CN109354491B - 一种高耐压温度稳定型介质材料配方及其制备方法 - Google Patents
一种高耐压温度稳定型介质材料配方及其制备方法 Download PDFInfo
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- 239000003989 dielectric material Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000009472 formulation Methods 0.000 title description 2
- 239000003985 ceramic capacitor Substances 0.000 claims abstract description 22
- 239000011521 glass Substances 0.000 claims abstract description 20
- 238000000498 ball milling Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 13
- 229910002113 barium titanate Inorganic materials 0.000 claims abstract description 8
- 238000010532 solid phase synthesis reaction Methods 0.000 claims abstract description 7
- 239000011656 manganese carbonate Substances 0.000 claims abstract description 6
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims abstract description 6
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- 238000002156 mixing Methods 0.000 claims description 19
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 11
- 238000004519 manufacturing process Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 229910052681 coesite Inorganic materials 0.000 claims description 8
- 229910052906 cristobalite Inorganic materials 0.000 claims description 8
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 229910052682 stishovite Inorganic materials 0.000 claims description 8
- 229910052905 tridymite Inorganic materials 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000010791 quenching Methods 0.000 claims description 7
- 230000000171 quenching effect Effects 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Inorganic materials [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 3
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 2
- 229910052779 Neodymium Inorganic materials 0.000 claims description 2
- 229910052772 Samarium Inorganic materials 0.000 claims description 2
- 239000002612 dispersion medium Substances 0.000 claims description 2
- 229910052746 lanthanum Inorganic materials 0.000 claims description 2
- 239000000155 melt Substances 0.000 claims description 2
- 229910052727 yttrium Inorganic materials 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 16
- 239000003990 capacitor Substances 0.000 abstract description 8
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000010304 firing Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 description 15
- 238000001354 calcination Methods 0.000 description 11
- 239000000919 ceramic Substances 0.000 description 11
- 238000005245 sintering Methods 0.000 description 7
- 239000002609 medium Substances 0.000 description 6
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 5
- 229910010293 ceramic material Inorganic materials 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 229910052726 zirconium Inorganic materials 0.000 description 5
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 2
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- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
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- 239000000872 buffer Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 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
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 description 1
- 150000002910 rare earth metals Chemical class 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
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
一种高耐压温度稳定型介质材料、陶瓷电容器及其制备方法。通过固相法合成ZnNb2O6、Ba(Zn1/3,Nb2/3)O3，烧制ZBS玻璃；以100重量份的BaTiO3，添加3～8重量份的ZnNb2O6；10～20重量份的Ba(Zn1/3,Nb2/3)O3；0.1～0.3重量份的MnCO3；0.1～0.4重量份的Re2O3；1～3重量份的ZBS玻璃。通过球磨分散、烘干破碎最终形成介质材料。本发明提供的介质材料，介电常数为450±50，损耗角正切值为DF≤20×10‑4，工作温度区间为‑55℃～125℃，电容温度系数为‑200ppm/K～200ppm/K，且具有极高的击穿强度(≥60V/μm)。利用本发明提供的介质材料可制备工作温度范围为‑55℃～125℃的脉冲储能电容器。
Description
技术领域
本发明涉及电介质功能陶瓷材料，特别是指一种具有高耐压、温度稳定特性的陶瓷介质材料及其制备方法，以及采用该介质材料制备陶瓷电容器。
背景技术
在脉冲功率系统中，电介质储能电容器是整个系统中不可缺少的重要组成部分，对整个脉冲功率系统起着至关重要的作用，它作为储能器件可以将大量的能量储存集中起来并在极短的时间内释放在负载上，形成强大的脉冲功率及较高的电流。这一系列特性使其在固体发动机点火系统、卫星电推进系统中都有广泛的应用需求，可大幅提高系统的安全性与可靠性；此外，在中高压储能电路、高压逆变器等民用领域具有推广应用前景，在引爆线路、点火系统、激光系统、能量存储模块、脉冲光电系统、石油勘探、地震评估、缓冲器、电源中断保护电路等诸多领域具有应用潜力。
目前电路设计中普遍采用的脉冲多层瓷介电容器，随着介质层厚度的降低，介质层的击穿强度程下降趋势，极大的提高了高压储能电容器产品体积，不利于电容器产品的工业化生产。因而，提高储能介质材料的击穿强度是目前储能陶瓷材料急需攻关的技术难题，本发明提供的一种高耐压温度稳定型介质材料，可以填补耐高压储能陶瓷材料市场空白。
发明内容
本发明的目的是针对现有技术的不足，提供一种高耐压温度稳定型介质材料及其制备方法，采用该介质材料制作高压储能多层陶瓷电容器。
本发明采用如下的技术方案：
一种高耐压温度稳定型介质材料，其原料组分为：
100重量份的BaTiO3；
3～8重量份的ZnNb2O6；
10～20重量份的Ba(Zn1/3,Nb2/3)O3；
0.1～0.3重量份的MnCO3；
0.1～0.4重量份的Re2O3；
1～3重量份的ZBS玻璃。
其中：Re2O3为稀土物质，Re包括但不限于：Y、La、Nd、Sm、Gd、Er等元素。
进一步的，所述ZnNb2O6主要由ZnO、Nb2O5固相法合成。
进一步的，所述Ba(Zn1/3,Nb2/3)O3主要由BaCO3、ZnO、Nb2O5固相法合成。
进一步的，所述ZBS玻璃由ZnO、H3BO3、SiO2合成。
一种高耐压温度稳定型陶瓷电容器，采用所述高耐压温度稳定型介质材料制成。
一种高耐压温度稳定型介质材料的制备方法，包括如下步骤：
(1)将ZnO和Nb2O5按摩尔比1:1进行配制，固相法合成ZnNb2O6，合成温度800～950℃，保温约1～4h；
(2)将BaCO3、ZnO和Nb2O5按摩尔比3:1:1进行配制，固相法合成Ba(Zn1/3,Nb2/3)O3，合成温度1000～1200℃，保温约1～4h；
(3)将ZnO、H3BO3、SiO2按摩尔比4:4:1混合，迅速升温至1350～1450℃，保温0.5h，将熔融物淬冷至室温，制成ZBS玻璃；
(4)以100重量份的BaTiO3为基材，添加3～8重量份的ZnNb2O6，10～20重量份的Ba(Zn1/3,Nb2/3)O3，0.1～0.3重量份的MnCO3，0.1～0.4重量份的Re2O3，1～3重量份的ZBS玻璃，用去离子水作为分散介质，球磨、烘干并造粒，制成所述高耐压温度稳定型介质材料。
一种高耐压温度稳定型陶瓷电容器的制备方法，包括如下步骤：将所述高耐压温度稳定型介质材料在空气气氛中，温度至1080～1180℃，保温煅烧2-5h，制成多层陶瓷电容器。
本发明的有益效果是：以BaTiO3为基础，添加适量的ZnNb2O6、Ba(Zn1/3,Nb2/3)O3，有效将介质材料的介电常数控制在450±50的范围，在适当降低损耗的同时，将电容温度系数控制在-200～200ppm/K的范围；适当添加ZBS玻璃化合物作助烧剂，有利于提高介质瓷体的致密度，降低损耗；在钛酸钡基介电陶瓷材料中适量添加稀土元素，既可以作为施主也可以作为受主进行掺杂改性，提高材料系统的绝缘电阻率、抗老化性能和抗还原性能；适当添加MnCO3，能够在烧结过程中有效阻止Ti4+的还原，在降低介质损耗中起决定作用。
附图说明
下面结合附图对本发明作进一步详细说明。
图1为本发明提供的高压储能多层陶瓷电容器结构示意图。
图中标注1为Sn/Pb，标注2为Ni，标注3为Ag，标注4为陶瓷，标注5为内电极：70Ag/30Pd。
具体实施方式
以下结合具体实施例对本发明做进一步详细描述：
实施例1
(1)按摩尔比1:1，称取23.44重量份ZnO，76.56重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于800℃温度煅烧4小时合成ZnNb2O6；
(2)按摩尔比3:1:1，称取63.03重量份BaCO3，8.66重量份ZnO和28.30重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于1000℃温度煅烧4小时合成Ba(Zn1/3,Nb2/3)O3；
(3)按摩尔比4:4:1，称取51.43重量份ZnO，39.08重量份H3BO3，9.49重量份SiO2，充分混合、40目筛网，加热至1350℃并保温0.5h，淬冷至室温，制成ZBS玻璃
(4)按重量份称取，100g BaTiO3，7.44g ZnNb2O6，17.30g Ba(Zn1/3,Nb2/3)O3，0.25gMnCO3，0.33g Er2O3，1.72g ZBS玻璃进行配料，以去离子水为球磨介质，采用2mm锆球研磨6h，150℃烘干、破碎，制成粉末状陶瓷介质材料。
(5)将步骤(4)制得的陶瓷介质材料，经过多层陶瓷电容器制造工艺，以70Ag30Pd为内电极，在空气气氛中于温度1180℃烧结保温2h，制成图1所示结构的多层陶瓷电容器。
实施例2
(1)按摩尔比1:1，称取23.44重量份ZnO，76.56重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于950℃温度煅烧1小时合成ZnNb2O6；
(2)按摩尔比3:1:1，称取63.03重量份BaCO3，8.66重量份ZnO和28.30重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于1050℃温度煅烧3小时合成Ba(Zn1/3,Nb2/3)O3；
(3)按摩尔比4:4:1，称取51.43重量份ZnO，39.08重量份H3BO3，9.49重量份SiO2，充分混合、40目筛网，加热至1400℃并保温0.5h，淬冷至室温，制成ZBS玻璃
(4)按重量份称取，100g BaTiO3，6.21g ZnNb2O6，19.37g Ba(Zn1/3,Nb2/3)O3，0.10gMnCO3，0.13g La2O3，2.92g ZBS玻璃进行配料。以去离子水为球磨介质，采用2mm锆球研磨6h，150℃烘干、破碎，制成粉末状陶瓷介质材料。
(5)将步骤(4)制得的陶瓷介质材料，经过多层陶瓷电容器制造工艺，以70Ag30Pd为内电极，在空气气氛中于1140℃烧结保温3h，制成图1所示结构的多层陶瓷电容器。
实施例3
(1)按摩尔比1:1，称取23.44重量份ZnO，76.56重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于850℃温度煅烧3小时合成ZnNb2O6；
(2)按摩尔比3:1:1，称取63.03重量份BaCO3，8.66重量份ZnO和28.30重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于1100℃温度煅烧2小时合成Ba(Zn1/3,Nb2/3)O3；
(3)按摩尔比4:4:1，称取51.43重量份ZnO，39.08重量份H3BO3，9.49重量份SiO2，充分混合、40目筛网，加热至1350℃并保温0.5h，淬冷至室温，制成ZBS玻璃
(4)按重量份称取，100g BaTiO3，8.00g ZnNb2O6，10.30g Ba(Zn1/3,Nb2/3)O3，0.10gMnCO3，0.36g Gd2O3，1.02g ZBS玻璃进行配料。以去离子水为球磨介质，采用2mm锆球研磨6h，150℃烘干、破碎，制成粉末状陶瓷介质材料。
(5)将步骤(4)制得的陶瓷介质材料，经过多层陶瓷电容器制造工艺，以70Ag30Pd为内电极，在空气气氛中于1140℃烧结保温3h，制成图1所示结构的多层陶瓷电容器。
实施例4
(1)按摩尔比1:1，称取23.44重量份ZnO，76.56重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于900℃温度煅烧2小时合成ZnNb2O6；
(2)按摩尔比3:1:1，称取63.03重量份BaCO3，8.66重量份ZnO和28.30重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于1150℃温度煅烧2小时合成Ba(Zn1/3,Nb2/3)O3；
(3)按摩尔比4:4:1，称取51.43重量份ZnO，39.08重量份H3BO3，9.49重量份SiO2，充分混合、40目筛网，加热至1450℃并保温0.5h，淬冷至室温，制成ZBS玻璃
(4)按重量份称取，100g BaTiO3，3.04g ZnNb2O6，19.99g Ba(Zn1/3,Nb2/3)O3，0.30gMnCO3，0.4g Nd2O3，3.00g ZBS玻璃进行配料。以去离子水为球磨介质，采用2mm锆球研磨6h，150℃烘干、破碎，制成粉末状陶瓷介质材料。
(5)将步骤(4)制得的陶瓷介质材料，经过多层陶瓷电容器制造工艺，以70Ag30Pd为内电极，在空气气氛中于1120℃烧结保温3h，制成图1所示结构的多层陶瓷电容器。
实施例5
(1)按摩尔比1:1，称取23.44重量份ZnO，76.56重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于950℃温度煅烧1小时合成ZnNb2O6；
(2)按摩尔比3:1:1，称取63.03重量份BaCO3，8.66重量份ZnO和28.30重量份Nb2O5，球磨混合、干燥，破碎过40目筛网，于1200℃温度煅烧1小时合成Ba(Zn1/3,Nb2/3)O3；
(3)按摩尔比4:4:1，称取51.43重量份ZnO，39.08重量份H3BO3，9.49重量份SiO2，充分混合、40目筛网，加热至1350℃并保温0.5h，淬冷至室温，制成ZBS玻璃
(4)按重量份称取，100g BaTiO3，5.47g ZnNb2O6，15.36g Ba(Zn1/3,Nb2/3)O3，0.24gMnCO3，0.27g Sm2O3，2.52g ZBS玻璃进行配料。以去离子水为球磨介质，采用2mm锆球研磨6h，150℃烘干、破碎，制成粉末状陶瓷介质材料。
(5)将步骤(4)制得的陶瓷介质材料，经过多层陶瓷电容器制造工艺，以70Ag30Pd为内电极，在空气气氛中于1080℃烧结保温5h，制成图1所示结构的多层陶瓷电容器。
上述5个实施例所制备的多层陶瓷电容器样品烧结后，经过倒角、端银、烧附、电镀后，测试样品的电学性能，其结果列于下表：
其中
K：介电常数
DF：损耗角正切值
TCC：电容温度系数
IR：绝缘电阻
BDV：击穿强度
由上述数据可知，本发明提供的高耐压温度稳定型介质材料具有介电损耗低，工作温度区间宽(-55℃～125℃)，温度稳定性良好(-200～200ppm/K)，极高的击穿强度≥60V/μm等优点。利用本发明可设计工作温度范围为-55℃～125℃的高压储能电容器，作为储能器件可以将大量的能量储存集中起来、并在极短的时间内释放在负载上，形成强大的脉冲功率及较高的电流，有极高的产业化前景及工业应用价值。
上述仅为本发明的具体实施方式，但本发明的设计构思并不局限于此，凡利用此构思对本发明进行非实质性的改动，均应属于侵犯本发明保护范围的行为。
Claims (3)
1.一种高耐压温度稳定型介质材料，用于制作高耐压温度稳定型陶瓷电容器，其原料组分为：
100重量份的BaTiO3；
3～8重量份的ZnNb2O6；
10～20重量份的Ba(Zn1/3, Nb2/3)O3；
0.1～0.3重量份的MnCO3；
0.1～0.4重量份的Re2O3；
1～3重量份的ZBS玻璃；
其中， Re为Y、La、Nd、Sm、Gd、Er元素；
（1）将ZnO和Nb2O5按摩尔比1:1进行配制，固相法合成ZnNb2O6，合成温度800～950℃，保温1～4h；
（2）将BaCO3、ZnO和Nb2O5按摩尔比3:1:1进行配制，固相法合成Ba(Zn1/3, Nb2/3)O3，合成温度1000～1200℃，保温1～4h；
（3）将ZnO、H3BO3、SiO2按摩尔比4:4:1混合，迅速升温至1350～1450℃，保温0.5h，将熔融物淬冷至室温，制成ZBS玻璃；
（4）以100重量份的BaTiO3为基材，添加3～8重量份的ZnNb2O6，10～20重量份的Ba(Zn1/3, Nb2/3)O3，0.1～0.3重量份的MnCO3，0.1～0.4重量份的Re2O3，1～3重量份的ZBS玻璃，用去离子水作为分散介质，球磨、烘干并造粒，制成所述高耐压温度稳定型介质材料。
2.一种高耐压温度稳定型陶瓷电容器，其特征在于：采用权利要求1所述高耐压温度稳定型介质材料制成。
3.一种高耐压温度稳定型陶瓷电容器的制备方法，包括如下步骤：将权利要求1所述高耐压温度稳定型介质材料在空气气氛中煅烧，温度1080～1180℃，保温煅烧2-5h，制成多层陶瓷电容器。
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