CN107324800A - 一种陶瓷电容器用介质材料及其制备工艺 - Google Patents

一种陶瓷电容器用介质材料及其制备工艺 Download PDF

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CN107324800A
CN107324800A CN201710537035.2A CN201710537035A CN107324800A CN 107324800 A CN107324800 A CN 107324800A CN 201710537035 A CN201710537035 A CN 201710537035A CN 107324800 A CN107324800 A CN 107324800A
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ceramic capacitor
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杨自芬
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Hefei Zhuo Zhuo Electric Power Co Ltd
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Abstract

本发明公开了一种陶瓷电容器用介质材料及其制备工艺,涉及电子元件与材料技术领域,该介质材料包括以下原料:BaTiO3、SrTiO3、BaZrO3、CaZrO3、ZnB2O4玻璃粉、Nb2O5、CeO2、MnCO3、Gd2O3和凹凸棒粘土。其制备工艺是通过对原料加水球磨混合、烘干、造粒压片及烧结即可。该种陶瓷电容器介质材料及介电常数高,耐电压高,电容温度变化率小,符合Y5U特性的要求,不含铅,对环境无污染,制备简单方便,烧结温度低,能耗少,适宜推广应用。

Description

一种陶瓷电容器用介质材料及其制备工艺
技术领域
本发明涉及电子元件与材料技术领域,具体涉及一种陶瓷电容器用介质材料及其制备工艺。
背景技术
近几年来,在高端民用产品市场中随着电力系统和脉冲功率的不断升级改造,例如遮断器、负载关闭器、高压电源等的设备对陶瓷电容器提出了高耐电压、低损耗、高可靠性、小型化和大容量等的要求。目前我国加大了对激光武器和电磁武器等的研究,并取得了一定的成果。激光武器需要瞬间提供巨大的能量,这种功能通过电路中的超高压电容倍压来实现,并且超高压电容器是电路中的核心器件。由于国内原材料的限制,我国在军事领域对超高压电容器的需求主要依赖进口,这给我国的国防安全带来了一定的风险。目前所需的超高压陶瓷电容器用介质材料不仅要求耐电压更高,而且还需要较小的介质损耗及较高的体积电阻率,以满足超高压电容器高可靠性。目前有些陶瓷电容器的电介质中含有铅和镉,在陶瓷电容器的生产、使用和废弃过程中对人体和环境的危害较大,其介电常数小,耐电压较低,使用效果及性能不理想,满足不了人们对其需求。
发明内容
针对现有技术中存在的问题,本发明提供了一种陶瓷电容器用介质材料及其制备工艺,该种陶瓷电容器介质材料及介电常数高,耐电压高,电容温度变化率小,符合Y5U特性的要求,不含铅,对环境无污染,制备简单方便,烧结温度低,能耗少,适宜推广应用。
为了达到上述目的,本发明通过以下技术方案来实现的:
一种陶瓷电容器用介质材料,包括以下按重量份计的原料:BaTiO325-35份、SrTiO320-30份、BaZrO310-20份、CaZrO38-12份、ZnB2O4玻璃粉5-15份、Nb2O54-8份、CeO23-7份、MnCO33-5份、Gd2O33-5份和凹凸棒粘土15-25份。
进一步地,所述介质材料包括以下按重量份计的原料:BaTiO330份、SrTiO325份、BaZrO315份、CaZrO310份、ZnB2O4玻璃粉10份、Nb2O56份、CeO25份、MnCO34份、Gd2O34份和凹凸棒粘土20份。
进一步地,所述BaTiO3是采用如下工艺制备:将常规的化学原料BaCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1120-1210℃保温60-80min,固相反应合成BaTiO3,冷却后研磨过150-250目筛,备用。
进一步地,所述SrTiO3是采用如下工艺制备:将常规的化学原料SrCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1020-1140℃保温80-100min,固相反应合成SrTiO3,冷却后研磨过150-250目筛,备用。
进一步地,所述CaZrO3是采用如下工艺制备:将常规的化学原料CaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1140-1220℃保温70-90min,固相反应合成CaZrO3,冷却后研磨过150-250目筛,备用。
进一步地,所述BaZrO3是采用如下工艺制备:将常规的化学原料BaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1080-1160℃保温60-80min,固相反应合成BaZrO3,冷却后研磨过150-250目筛,备用。
上述的一种陶瓷电容器用介质材料的制备工艺,按照以下步骤进行:
(1)按所述重量份配比称取原料,将所述凹凸棒粘土置于8%-12%的盐酸溶液中浸泡40-60min,抽滤后将所得物料烘干,再在250-350℃下进行高温煅烧1-2h,取出冷却后通过研磨机研磨成120-160目的细粉,备用;
(2)将所有原料输送至行星球磨机中加入去离子水球磨混合,且料:球:水=1:3:(0.6-0.9)(质量比),球磨2-4h后,烘干得干粉料;
(3)向干粉料中加入粘合剂进行造粒,混研后过40-60目筛,再在20-30Mpa压力下进行干压成生坯片;
(4)将制得的生坯片在稀有气体环境下烧结2-4h,待冷却至780-860℃时保温1-2h,随后随炉冷却,再在480-520℃下保温15-25min进行烧银,形成银电极,再焊引线,进行包封,即可。
进一步地,在步骤(3)中,所述粘合剂采用重量百分比浓度为15-25%的聚乙烯醇水溶液,该聚乙烯醇水溶液的重量为干粉料重量的8-12%。
进一步地,在步骤(4)中,所述稀有气体为氮气或者氩气,烧结温度为980-1060℃。
本发明具有如下的有益效果:
(1)本发明的电容器介质材料制备简单方便,相比现有技术中的工艺流程,其烧结温度低,能耗少,原料中不含铅和镉等有害元素,对环境无污染,对人体无危害,符合国家倡导的绿色环保的标准;
(2)本发明的电容器介质材料的介电常数高,可达20000以上;耐电压程度高,直流耐电压可达20kV/mm以上,交流耐压可达15kV/mm以上;因本发明的电容器介质介电常数高,能实现陶瓷电容器的小型化和大容量,同样能降低成本;
(3)本发明的电容器介质的电容温度变化率小,符合Y5U特性的要求;另外因其介质损耗小于0.3%,在使用过程中性能稳定性好,安全性高,适宜推广应用。
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描述,以下实施例仅用于更加清楚地说明本发明的技术方案,而不能以此来限制本发明的保护范围。
实施例1
一种陶瓷电容器用介质材料,称取以下原料待用:BaTiO325kg、SrTiO320kg、BaZrO310kg、CaZrO38kg、ZnB2O4玻璃粉5kg、Nb2O54kg、CeO23kg、MnCO33kg、Gd2O33kg和凹凸棒粘土15kg。
其中,上述的BaTiO3是采用如下工艺制备:将常规的化学原料BaCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1120℃保温60min,固相反应合成BaTiO3,冷却后研磨过150目筛,备用。
上述的SrTiO3是采用如下工艺制备:将常规的化学原料SrCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1020℃保温80min,固相反应合成SrTiO3,冷却后研磨过150目筛,备用。
上述的CaZrO3是采用如下工艺制备:将常规的化学原料CaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1140℃保温70min,固相反应合成CaZrO3,冷却后研磨过150目筛,备用。
上述的BaZrO3是采用如下工艺制备:将常规的化学原料BaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1080℃保温60min,固相反应合成BaZrO3,冷却后研磨过150目筛,备用。
上述的一种陶瓷电容器用介质材料的制备工艺,按照以下步骤进行:
(1)先将称取的凹凸棒粘土置于8%的盐酸溶液中浸泡40min,抽滤后将所得物料烘干,再在250℃下进行高温煅烧1h,取出冷却后通过研磨机研磨成120目的细粉,备用;
(2)再将所有原料输送至行星球磨机中加入去离子水球磨混合,且料:球:水=1:3:0.6(质量比),球磨2h后,烘干得干粉料;
(3)之后向干粉料中加入其重量8%重量百分比浓度为15%的聚乙烯醇水溶液进行造粒,混研后过40目筛,再在20Mpa压力下进行干压成生坯片;
(4)然后将制得的生坯片在充满氮气环境下烧结2h,烧结温度控制在980℃,待冷却至780℃时保温1h,随后随炉冷却,再在480℃下保温15min进行烧银,形成银电极,再焊引线,进行包封,即制得本发明的陶瓷电容器用介质材料。
实施例2
一种陶瓷电容器用介质材料,称取以下原料待用:BaTiO330kg、SrTiO325kg、BaZrO315kg、CaZrO310kg、ZnB2O4玻璃粉10kg、Nb2O56kg、CeO25kg、MnCO34kg、Gd2O34kg和凹凸棒粘土20kg。
其中,上述的BaTiO3是采用如下工艺制备:将常规的化学原料BaCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1160℃保温70min,固相反应合成BaTiO3,冷却后研磨过200目筛,备用。
上述的SrTiO3是采用如下工艺制备:将常规的化学原料SrCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1080℃保温90min,固相反应合成SrTiO3,冷却后研磨过200目筛,备用。
上述的CaZrO3是采用如下工艺制备:将常规的化学原料CaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1180℃保温80min,固相反应合成CaZrO3,冷却后研磨过200目筛,备用。
上述的BaZrO3是采用如下工艺制备:将常规的化学原料BaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1120℃保温70min,固相反应合成BaZrO3,冷却后研磨过200目筛,备用。
上述的一种陶瓷电容器用介质材料的制备工艺,按照以下步骤进行:
(1)先将称取的凹凸棒粘土置于10%的盐酸溶液中浸泡50min,抽滤后将所得物料烘干,再在300℃下进行高温煅烧1.5h,取出冷却后通过研磨机研磨成140目的细粉,备用;
(2)再将所有原料输送至行星球磨机中加入去离子水球磨混合,且料:球:水=1:3:0.8(质量比),球磨3h后,烘干得干粉料;
(3)之后向干粉料中加入其重量10%重量百分比浓度为20%的聚乙烯醇水溶液进行造粒,混研后过50目筛,再在25Mpa压力下进行干压成生坯片;
(4)然后将制得的生坯片在充满氩气环境下烧结3h,烧结温度控制在1020℃,待冷却至820℃时保温1.5h,随后随炉冷却,再在500℃下保温20min进行烧银,形成银电极,再焊引线,进行包封,即制得本发明的陶瓷电容器用介质材料。
实施例3
一种陶瓷电容器用介质材料,称取以下原料待用:BaTiO335kg、SrTiO330kg、BaZrO320kg、CaZrO312kg、ZnB2O4玻璃粉15kg、Nb2O58kg、CeO27kg、MnCO35kg、Gd2O35kg和凹凸棒粘土25kg。
其中,上述的BaTiO3是采用如下工艺制备:将常规的化学原料BaCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1210℃保温80min,固相反应合成BaTiO3,冷却后研磨过250目筛,备用。
上述的SrTiO3是采用如下工艺制备:将常规的化学原料SrCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1140℃保温100min,固相反应合成SrTiO3,冷却后研磨过250目筛,备用。
上述的CaZrO3是采用如下工艺制备:将常规的化学原料CaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1220℃保温90min,固相反应合成CaZrO3,冷却后研磨过250目筛,备用。
上述的BaZrO3是采用如下工艺制备:将常规的化学原料BaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1160℃保温80min,固相反应合成BaZrO3,冷却后研磨过250目筛,备用。
上述的一种陶瓷电容器用介质材料的制备工艺,按照以下步骤进行:
(1)先将称取的凹凸棒粘土置于12%的盐酸溶液中浸泡60min,抽滤后将所得物料烘干,再在350℃下进行高温煅烧2h,取出冷却后通过研磨机研磨成160目的细粉,备用;
(2)再将所有原料输送至行星球磨机中加入去离子水球磨混合,且料:球:水=1:3:0.9(质量比),球磨4h后,烘干得干粉料;
(3)之后向干粉料中加入其重量12%重量百分比浓度为25%的聚乙烯醇水溶液进行造粒,混研后过60目筛,再在30Mpa压力下进行干压成生坯片;
(4)然后将制得的生坯片在充满氮气环境下烧结4h,烧结温度控制在1060℃,待冷却至860℃时保温2h,随后随炉冷却,再在520℃下保温25min进行烧银,形成银电极,再焊引线,进行包封,即制得本发明的陶瓷电容器用介质材料。
以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。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 (9)

1.一种陶瓷电容器用介质材料,该陶瓷电容器的电介质耐高压高温,直流耐电压可达20kV/mm以上,交流耐压可达15kV/mm以上;介电常数为20000以上;介质损耗小于0.3%;电容温度变化率小,符合Y5U特性的要求,其特征在于,所述介质材料包括以下按重量份计的原料:BaTiO325-35份、SrTiO320-30份、BaZrO310-20份、CaZrO38-12份、ZnB2O4玻璃粉5-15份、Nb2O54-8份、CeO23-7份、MnCO33-5份、Gd2O33-5份和凹凸棒粘土15-25份。
2.根据权利要求1所述的一种陶瓷电容器用介质材料,其特征在于,所述介质材料包括以下按重量份计的原料:BaTiO330份、SrTiO325份、BaZrO315份、CaZrO310份、ZnB2O4玻璃粉10份、Nb2O56份、CeO25份、MnCO34份、Gd2O34份和凹凸棒粘土20份。
3.根据权利要求1所述的一种陶瓷电容器用介质材料,其特征在于,所述BaTiO3是采用如下工艺制备:将常规的化学原料BaCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1120-1210℃保温60-80min,固相反应合成BaTiO3,冷却后研磨过150-250目筛,备用。
4.根据权利要求1所述的一种陶瓷电容器用介质材料,其特征在于,所述SrTiO3是采用如下工艺制备:将常规的化学原料SrCO3和TiO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1020-1140℃保温80-100min,固相反应合成SrTiO3,冷却后研磨过150-250目筛,备用。
5.根据权利要求1所述的一种陶瓷电容器用介质材料,其特征在于,所述CaZrO3是采用如下工艺制备:将常规的化学原料CaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1140-1220℃保温70-90min,固相反应合成CaZrO3,冷却后研磨过150-250目筛,备用。
6.根据权利要求1所述的一种陶瓷电容器用介质材料,其特征在于,所述BaZrO3是采用如下工艺制备:将常规的化学原料BaO和ZrO2按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1080-1160℃保温60-80min,固相反应合成BaZrO3,冷却后研磨过150-250目筛,备用。
7.一种根据权利要求1-6任意一项所述的陶瓷电容器用介质材料的制备工艺,其特征在于,包括以下步骤:
(1)按所述重量份配比称取原料,将所述凹凸棒粘土置于8%-12%的盐酸溶液中浸泡40-60min,抽滤后将所得物料烘干,再在250-350℃下进行高温煅烧1-2h,取出冷却后通过研磨机研磨成120-160目的细粉,备用;
(2)将所有原料输送至行星球磨机中加入去离子水球磨混合,且料:球:水=1:3:(0.6-0.9)(质量比),球磨2-4h后,烘干得干粉料;
(3)向干粉料中加入粘合剂进行造粒,混研后过40-60目筛,再在20-30Mpa压力下进行干压成生坯片;
(4)将制得的生坯片在稀有气体环境下烧结2-4h,待冷却至780-860℃时保温1-2h,随后随炉冷却,再在480-520℃下保温15-25min进行烧银,形成银电极,再焊引线,进行包封,即可。
8.根据权利要求7所述的一种陶瓷电容器用介质材料的制备工艺,其特征在于,在步骤(3)中,所述粘合剂采用重量百分比浓度为15-25%的聚乙烯醇水溶液,该聚乙烯醇水溶液的重量为干粉料重量的8-12%。
9.根据权利要求7所述的一种陶瓷电容器用介质材料的制备工艺,其特征在于,在步骤(4)中,所述稀有气体为氮气或者氩气,烧结温度为980-1060℃。
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