CN114685161A - 一种x8r型陶瓷电容器电介质材料及其制备方法 - Google Patents
一种x8r型陶瓷电容器电介质材料及其制备方法 Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 42
- 239000003989 dielectric material Substances 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 32
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 31
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims abstract description 28
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 claims abstract description 28
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 27
- 230000000996 additive effect Effects 0.000 claims abstract description 18
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 18
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 18
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 15
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 15
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 15
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 15
- 229910002976 CaZrO3 Inorganic materials 0.000 claims abstract description 6
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 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 4
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 claims abstract description 4
- FKTOIHSPIPYAPE-UHFFFAOYSA-N samarium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Sm+3].[Sm+3] FKTOIHSPIPYAPE-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000000498 ball milling Methods 0.000 claims description 54
- 238000001035 drying Methods 0.000 claims description 25
- 239000002245 particle Substances 0.000 claims description 24
- 238000007873 sieving Methods 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 19
- 238000005303 weighing Methods 0.000 claims description 19
- 238000005245 sintering Methods 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 12
- 238000001354 calcination Methods 0.000 claims description 11
- 238000000227 grinding Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- 238000003825 pressing Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 239000000919 ceramic Substances 0.000 claims description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 239000011812 mixed powder Substances 0.000 claims description 4
- 238000000465 moulding Methods 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 230000015556 catabolic process Effects 0.000 claims description 3
- 238000000713 high-energy ball milling Methods 0.000 claims description 3
- 238000009413 insulation Methods 0.000 claims description 3
- 238000003801 milling Methods 0.000 claims description 2
- 239000007790 solid phase Substances 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 claims 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 14
- 229910001928 zirconium oxide Inorganic materials 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 8
- 238000009740 moulding (composite fabrication) Methods 0.000 description 7
- 238000009472 formulation Methods 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000010953 base metal Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 229910003237 Na0.5Bi0.5TiO3 Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Abstract
本发明涉及一种X8R型陶瓷电容器电介质材料及其制备方法。所述X8R型陶瓷电容器电介质材料组成为BaTiO3+Re2O3+MeO+BaSiO3+添加剂;其中,所述主料为BaTiO3;所述Re2O3为Y2O3、Sm2O3、La2O3、Yb2O3中的至少一种,所述MeO为MgO、CaO、BaO、ZnO中的至少一种,所述添加剂为MnCO3、MoO3、ZrO2、BaCO3、WO3、CaZrO3、SiO2中的至少一种。
Description
技术领域
本发明属于电子元器件的陶瓷材料领域,特别涉及一种高介电常数X8R型陶瓷电容器电介质材料。
背景技术
多层陶瓷电容器由于其独特的电学性能被广泛地应用于个人计算机(PC),移动电话,汽车电子设备、航天航空电子设备等多种电子设备中。随着科技的进步和发展,大量多层陶瓷电容器需要在高温、高压等严苛的工作环境中保持高可靠性。例如,近年来,新能源汽车的不断发展,汽车电子设备例如电子发动机控制单元(ECU),防抱死制动系统(ABS),编程燃料喷射系统(PGM FI)等,需要高温下运行,其工作温度可高达150℃。因此,具有宽温度稳定性的多层陶瓷电容器的需求量将持续增长,这将促使研发具有X8R温度特性(-55~+150℃,|ΔC/C25℃|≤±15%)的介电材料成为当前的迫切需求。
目前,国内外涉及X8R陶瓷电容器电介质材料的专利比较多。大部分X8R电介质材料主要成分为BaTiO3,通过掺杂改性等方式改善其温度特性。许多专利报道了在BaTiO3中添加含Bi、B、Na、Li等易挥发元素的氧化物以及稀土氧化物、玻璃粉等来使材料达到X8R温度特性。例如BaTiO3-Na0.5Bi0.5TiO3体系,在CN108083795A、CN106348748A、CN102992756B等专利中均有报道,当该材料体系高温烧结时,Bi易挥发,易对环境造成污染,且只可以于空气中烧结,需与Ag、Ag-Pd贵金属电极共烧,使成本升高,若在氮气中烧结,B会析出,从而影响多层陶瓷电容器性能。部分专利通过严格控制晶粒大小,并掺杂Ca、Zr等元素,来达到X8R温度特性,但其介电常数偏低,如CN103534223A。此外,近年来关于非还原性X8R型电容器电介质材料的研究越来越多,如专利CN101589004A中BaTiO3-MgO-稀土氧化物体系等材料,该材料介电常数较高、介电损耗较低,可与Ni等贱金属电极共烧,降低了生产成本,但绝缘电阻偏低。
发明内容
为解决上述问题,本发明提供了一种具有可规模化生产、具有高介电常数、宽温度稳定的X8R型陶瓷电介质材料及其制备方法。
第一方面,本发明提供了一种X8R型陶瓷电容器电介质材料,所述X8R型陶瓷电容器电介质材料组成为BaTiO3+Re2O3+MeO+BaSiO3+添加剂;其中,所述主料为BaTiO3;所述Re2O3为Y2O3、Sm2O3、La2O3、Yb2O3中的至少一种,所述MeO为MgO、CaO、BaO、ZnO中的至少一种,所述添加剂为MnCO3、MoO3、ZrO2、BaCO3、WO3、CaZrO3、SiO2、中的至少一种;以100重量份的所述主料的BaTiO3为基础,各成分和相对含量如下:主料BaTiO3为100份;Re2O3为0.35~5份;MeO为0.2~4份;BaSiO3为0.45~4份;添加剂总量为0.2~6份,每种添加剂为0.004~5份。
本发明所述X8R型陶瓷电介质材料组成为BaTiO3+Re2O3+MeO+BaSiO3+添加剂,加入Re2O3,可以使室温下介电常数提高并;若含量过低,会导致介电常数偏低;若含量过高,会影响温度稳定性。加入MeO,可以使展宽居里峰;若含量过低,会导致展宽效果不够,无法到达X8R标准;若含量过高,会导致居里峰向低温方向偏移过大。加入添加剂,可以使烧结温度降低并改善介电性能;若含量过低或过高,都会影响其温度稳定性。
较佳的,所述Re2O3为Y2O3,所述MeO为MgO,所述添加剂为MnCO3、MoO3、ZrO2、BaCO3。
较佳的,所述陶瓷电容器电介质材料在室温下的介电常数为1500~2200,室温下损耗因子≦0.02,直流击穿电压≧10kV/mm,绝缘电阻率为≧1010Ω·cm,-55℃容温变化率为-12~-3%,125℃容温变化率为0.5~6%,150℃容温变化率为-4~-15%,满足X8R温度特性。
较佳的,所述介质材料为粉末状,粒径为0.3~1.5微米,粒径过低或过高都影响其温度稳定性。
较佳的,所述主料BaTiO3的粒径为0.3~1微米。
较佳的,所述Re2O3、MeO、BaSiO3和添加剂的粒径为0.05~0.5微米。
较佳的,按照1:1摩尔比称取BaCO3与SiO2,球磨5~8小时后,70~90℃烘干,研磨后过60目筛网,在1000~1100℃下煅烧1~3h,冷却后,砂磨1~3h,干燥、过60目筛网,得到所述BaSiO3。
第二方面,本发明提供了上述陶瓷电容器电介质材料的制备方法。所述制备方法包括:主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂经第一次球磨混合均匀,得到粒径为0.3~1.5微米的混合粉体;将上述混合粉体干燥后进行固相合成,固相合成温度可为1050~1150℃,保温时间可为1~4小时;将固相合成的陶瓷粉料二次球磨后,压制成型,进一步烧结,得到X8R型陶瓷电容电介质材料。
较佳的,所述第一次球磨为湿法球磨,球磨的磨球可采用氧化锆球,球磨介质可采用无水乙醇,球磨时间可为6~8小时。
较佳的,所述第二次球磨为高能球磨,球磨转速1800~2200r/min,时间20~40min,优选球磨转速2000r/min,时间30min。
较佳的,所述烧结的温度可为1260~1350℃,保温时间可为4~6小时。
有益效果:
本发明制备的陶瓷电容器电介质材料粒度分布均匀、分散性好、并且具有高介电常数(1500~2200)、低损耗(≤2%)、温度特性满足X8R要求,直流击穿电压≧10kV/mm,成本较低、生产工艺简单,易于控制,稳定性好,不含Bi、B、K、Na等易挥发元素,可与Ni等贱金属电极共烧,介质粉体粒径最小可达到0.3微米,有利于制备小型化、高电容量的多层陶瓷电容器。
附图说明
图1显示出实施例1所制备的高介电常数X8R型陶瓷电容器电介质材料的XRD照片;从图中可以看出实施例1中电介质陶瓷材料为单一的钙钛矿相,无其他杂相。
图2显示出实施例1所制备的高介电常数X8R型陶瓷电容器电介质材料的低温介电性能图谱;从图中可以看出实施例1中电介质陶瓷材料室温下介电常数大于2000。
图3显示出实施例1所制备的高介电常数X8R型陶瓷电容器电介质材料的容温变化率图谱;从图中可以看出实施例1中电介质陶瓷材料满足X8R温度特性。
具体实施方式
以下结合附图和下述实施方式进一步说明本发明,应理解,下述实施方式仅用于说明本发明,而非限制本发明。
本发明以BaTiO3+Re2O3+MeO+BaSiO3+添加剂作为原料,通过固相法制备高介电常数X8R型陶瓷电容器电介质材料。其中,所述主料为BaTiO3。所述Re2O3为Y2O3、Sm2O3、La2O3、Yb2O3中的一种或多种。所述MeO为MgO、CaO、BaO、ZnO中的一种或多种。所述添加剂为MnCO3、MoO3、ZrO2、BaCO3、WO3、CaZrO3、SiO2中的一种或多种。以100重量份的所述主料的BaTiO3为基础,各成分和相对含量如下:主料BaTiO3为100份;Re2O3为0.35~5份;MeO为0.2~4份;BaSiO3为0.45~4份;添加剂总量为0.2~6份,每种添加剂为0.004~5份。
所述介质材料为粉末状,粒径为0.3~1.5微米。
所述主料BaTiO3的粒径为0.3~1微米。
所述Re2O3、MeO、BaSiO3和添加剂的粒径为0.05~0.5微米。
所述BaSiO3按照1:1摩尔比称取BaCO3与SiO2,球磨5~8小时后,70~90℃烘干,研磨后过60目筛网,在1000~1100℃下煅烧1~3h,冷却后,砂磨1~3h,干燥、过60目筛网,装袋备用。
主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂可采用湿法球磨(一次球磨)混合均匀。
一次球磨的磨球可采用氧化锆球,球磨介质可采用无水乙醇,球磨时间可为6~8小时。
经一次球磨的粉体干燥后进行固相合成,固相合成温度可为1050~1150℃,保温时间可为1~4小时。
合成的陶瓷粉料经二次球磨,第二次球磨为高能球磨,球磨转速2000r/min,时间30min。
将二次球磨后的陶瓷粉料压制成型,进一步烧结即可得到高耐压X8R型陶瓷电容器电介质材料,烧结温度可为1260~1350℃,保温时间可为4~6小时。
下面进一步例举实施例以详细说明本发明。同样应理解,以下实施例只用于对本发明进行进一步说明,不能理解为对本发明保护范围的限制,本领域的技术人员根据本发明的上述内容作出的一些非本质的改进和调整均属于本发明的保护范围。下述示例具体的工艺参数等也仅是合适范围中的一个示例,即本领域技术人员可以通过本文的说明做合适的范围内选择,而并非要限定于下文示例的具体数值。
实施例1
按重量份称取BaCO3 197.54份与SiO2 60.14份,球磨6时后,80℃烘干,研磨后过60目筛网,在1100℃下煅烧2h,冷却后,砂磨1h,干燥、过60目筛网,得到BaSiO3,装袋备用。
按重量份称取BaTiO3为100份;Y2O3为2.48份;MgO为0.47份;MnCO3为0.06份;MoO3为0.03份;ZrO2为0.9份;BaCO3为2.57份;BaSiO3为3.05份(500nm);其中BaTiO3粒径为0.5微米。
将主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂采用湿式球磨法混合6小时;在空气中升温至1100℃,保温2小时,二次球磨0.5小时,球磨转速2000r/min;压制成型,在1290℃中烧结6小时,自然冷却,得到X8R型陶瓷电容器电介质材料。
实施例2
按重量份称取BaCO3 197.54份与SiO2 60.14份,球磨6时后,80℃烘干,研磨后过60目筛网,在1100℃下煅烧2h,冷却后,砂磨1h干燥、过60目筛网,得到BaSiO3,装袋备用。
按重量份称取BaTiO3为100份;Y2O3为2.62份;MgO为0.5份;MnCO3为0.06份;MoO3为0.03份;ZrO2为0.95份;BaCO3为2.72份;BaSiO3为3.23份(500nm);其中BaTiO3粒径为0.5微米。
将主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂采用湿式球磨法混合6小时;在空气中升温至1100℃,保温2小时,二次球磨0.5小时,球磨转速2000r/min;压制成型,在1290℃中烧结6小时,自然冷却,得到X8R型陶瓷电容器电介质材料。
实施例3
按重量份称取BaCO3 197.54份与SiO2 60.14份,球磨6时后,80℃烘干,研磨后过60目筛网,在1100℃下煅烧2h,冷却后,砂磨1h,干燥、过60目筛网,得到BaSiO3,装袋备用。
按重量份称取BaTiO3为100份;Y2O3为2.77份;MgO为0.52份;MnCO3为0.07份;MoO3为0.04份;ZrO2为1.00份;BaCO3为2.88份;BaSiO3为3.40份(500nm);其中BaTiO3粒径为0.5微米。
将主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂采用湿式球磨法混合6小时;在空气中升温至1100℃,保温2小时,二次球磨0.5小时,球磨转速2000r/min;压制成型,在1290℃中烧结6小时,自然冷却,得到X8R型陶瓷电容器电介质材料。
实施例4
按重量份称取BaCO3 197.54份与SiO2 60.14份,球磨6时后,80℃烘干,研磨后过60目筛网,在1100℃下煅烧2h,冷却后,砂磨1h,干燥、过60目筛网,得到BaSiO3,装袋备用。
按重量份称取BaTiO3为100份;Y2O3为2.91份;MgO为0.55份;MnCO3为0.07份;MoO3为0.04份;ZrO2为1.05份;BaCO3为3.03份;BaSiO3为3.58份(500nm);其中BaTiO3粒径为0.5微米。
将主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂采用湿式球磨法混合6小时;在空气中升温至1100℃,保温2小时,二次球磨0.5小时,球磨转速2000r/min;压制成型,在1290℃中烧结6小时,自然冷却,得到X8R型陶瓷电容器电介质材料。
实施例5
按重量份称取BaCO3 197.54份与SiO2 60.14份,球磨6时后,80℃烘干,研磨后过60目筛网,在1100℃下煅烧2h,冷却后,砂磨1h,干燥、过60目筛网,得到BaSiO3,装袋备用。
按重量份称取BaTiO3为100份;Yb2O3为3.81份;MgO为0.47份;MnCO3为0.06份;MoO3为0.03份;ZrO2为0.9份;BaCO3为2.57份;BaSiO3为3.05份(500nm);其中BaTiO3粒径为0.5微米。
将主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂采用湿式球磨法混合6小时;在空气中升温至1100℃,保温2小时,二次球磨0.5小时,球磨转速2000r/min;压制成型,在1300℃中烧结6小时,自然冷却,得到X8R型陶瓷电容器电介质材料。
实施例6
按重量份称取BaCO3 197.54份与SiO2 60.14份,球磨6时后,80℃烘干,研磨后过60目筛网,在1100℃下煅烧2h,冷却后,砂磨1h,干燥、过60目筛网,得到BaSiO3,装袋备用。
按重量份称取BaTiO3为100份;Y2O3为2.48份;MgO为0.47份;MnCO3为0.06份;MoO3为0.03份;ZrO2为0.9份;BaCO3为2.57份;BaSiO3为3.05份(500nm);CaZrO3为2.30份;其中BaTiO3粒径为0.5微米。
将主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂采用湿式球磨法混合6小时;在空气中升温至1100℃,保温2小时,二次球磨0.5小时,球磨转速2000r/min;压制成型,在1300℃中烧结6小时,自然冷却,得到X8R型陶瓷电容器电介质材料。
实施例7
本实施例7中X8R型陶瓷电容器电介质材料和实施例1的制备过程一致,区别在于:其中BaTiO3粒径为1微米。
对比例1
按重量份称取BaCO3 197.54份与SiO2 60.14份,球磨6时后,80℃烘干,研磨后过60目筛网,在1100℃下煅烧2h,冷却后,砂磨1h,干燥、过60目筛网,得到BaSiO3,装袋备用。
按重量份称取BaTiO3为100份;Y2O3为2.48份;MgO为0.47份;MnCO3为0.06份;MoO3为0.03份;ZrO2为0.9份;BaCO3为2.57份;BaSiO3为3.05份(500nm),其中BaTiO3粒径为0.2微米。
将主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂采用湿式球磨法混合6小时;在空气中升温至1100℃,保温2小时,二次球磨0.5小时,球磨转速2000r/min;压制成型,在1280℃中烧结6小时,自然冷却,得到陶瓷电容器电介质材料。
对比例2
按重量份称取BaCO3 197.54份与SiO2 60.14份,球磨6时后,80℃烘干,研磨后过60目筛网,在1100℃下煅烧2h,冷却后,砂磨1h,干燥、过60目筛网,得到BaSiO3,装袋备用。
按重量份称取BaTiO3为100份;Y2O3为2.48份;MnCO3为0.06份;MoO3为0.03份;BaCO3为2.57份;BaSiO3为3.05份(500nm);其中BaTiO3粒径为0.5微米。
将主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂采用湿式球磨法混合6小时;在空气中升温至1100℃,保温2小时,二次球磨0.5小时,球磨转速2000r/min;压制成型,在1280℃中烧结6小时,自然冷却,得到陶瓷电容器电介质材料。
表1为实施例1~4、实施例7的配方:
BaTiO<sub>3</sub> | MnCO<sub>3</sub> | Y<sub>2</sub>O<sub>3</sub> | ZrO<sub>2</sub> | MgO | BaCO<sub>3</sub> | BaSiO<sub>3</sub> | MoO<sub>3</sub> | |
实施例1 | 100.00 | 0.06 | 2.48 | 0.90 | 0.47 | 2.57 | 3.05 | 0.03 |
实施例2 | 100.00 | 0.06 | 2.62 | 0.95 | 0.50 | 2.72 | 3.23 | 0.03 |
实施例3 | 100.00 | 0.07 | 2.77 | 1.00 | 0.52 | 2.88 | 3.40 | 0.04 |
实施例4 | 100.00 | 0.07 | 2.91 | 1.05 | 0.55 | 3.03 | 3.58 | 0.04 |
实施例7 | 100.00 | 0.06 | 2.48 | 0.90 | 0.47 | 2.57 | 3.05 | 0.03 |
表2为实施例5的配方:
BaTiO<sub>3</sub> | MnCO<sub>3</sub> | Yb<sub>2</sub>O<sub>3</sub> | ZrO<sub>2</sub> | MgO | BaCO<sub>3</sub> | BaSiO<sub>3</sub> | MoO<sub>3</sub> | |
实施例5 | 100.00 | 0.06 | 3.81 | 0.90 | 0.47 | 2.57 | 3.05 | 0.03 |
表3为实施例6的配方:
BaTiO<sub>3</sub> | MnCO<sub>3</sub> | Y<sub>2</sub>O<sub>3</sub> | ZrO<sub>2</sub> | MgO | BaCO<sub>3</sub> | BaSiO<sub>3</sub> | MoO<sub>3</sub> | CaZrO<sub>3</sub> | |
实施例6 | 100.00 | 0.06 | 2.48 | 0.90 | 0.47 | 2.57 | 3.05 | 0.03 | 2.30 |
表4为对比例1~2的配方:
BaTiO<sub>3</sub> | MnCO<sub>3</sub> | Y<sub>2</sub>O<sub>3</sub> | ZrO<sub>2</sub> | MgO | BaCO<sub>3</sub> | BaSiO<sub>3</sub> | MoO<sub>3</sub> | |
对比例1 | 100.00 | 0.06 | 2.48 | 0.90 | 0.47 | 2.57 | 3.05 | 0.03 |
对比例2 | 100.00 | 0.06 | 2.48 | 0.00 | 0.00 | 2.57 | 3.05 | 0.03 |
表5为实施例1~7与对比例1~2的相关性能测试结果:
实施例1与对比例1配方相同,实施例1中采用的BaTiO3粒径为0.5微米,而对比例1中BaTiO3粒径为0.2微米,相比之下,对比例1中介电常数低于实施例1,并且未达到X8R温度特性。与实施例1相比,对比例2中未加入MgO和ZrO2,该材料未达到X8R温度特性。
Claims (10)
1.一种X8R型陶瓷电容器电介质材料,其特征在于,所述X8R型陶瓷电容器电介质材料组成为BaTiO3+ Re2O3+MeO+BaSiO3+添加剂;
其中,所述主料为BaTiO3;所述Re2O3为Y2O3、Sm2O3、La2O3、Yb2O3中的至少一种,所述MeO为MgO、CaO、BaO、ZnO中的至少一种,所述添加剂为MnCO3、MoO3、ZrO2、BaCO3、WO3、CaZrO3、SiO2中的至少一种;
以100重量份的所述主料的BaTiO3为基础,各成分和相对含量如下:主料BaTiO3为100份; Re2O3为0.35~5份; MeO为0.2~4份;BaSiO3为0.45~4份;添加剂总量为0.2~6份,每种添加剂为0.004~5份。
2.根据权利要求1所述的X8R型陶瓷电容器电介质材料,其特征在于,所述Re2O3为Y2O3,所述MeO为MgO,所述添加剂为MnCO3、MoO3、ZrO2、BaCO3。
3.根据权利要求1或2所述的X8R型陶瓷电容器电介质材料,其特征在于,所述陶瓷电容器电介质材料在室温下的介电常数为1500~2200,室温下损耗因子≦0.02,直流击穿电压≧10kV/mm,绝缘电阻率为≧1010Ω•cm,-55℃容温变化率为-12~-3%,125℃容温变化率为0.5~6%,150℃容温变化率为-4~-15%,满足X8R温度特性。
4.根据权利要求1至3中任一项所述的X8R型陶瓷电容器电介质材料,其特征在于,所述主料BaTiO3的粒径为0.3~1微米。
5.根据权利要求1至4中任一项所述的X8R型陶瓷电容器电介质材料,其特征在于,所述Re2O3、MeO、BaSiO3和添加剂的粒径为0.05~0.5微米。
6.根据权利要求1至5中任一项所述的X8R型陶瓷电容器电介质材料,其特征在于,按照1:1摩尔比称取BaCO3与SiO2,球磨5~8小时后,70~90℃烘干,研磨后过60目筛网,在1000~1100℃下煅烧1~3h,冷却后,砂磨1~3h,干燥、过60目筛网,得到所述BaSiO3。
7.一种权利要求1至6中任一项所述的X8R型陶瓷电容器电介质材料的制备方法,其特征在于,所述制备方法包括:主料BaTiO3、Re2O3、MeO、BaSiO3、添加剂经第一次球磨混合均匀,得到粒径为0.3~1.5微米的混合粉体;将上述混合粉体干燥后进行固相合成,固相合成温度为1050~1150℃,保温时间为1~4小时;将固相合成的陶瓷粉料二次球磨后,压制成型,进一步烧结,得到X8R型陶瓷电容电介质材料。
8.根据权利要求7所述的制备方法,其特征在于,所述第一次球磨为湿法球磨,球磨的磨球采用氧化锆球,球磨介质采用无水乙醇,球磨时间为6~8小时。
9.根据权利要求7或8所述的制备方法,其特征在于,所述第二次球磨为高能球磨,球磨转速1800~2200r/min,时间20~40min。
10.根据权利要求7至9中任一项所述的制备方法,其特征在于,所述烧结的温度为1260~1350℃,保温时间为4~6小时。
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