CN113563066B - 一种介电常数大于12000的介电材料及制备方法 - Google Patents
一种介电常数大于12000的介电材料及制备方法 Download PDFInfo
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- DJOYTAUERRJRAT-UHFFFAOYSA-N 2-(n-methyl-4-nitroanilino)acetonitrile Chemical class N#CCN(C)C1=CC=C([N+]([O-])=O)C=C1 DJOYTAUERRJRAT-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229940071182 stannate Drugs 0.000 claims abstract description 60
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 59
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 54
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000006184 cosolvent Substances 0.000 claims abstract description 30
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims description 71
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 64
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 48
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 48
- 229910001868 water Inorganic materials 0.000 claims description 48
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 44
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 44
- 238000005245 sintering Methods 0.000 claims description 32
- 238000000034 method Methods 0.000 claims description 28
- 238000002156 mixing Methods 0.000 claims description 25
- 238000000498 ball milling Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 239000007790 solid phase Substances 0.000 claims description 24
- 239000004408 titanium dioxide Substances 0.000 claims description 24
- 229910044991 metal oxide Inorganic materials 0.000 claims description 22
- 150000004706 metal oxides Chemical group 0.000 claims description 22
- 239000011787 zinc oxide Substances 0.000 claims description 22
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 16
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims description 16
- 238000005303 weighing Methods 0.000 claims description 16
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 15
- 230000002194 synthesizing effect Effects 0.000 claims description 10
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 8
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 8
- 238000002309 gasification Methods 0.000 claims description 8
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 description 9
- 229920002451 polyvinyl alcohol Polymers 0.000 description 9
- 238000009775 high-speed stirring Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 239000004576 sand Substances 0.000 description 7
- 238000005469 granulation Methods 0.000 description 6
- 230000003179 granulation Effects 0.000 description 6
- 238000000227 grinding Methods 0.000 description 6
- 239000000919 ceramic Substances 0.000 description 3
- 239000003990 capacitor Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 150000001552 barium Chemical class 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
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Abstract
本发明公开一种介电常数大于12000的介电材料及制备方法,包括钛酸钡、改性锆酸钙、锡酸铋和助溶剂;所述钛酸钡、改性锆酸钙、锡酸铋之间的重量比为(0.8~0.9):(0.1~0.15):(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%。本发明的材料介电常数大于12000,抗电强度大于4.5KV(AC)/mm,温度系数同时还能满足现有2E4材料的要求。
Description
技术领域
本发明涉及复合材料及其制备方法技术领域,尤其涉及一种介电常数大于12000的介电材料及制备方法。
背景技术
随着电子技术的不断发展,小型化,高性能的要求不断的提高,对高介电常数、高稳定、高抗电强度的材料的要求越来越高。现有的Y5U和2E4 体系的材料已经不能满足要求,特别是不能适应贴片类安规电容的发展。现有的2E4材料介电常数一般只能做到9000~10000,抗电强度一般小于4.0KV(AC)/mm,已经不能达到很多高要求设计时的要求。所以市场急需要一种介电常数大于12000,且抗电强度大于4.5KV(AC)/mm,温度特性满足 2E4的材料。
发明内容
本发明针对上述现有技术的不足,提供了一种介电常数大于12000的介电材料,其具有介电常数大于12000,抗电强度大于4.5KV(AC)/mm,温度系数同时还能满足现有2E4材料的要求。
为解决现有技术中存在的问题,采用的具体技术方案是:
一种介电常数大于12000的介电材料包括钛酸钡、改性锆酸钙、锡酸铋和助溶剂;所述固相合成钛酸钡、改性锆酸钙、锡酸铋之间的重量比为 (0.8~0.9):(0.1~0.15):(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%;所述钛酸钡的结构式为:x(BaTiO3),其中,x取值范围为0.8~0.9;所述改性锆酸钙的结构式为:y(CaZruBi(1-u))O3, y取值范围为0.1~0.15,u的取值范围为0.92~0.98;所述锡酸铋的结构式为:zBiSnO3,其中,z的取值范围为0.01~0.05。
优选的技术方案,所述助溶剂为金属氧化物。
优选的技术方案,所述金属氧化物为二氧化锰、氧化锌或者二氧化锰与氧化锌的混合物。
优选的技术方案,所述金属氧化物为二氧化锰与氧化锌的混合物,二氧化锰与氧化锌的重量比为1:(3.6~4.8)。
本发明的再一目的是提供一种介电常数大于12000的介电材料制备方法,其包括以下步骤:
钛酸钡的制备:将粉末状的碳酸钡、二氧化钛按照摩尔比1:1称量配好;再将二氧化钛、碳酸钡以及水按重量比称重后加入球磨机,其中碳酸钡、二氧化钛的重量之和与水的重量比等于1:0.8;球磨两小时后,烘干混合物至水份少于6%;再在1280±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,即制得x(BaTiO3),其中,x取值范围为0.8~0.9;
改性锆酸钙的制备:
将电子级碳酸钙和纯度大于99.3%,粒度小于5um的二氧化锆及三氧化二铋和去离子水,按重量比(90-110):(110-130):(5-9):190的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1260±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的改性锆酸钙;
锡酸铋的制备:
将气化法生产的二氧化锡和三氧化二铋和去离子水,按重量比 (100-110):(110-130):180的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1000±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的锡酸铋;
将钛酸钡、改性锆酸钙、锡酸铋混合后加入助溶剂后即制得成品,其中,所述钛酸钡、改性锆酸钙、锡酸铋的重量比为(0.8~0.9):(0.1~0.15): (0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%。
优选的技术方案,在分别制备钛酸钡、改性锆酸钙、锡酸铋的过程中,所述球磨机球体的重量与加入的水的重量比为3:0.8。
优选的技术方案,所述助溶剂为金属氧化物。
优选的技术方案,所述助溶剂的金属氧化物为二氧化锰和氧化锌的混合物。
优选的技术方案,所述二氧化锰与氧化锌之间的重量比等于1:(3.6~4.8)。且将二氧化锰、氧化锌、钛酸钡、改性锆酸钙、锡酸铋的混合物在高速搅拌磨或者砂磨机中,将混合物的粒度打磨到2微米以下,加入2.6%的PVA在造粒塔中造粒。
优选的技术方案,所述烧结采用的是箱式炉或者隧道炉。
通过采用上述方案,本发明的一种介电常数大于12000的介电材料及其制备方法与现有技术相比,其技术效果在于:
1、本发明采用改性过的锆酸钙和锡酸铋加金属氧化物对钛酸钡基材料做改性,做成了介电常数大于12000,满足2E4温度变化,用于贴片安规电容的介质材料。
2、通过对钛酸钡基材料的改性,结合添加的金属氧化物二氧化锰和氧化锌等,有效的提高了瓷体的抗电强度,达到了击穿电压大于4.5KV(AC)/mm 的陶瓷材料。
3、本发明通过不同配比,分别在1280±15℃、1300±15℃、1000摄氏度对钛酸钡、锆酸钙、锡酸铋进行烧结和改性,使其介电系数达12000到 13000,温度特性满足2E4,抗电强度大于4.5KV(AC)/mm。
具体实施方式
为使本发明的目的、技术方案和优点更加清楚明了,下面结合具体实例,对本发明进一步详细说明。应该理解,这些描述只是示例性的,而并非要限制本发明的范围。此外,在以下说明中,省略了对公知结构和技术的描述,以避免不必要地混淆本发明的概念。
实施例1,本发明一种介电常数大于12000的介电材料,采用了以下方法制得:
一种介电常数大于12000的介电材料制备方法,其包括以下步骤:
钛酸钡的制备:将粉末状的碳酸钡、二氧化钛按照摩尔比1:1称量配好;再将二氧化钛、碳酸钡以及水按重量比称重后加入球磨机,其中碳酸钡、二氧化钛的重量之和与水的重量比等于1:0.8;球磨两小时后,烘干混合物至水份少于6%;再在1280±15℃的烧结温度下采用的是箱式炉或者隧道炉烧结两小时,自然气氛下固相合成,再自然降温至常温,即制得x(BaTiO3),其中,x取值范围为0.8~0.9;
改性锆酸钙的制备:
将电子级碳酸钙和纯度大于99.3%,粒度小于5um的二氧化锆及三氧化二铋和去离子水,按重量比(90-110):(110-130):(5-9):190的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1260±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的改性锆酸钙。
锡酸铋的制备:
将气化法生产的二氧化锡和三氧化二铋和去离子水,按重量比 (100-110):(110-130):180的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1000±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的锡酸铋。
在分别制备钛酸钡、改性锆酸钙、锡酸铋的过程中,所述球磨机球体的重量与加入的水的重量比为3:0.8。
将钛酸钡、改性锆酸钙、锡酸铋混合后加入助溶剂,再在高速搅拌磨或者砂磨机中,将混合物的粒度打磨到2微米以下,加入2.6%的PVA在造粒塔中造粒后即制得成品。其中,所述钛酸钡、改性锆酸钙、锡酸铋的重量比为0.8:(0.1~0.15):(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%。本实施例中的助溶剂为金属氧化物,且金属氧化物为二氧化锰和氧化锌的混合物。二氧化锰与氧化锌之间的重量比等于1:(3.6~4.8)。
实施例2,本发明一种介电常数大于12000的介电材料,采用了以下方法制得:
钛酸钡的制备:将粉末状的碳酸钡、二氧化钛按照摩尔比1:1称量配好;再将二氧化钛、碳酸钡以及水按重量比称重后加入球磨机,其中碳酸钡、二氧化钛的重量之和与水的重量比等于1:0.8;球磨两小时后,烘干混合物至水份少于6%;再在1280±15℃的烧结温度下采用的是箱式炉或者隧道炉烧结两小时,自然气氛下固相合成,再自然降温至常温,即制得x(BaTiO3),其中,x取值范围为0.8~0.9;
改性锆酸钙的制备:
将电子级碳酸钙和纯度大于99.3%,粒度小于5um的二氧化锆及三氧化二铋和去离子水,按重量比(90-110):(110-130):(5-9):190的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1260±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的改性锆酸钙。
锡酸铋的制备:
将气化法生产的二氧化锡和三氧化二铋和去离子水,按重量比 (100-110):(110-130):180的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1000±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的锡酸铋。
在分别制备钛酸钡、改性锆酸钙、锡酸铋的过程中,所述球磨机球体的重量与加入的水的重量比为3:0.8。
将改酸钡、改性锆酸钙、锡酸铋混合后加入助溶剂,再在高速搅拌磨或者砂磨机中,将混合物的粒度打磨到2微米以下,加入2.6%的PVA在造粒塔中造粒后即制得成品。其中,所述钛酸钡、改性锆酸钙、锡酸铋的重量比为0.83:(0.1~0.15):(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%。本实施例中的助溶剂为金属氧化物,且金属氧化物为二氧化锰和氧化锌的混合物。二氧化锰与氧化锌之间的重量比等于 1:(3.6~4.8)。
实施例3,本发明一种介电常数大于12000的介电材料,采用了以下方法制得:
钛酸钡的制备:将粉末状的碳酸钡、二氧化钛按照摩尔比1:1称量配好;再将二氧化钛、碳酸钡以及水按重量比称重后加入球磨机,其中碳酸钡、二氧化钛的重量之和与水的重量比等于1:0.8;球磨两小时后,烘干混合物至水份少于6%;再在1280±15℃的烧结温度下采用的是箱式炉或者隧道炉烧结两小时,自然气氛下固相合成,再自然降温至常温,即制得x(BaTiO3),其中,x取值范围为0.8~0.9;
改性锆酸钙的制备:
将电子级碳酸钙和纯度大于99.3%,粒度小于5um的二氧化锆及三氧化二铋和去离子水,按重量比(90-110):(110-130):(5-9):190的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1260±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的改性锆酸钙。
锡酸铋的制备:
将气化法生产的二氧化锡和三氧化二铋和去离子水,按重量比 (100-110):(110-130):180的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1000±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的锡酸铋。
在分别制备钛酸钡、改性锆酸钙、锡酸铋的过程中,所述球磨机球体的重量与加入的水的重量比为3:0.8。
将钛酸钡、改性锆酸钙、锡酸铋混合后加入助溶剂,再在高速搅拌磨或者砂磨机中,将混合物的粒度打磨到2微米以下,加入2.6%PVA在造粒塔中造粒后即制得成品。其中,所述钛酸钡、改性锆酸钙、锡酸铋的重量比为 0.85:(0.1~0.15):(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%。本实施例中的助溶剂为金属氧化物,且金属氧化物为二氧化锰和氧化锌的混合物。二氧化锰与氧化锌之间的重量比等于1:(3.6~4.8)。
实施例4,本发明一种介电常数大于12000的介电材料,采用了以下方法制得:
钛酸钡的制备:将粉末状的碳酸钡、二氧化钛按照摩尔比1:1称量配好;再将二氧化钛、碳酸钡以及水按重量比称重后加入球磨机,其中碳酸钡、二氧化钛的重量之和与水的重量比等于1:0.8;球磨两小时后,烘干混合物至水份少于6%;再在1280±15℃的烧结温度下采用的是箱式炉或者隧道炉烧结两小时,自然气氛下固相合成,再自然降温至常温,即制得x(BaTiO3),其中,x取值范围为0.8~0.9;
改性锆酸钙的制备:
将电子级碳酸钙和纯度大于99.3%,粒度小于5um的二氧化锆及三氧化二铋和去离子水,按重量比(90-110):(110-130):(5-9):190的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1260±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的改性锆酸钙。
锡酸铋的制备:
将气化法生产的二氧化锡和三氧化二铋和去离子水,按重量比(100-110):(110-130):180的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1000±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的锡酸铋。
在分别制备钛酸钡、改性锆酸钙、锡酸铋的过程中,所述球磨机球体的重量与加入的水的重量比为3:0.8。
将钛酸钡、改性锆酸钙、锡酸铋混合后加入助溶剂,再在高速搅拌磨或者砂磨机中,将混合物的粒度打磨到2微米以下,加入2.6%的PVA在造粒塔中造粒后即制得成品。其中,所述钛酸钡、改性锆酸钙、锡酸铋的重量比为0.87:(0.1~0.15):(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%。本实施例中的助溶剂为金属氧化物,且金属氧化物为二氧化锰和氧化锌的混合物。二氧化锰与氧化锌之间的重量比等于 1:(3.6~4.8)。
实施例5,本发明一种介电常数大于12000的介电材料,采用了以下方法制得:
钛酸钡的制备:将粉末状的碳酸钡、二氧化钛按照摩尔比1:1称量配好;再将二氧化钛、碳酸钡以及水按重量比称重后加入球磨机,其中碳酸钡、二氧化钛的重量之和与水的重量比等于1:0.8;球磨两小时后,烘干混合物至水份少于6%;再在1280±15℃的烧结温度下采用的是箱式炉或者隧道炉烧结两小时,自然气氛下固相合成,再自然降温至常温,即制得x(BaTiO3),其中,x取值范围为0.8~0.9;
改性锆酸钙的制备:
将电子级碳酸钙和纯度大于99.3%,粒度小于5um的二氧化锆及三氧化二铋和去离子水,按重量比(90-110):(110-130):(5-9):190的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1260±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的改性锆酸钙。
锡酸铋的制备:
将气化法生产的二氧化锡和三氧化二铋和去离子水,按重量比 (100-110):(110-130):180的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1000±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的锡酸铋。
在分别制备钛酸钡、改性锆酸钙、锡酸铋的过程中,所述球磨机球体的重量与加入的水的重量比为3:0.8。
将钛酸钡、改性锆酸钙、锡酸铋混合后加入助溶剂,再在高速搅拌磨或者砂磨机中,将混合物的粒度打磨到2微米以下,加入2.6%的PVA在造粒塔中造粒后即制得成品。其中,所述钛酸钡、改性锆酸钙、锡酸铋的重量比为0.89:(0.1~0.15):(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%。本实施例中的助溶剂为金属氧化物,且金属氧化物为二氧化锰和氧化锌的混合物。二氧化锰与氧化锌之间的重量比等于 1:(3.6~4.8)。
实施例6,本发明一种介电常数大于12000的介电材料,采用了以下方法制得:
钛酸钡的制备:将粉末状的碳酸钡、二氧化钛按照摩尔比1:1称量配好;再将二氧化钛、碳酸钡以及水按重量比称重后加入球磨机,其中碳酸钡、二氧化钛的重量之和与水的重量比等于1:0.8;球磨两小时后,烘干混合物至水份少于6%;再在1280±15℃的烧结温度下采用的是箱式炉或者隧道炉烧结两小时,自然气氛下固相合成,再自然降温至常温,即制得x(BaTiO3),其中,x取值范围为0.8~0.9;
改性锆酸钙的制备:
将电子级碳酸钙和纯度大于99.3%,粒度小于5um的二氧化锆及三氧化二铋和去离子水,按重量比(90-110):(110-130):(5-9):190的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1260±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的改性锆酸钙。
锡酸铋的制备:
将气化法生产的二氧化锡和三氧化二铋和去离子水,按重量比 (100-110):(110-130):180的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,混合物水份少于6%;再在1000±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,制成固相合成的锡酸铋。
在分别制备钛酸钡、改性锆酸钙、锡酸铋的过程中,所述球磨机球体的重量与加入的水的重量比为3:0.8。
将钛酸钡、改性锆酸钙、锡酸铋混合后加入助溶剂,再在高速搅拌磨或者砂磨机中,将混合物的粒度打磨到2微米以下,加入2.6%的PVA在造粒塔中造粒后即制得成品。其中,所述钛酸钡、改性锆酸钙、锡酸铋的重量比为(0.8~0.9):0.13:(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%。本实施例中的助溶剂为金属氧化物,且金属氧化物为二氧化锰和氧化锌的混合物。二氧化锰与氧化锌之间的重量比等于1:(3.6~4.8)。
将上述实施例分别制得的成品进行分析,得到分析结果如下:
介电系数达12000到13000,温度特性满足2E4材料的要求,本发明改性后的材料介电常数明显大于没有改性的钛酸钡材料。将本发明实施例分别得到的材料与没有改性的钛酸钡(也没有添加改性锆酸钙、锡酸铋和助溶剂) 进行比对分析,具体实验数据如下表:
介电常数比较表
介电常数 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 |
以前配方 | 9200 | 9300 | 9350 | 9400 | 9450 | 9600 |
本发明 | 12600 | 13000 | 12800 | 12700 | 12600 | 12700 |
抗电强度比较表
从以上数据可以看出本发明的抗电强度远远大于以前的材料,达到了 152贴片安规的使用要求。
同时检测得到本发明上述6个实施例得到的材料在温度特性上也有很好的表现。
温度特性比较表
温度系数 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 |
原配方 | <58 | <60 | <70 | <69 | <57 | <60 |
本发明 | <56 | <56 | <56 | <56 | <56 | <56 |
介质损耗比较表
介质损耗 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 实施例5 | 实施例6 |
原配方 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
本发明 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
从以上数据可以看出,本发明完全达到了贴片安规的要求,在大幅度提高材料的介电常数和抗电强度的时候,同时材料的温度特性和介质损耗也同时满足2E4材料的相关要求。
综上所述,本发明用改性过的锆 酸钙、锡酸铋同时改性钛酸钡提高了介电常数,改善了温度特性。同时,利用金属氧化物参杂改性,提高材料的抗电强度。解决了陶瓷贴片安规Y1-102、Y1-152对介质材料的要求问题,已经批量生产,满足了市场的需求。
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明的保护范围,凡在本发明的精神和原则之内,所作的任何修改、等同替换、均包含在本发明的保护范围之内。
Claims (4)
1.一种介电常数大于12000的介电材料制备方法,其特征在于,其包括以下步骤:
钛酸钡的制备:将粉末状的电子级的碳酸钡、二氧化钛按照摩尔比1:1称量配好;再将二氧化钛、碳酸钡以及水按重量比称重后加入球磨机,其中碳酸钡、二氧化钛的重量之和与水的重量比等于1:0.8;球磨两小时后,烘干混合物至水分少于6%;再在1280±15℃的烧结温度下烧结两小时,自然气氛下固相合成,再自然降温至常温,即制得钛酸钡;
改性锆酸钙的制备:
将电子级的碳酸钙、纯度大于99.3%且粒度小于5um的二氧化锆、三氧化二铋、去离子水按重量比(90-110):(110-130):(5-9):190的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,待混合物水分少于6%;再在1260±15℃的烧结温度下烧结两小时,自然气氛下固相合成,自然降温至常温,即制成固相合成的改性锆酸钙;
锡酸铋的制备:
将气化法生产的二氧化锡、三氧化二铋、去离子水按重量比(100-110):(110-130):180的比例,加入球磨机中,球磨两小时后,倒入烘盘中烘干,待混合物水分少于6%;再在1000±15℃的烧结温度下烧结两小时,自然气氛下固相合成,自然降温至常温,即制成固相合成的锡酸铋;
将钛酸钡、改性锆酸钙、锡酸铋混合后加入助溶剂后即制得成品,其中,所述钛酸钡、改性锆酸钙、锡酸铋的重量比为(0.8~0.9):(0.1~0.15):(0.01~0.05);助溶剂的重量为钛酸钡、改性锆酸钙、锡酸铋重量和的1%~8%,所述助溶剂为金属氧化物,所述助溶剂的金属氧化物为二氧化锰和氧化锌的混合物。
2.根据权利要求1所述的一种介电常数大于12000的介电材料制备方法,其特征在于,在分别制备钛酸钡、改性锆酸钙、锡酸铋的过程中,所述球磨机中球体的重量与加入的水的重量比为3:0.8。
3.根据权利要求1所述的一种介电常数大于12000的介电材料制备方法,其特征在于,二氧化锰与氧化锌之间的重量比等于1:(3.6~4.8)。
4.根据权利要求1所述的一种介电常数大于12000的介电材料制备方法,其特征在于,烧结采用的是箱式炉或者隧道炉。
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