时，既能够达到干燥的目的，又不会影响分散体系的物料分布状态。
在另一个具体的实施例中，所述钛酸钡采用水热法制备；所述煅烧处理的温度为600-900℃，优选为650-850℃。
具体地，以水热法制备的钛酸钡，其颗粒尺寸较小，通常在20-80nm。并且，颗粒尺寸较均匀，便于使介质材料的颗粒尺寸保持在较小的范围。具体地，采用上述方法制备的介质材料，其颗粒尺寸可以保持在100-200nm。
具体地，干料进行煅烧时，其煅烧处理温度为600-900℃。温度过低，物料煅烧不充分，均匀性差，影响其可靠性；温度过高，颗粒大，不利于薄层化，且介电常数低。
具体地，将所获得的介质材料按照比例与粘合剂、溶剂等混合，然后经过分散制成浆料，把浆料通过流延机制成介质生坯膜片，通过丝印机在膜片表面上印刷镍或镍合金电极，再根据设计层数，叠层膜片和印刷内电极；交替叠层印刷内电极的介质薄膜，形成叠层片；再经过等静压、切割形成生坯，将生坯在还原气氛中烧结，形成陶瓷体，经过倒角后在陶瓷体两端封上Cu或Cu合金的外部电极，在保护性气氛中烧结，最终获得多层陶瓷电容器MLCC。
本发明的有益效果主要如下：
(1)原料均匀包覆于钛酸钡的表面，能够有效的抑制煅烧过程中晶粒的长大，从而控制介质材料的尺寸保持在较小的范围，同时，还能够避免原料在局部区域的富集，提高介质材料的可靠性；
(2)所添加的原料能够有效的提高介质材料的耐压性能，改善所制作陶瓷电容器的绝缘电阻性能，提高其使用寿命。
具体实施方式
下面结合实施例，对本发明的具体实施方式作进一步详细描述。以下实施例用于说明本发明，但不用来限制本发明的范围。
采用本发明的制备方法，制备得到的介质材料，用于制作陶瓷电容器。可以理解的是，根据实验或生产规模，可以适当的整体调整本发明中物质的相对用量及处理时间，以使其满足实验或生产的需求。
实施例1-60中的介质材料采用如下方法制备。将原料A、原料B、原料C和原料D混合后，溶于溶剂中，采用砂磨机进行研磨1h；所得混合物再与100摩尔份的钛酸钡混合，并加入同样的溶剂进行湿式分散处理，所得分散体系采用离心式喷雾干燥机干燥1-2h；得到的干料在一定温度下煅烧2h。煅烧后所得的煅烧料再与原料E混合，并加入溶剂，在砂磨机中研磨以分散混合。此时分散混合得到的浆料再采用离心式喷雾干燥机干燥处理，所得的粉体即为介质材料。具体，每一个实施例中所用的溶剂为同一物质。具体地，制备介质材料时，原料A、原料B、原料C和原料D选用的具体物质参见表1-表3。
介质材料制备好后，将所获得的介质材料按照比例与粘合剂、溶剂等混合，然后经过分散制成浆料，把浆料通过流延机制成介质生坯膜片，通过丝印机在膜片表面上印刷镍或镍合金电极，再根据设计层数，叠层膜片和印刷内电极；交替叠层印刷内电极的介质薄膜，形成叠层片；再经过等静压、切割形成生坯，将生坯在还原气氛中烧结，形成陶瓷体，经过倒角后在陶瓷体两端封上Cu或Cu合金的外部电极，在保护性气氛中烧结，最终获得多层陶瓷电容器MLCC。
采用上述方法制备的陶瓷电容器的高温加速寿命采用如下方法检测：在150℃下，对电容器样品施加20KV/mm直流电压，测定寿命时间，由此评价高温加速寿命可靠性(HALT)。本发明的实施例中，从施加开始到绝缘电阻降低106以下的时间定义为寿命。具体参数参见表1-表3。
表1实施例1-20的主要参数对照表
表2实施例21-40的主要参数对照表
表3实施例41-60的主要参数对照表
实施例61
采用与实施例3相同的组成、溶剂、物料煅烧温度，并采用相同的检测方法进行检测，其区别仅在于：原料A采用Yb2O3。
所制作的陶瓷电容器，其介质厚度为1.2μm，HALT为24h。
实施例62
采用与实施例3相同的组成、溶剂、物料煅烧温度，并采用相同的检测方法进行检测，其区别仅在于：原料B采用MoO3。
所制作的陶瓷电容器，其介质厚度为1.2μm，HALT为23h。
实施例63
采用与实施例3相同的组成、溶剂、物料煅烧温度，并采用相同的检测方法进行检测，其区别仅在于：原料A、原料B、原料C、原料D与钛酸钡的混合方式不一样。
具体地，先将原料A、原料B和原料C采用湿式分散的方法混合均匀，该混合均匀后的物料与钛酸钡湿式分散混合，混合均匀后，再与原料D采用湿式分散混合。
由该方式混合而制备的介质材料制作的陶瓷电容器，其介质厚度为1.2μm，HALT为24h。
最后，本发明的方法仅为较佳的实施方案，并非用于限定本发明的保护范围。凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。
Claims (8)
1.一种用于陶瓷电容器的介质材料，其特征在于，所述介质材料包含如下摩尔份含量的组分：98-105份的钛酸钡、0.5-2.5份的原料A、0.2-0.8份的原料B、0.1-0.5份的原料C、0.2-0.8份的原料D和0.2-1.0份的原料E；
其中，原料A为Ho、Yb、Gd、Dy、Sm和Y中的至少一种元素的氧化物；
原料B为W、Mo和V中的至少一种元素的氧化物；
原料C为Mn、Cr和Co中的至少一种元素的氧化物；
原料D为Mg、Ca和Ba中的至少一种元素的碳酸盐；
原料E为Si、Li、AL和B中的至少一种元素的氧化物。
2.如权利要求1所述的一种用于陶瓷电容器的介质材料，其特征在于，所述介质材料包含如下摩尔份含量的组分：优选100份的钛酸钡、1-1.5份的原料A、0.3-0.6份的原料B、0.2-0.3份的原料C、0.5-0.7份的原料D和0.5-0.8份的原料E。
3.如权利要求1或2所述的一种用于陶瓷电容器的介质材料，其特征在于，所述原料A优选为Dy2O3和/或Y2O3；
所述原料B优选为V2O5；
所述原料C优选为Mn3O4和/或Cr2O3；
所述原料D优选为MgCO3和CaCO3；
所述原料E优选为SiO2和/或Al2O3。
4.如权利要求1-3任一项所述的一种用于陶瓷电容器的介质材料，其特征在于，BaTiO3采用水热法生产，BaTiO3的颗粒尺寸为20-80nm。
5.如权利要求4所述的一种用于陶瓷电容器的介质材料，其特征在于，BaTiO3的颗粒尺寸优选为40-60nm。
6.如权利要求1-5任一项所述介质材料的制备方法，其特征在于，包括：
步骤S1、基于所述陶瓷电容器的规格要求，将所述原料A、原料B、原料C、原料D与钛酸钡分次湿式分散混合后，得到分散体系；
步骤S2、所述分散体系干燥处理后进行煅烧处理得到煅烧料，所述煅烧料与所述原料E混合后，再依次经湿式分散和干燥处理后得到所述介质材料。
7.如权利要求6所述的制备方法，其特征在于，步骤S1中所述分次湿式分散混合具体包括：
步骤S11、将所述原料A、原料B、原料C、原料D与钛酸钡中的任意两类或两类以上的物质湿式分散混合后，经干燥、煅烧处理得到第一混合物；
步骤S12、所述原料A、原料B、原料C、原料D和钛酸钡中与所述第一混合物不同种类的物质中的一类或多类物质再与所述第一混合物湿式分散混合后，经干燥、煅烧处理，得到第二混合物；直至原料A、原料B、原料C、原料D和钛酸钡均混合均匀，得到所述分散体系。
8.如权利要求6或7所述的制备方法，其特征在于：所述煅烧处理的温度为600-900℃，优选为650-850℃。
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