CN114591079B - 一种高压低损陶瓷电容器介质及其制备方法 - Google Patents

一种高压低损陶瓷电容器介质及其制备方法 Download PDF

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CN114591079B
CN114591079B CN202210239179.0A CN202210239179A CN114591079B CN 114591079 B CN114591079 B CN 114591079B CN 202210239179 A CN202210239179 A CN 202210239179A CN 114591079 B CN114591079 B CN 114591079B
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彭道华
陈映义
牛继恩
陈甲天
姜学文
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Shantou Ruisheng Electron Co ltd
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Abstract

一种高压低损陶瓷电容器介质,其特征在于由下述重量配比的原料制成:BaZrO3 5‑7%,CeO2 0.5‑0.7%,ZnO 0.8‑1.2%,MnCO3 0.3‑0.5%,La2O3 1.5‑2.5%,W2O3 0.8‑1.2%,余量为BaTiO3。本发明还提供上述高压低损陶瓷电容器介质的一种制备方法。本发明与现有技术相比,具有如下优点:本发明的陶瓷电容器介质的介电常数高(介电常数为3400以上),耐电压高(直流耐电压可达7kV/mm以上,交流耐压可达5kV/mm以上),介质损耗小(介质损耗小于0.8%)。本发明的陶瓷电容器介质适合于制造满足Y5P特性要求的陶瓷电容器。而且,本发明的陶瓷电容器介质不含铋、铅和镉,在制备和使用过程中对环境无污染。

Description

一种高压低损陶瓷电容器介质及其制备方法
技术领域
本发明涉及无机非金属材料技术领域,具体涉及一种高压低损陶瓷电容器介质以及这种高压低损陶瓷电容器介质的制备方法。
背景技术
彩电、电脑、通迅、航空航天、导弹、航海等领域迫切需要击穿电压高、温度特性稳定、可靠性高、小型化、大容量的陶瓷电容器。目前,用于生产高压陶瓷电容器的介质中通常含有一定量的铋、铅、镉,会对人体和环境造成危害,逐渐被淘汰。有些陶瓷电容器介质虽属无铋、无铅、无镉介质材料,但介电常数小、介质损耗高、耐电压低,不利于陶瓷电容器的小型化,且耐压性较差,也不利于扩大陶瓷电容器的使用范围及提高安全性。
发明内容
本发明所要解决的技术问题是提供一种高压陶瓷电容器介质以及这种高压低损陶瓷电容器介质的制备方法,这种高压低损陶瓷电容器介质介电常数高,介质损耗低,耐电压高,且在制备和使用过程中不污染环境,制成的陶瓷电容器的温度特性满足Y5P特性的要求。采用的技术方案如下:
一种高压低损陶瓷电容器介质,其特征在于由下述重量配比的原料制成: BaZrO35-7%, CeO2 0.5-0.7%,ZnO 0.8-1.2%,MnCO3 0.3-0.5%,La2O3 1.5-2.5%,W2O3 0.8-1.2%,余量为BaTiO3
优选方案中,上述高压低损陶瓷电容器介质由下述重量配比的原料制成:BaTiO389%,BaZrO3 6%, CeO2 0.6%,ZnO 1%,MnCO3 0.4%,La2O3 2%,W2O3 1%。
上述BaTiO3(钛酸钡)形成主晶相,BaZrO3(锆酸钡)形成第二主晶相, BaTiO3(钛酸钡)与BaZrO3(锆酸钡)配合,形成双峰结构(即在15℃、50℃各形成一个居里峰),从而使介质的温度特性在Y5P范围内(±10%变化率(-25-+85℃))。添加适量的CeO2(氧化铈)、La2O3(氧化镧)在晶体的晶界层,抑制晶体长大,从而能够细化晶粒,形成细晶结构,提高介质的耐电压水平。添加适量的ZnO(氧化锌)、MnCO3 (碳酸锰)掺杂后,能够降低介质的介质损耗。适量的W2O3(三氧化二钨)掺杂改性,W2O3在晶体中因为W的化合价是+3价,引起晶体形变,形成极化,从而提高介质的介电常数。
优选上述BaTiO3、BaZrO3分别是采用常规的化学原料以固相法合成。
上述BaTiO3可采用如下工艺制备:按1:1的摩尔比配备BaCO3和TiO2,然后对BaCO3和TiO2进行研磨并混合均匀,再将BaCO3和TiO2的混合物料放入氧化铝坩埚内,于1260℃下保温180分钟,得到BaTiO3。优选采用行星球磨机对BaCO3和TiO2的混合物料进行球磨,被球磨的混合物料、所用球、所用水的重量比例为:混合物料:球:水=1:5:1.5,球磨过程持续3小时以上(如3-6小时);球磨完成后对混合物料进行烘干并过80目筛,再将混合物料放入氧化铝坩埚内。水可采用蒸馏水或去离子水。上述BaCO3的纯度通常达到99.7%以上;TiO2的纯度通常达到99.5%以上。
上述BaZrO3可采用如下工艺制备:按1:1的摩尔比配备BaCO3和ZrO2,然后对BaCO3和ZrO2进行研磨并混合均匀,再将BaCO3和ZrO2的混合物料放入氧化铝坩埚内,于1330℃下保温180分钟,得到BaZrO3。优选采用行星球磨机对BaCO3和ZrO2的混合物料进行球磨,被球磨的混合物料、所用球、所用水的重量比例为:混合物料:球:水=1:5:2,球磨过程持续3小时以上(如3-6小时);球磨完成后对混合物料进行烘干并过80目筛,再将混合物料放入氧化铝坩埚内。水可采用蒸馏水或去离子水。上述BaCO3的纯度通常达到99.7%以上;ZrO2的纯度通常达到99.5%以上。
本发明还提供上述高压低损陶瓷电容器介质的一种制备方法,其特征在于包括下述步骤:
(1)按比例配备BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3
(2)将步骤(1)所配备的BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3混合并采用球磨机进行球磨,然后将球磨获得的料浆转移至砂磨机进行砂磨;
(3)步骤(2)砂磨至料浆中物料粒度D50达到1.0μm时,将料浆转移至搅拌罐中,再加入粘结剂,搅拌均匀后进行烘干造粒,得到粉料;
(4)将步骤(3)得到的粉料压制成生坯片;
(5)将生坯片置于1320-1350℃下保温2-4小时,使生坯片排出粘结剂并烧结,得到所述高压低损陶瓷电容器介质。
得到的高压低损陶瓷电容器介质为陶瓷片,涂刷银电极浆料后在780-850℃下保温15分钟进行烧银,形成银电极,再焊引线,进行包封,即得陶瓷电容器。
优选步骤(2)中,采用行星球磨机对配备好的原料进行球磨,被球磨的原料、所用球、所用水的重量比例为:原料:球:水=1:3:0.5,球磨过程持续5小时以上(如5-8小时)。水可采用蒸馏水或去离子水。
更优选步骤(2)中,进行球磨前向球磨机中加入分散剂,分散剂的用量为步骤(1)所配备原料总重的0.1%。上述分散剂可采用铵盐分散剂。
步骤(3)的粘结剂可采用聚乙烯醇水溶液(即PVA溶液)。优选步骤(3)的粘结剂采用重量百分比浓度为10%的聚乙烯醇溶液,所加入的聚乙烯醇溶液的重量为料浆干重的30%(即粘结剂所含聚乙烯醇的重量为步骤(1)所配备原料总重的3%)。
优选步骤(4)中,对粉料进行干压成型,得到生坯片。
本发明与现有技术相比,具有如下优点:本发明的陶瓷电容器介质的介电常数高(介电常数为3400以上),耐电压高(直流耐电压可达7kV/mm以上,交流耐压可达5kV/mm以上),介质损耗小(介质损耗小于0.8%)。本发明的陶瓷电容器介质适合于制造满足Y5P特性要求的陶瓷电容器。而且,本发明的陶瓷电容器介质不含铋(氧化铋在高温烧结过程中易挥发,会造成对设备和环境的污染,另外还会影响介质中铋含量的准确性),在制备和使用过程中对环境无污染。
具体实施方式
实施例1
首先,以固相法合成BaTiO3、BaZrO3
BaTiO3采用如下工艺制备:按1:1的摩尔比配备BaCO3和TiO2,然后对BaCO3和TiO2进行研磨并混合均匀(采用行星球磨机对BaCO3和TiO2的混合物料进行球磨,被球磨的混合物料、所用球、所用水的重量比例为:混合物料:球:水=1:5:1.5,球磨过程持续4小时;球磨完成后对混合物料进行烘干并过80目筛),再将BaCO3和TiO2的混合物料放入氧化铝坩埚内,于1260℃下保温180分钟,得到BaTiO3
BaZrO3采用如下工艺制备:按1:1的摩尔比配备BaCO3和ZrO2,然后对BaCO3和ZrO2进行研磨并混合均匀(采用行星球磨机对BaCO3和ZrO2的混合物料进行球磨,被球磨的混合物料、所用球、所用水的重量比例为:混合物料:球:水=1:5:2,球磨过程持续4小时;球磨完成后对混合物料进行烘干并过80目筛),再将BaCO3和ZrO2的混合物料放入氧化铝坩埚内,于1330℃下保温180分钟,得到BaZrO3
然后,按下述步骤制备高压低损陶瓷电容器介质:
(1)按比例配备BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3
本实施例中配备的各种原料的重量百分比如下:BaTiO89.9%,BaZrO3 5.5%,CeO2 0.5%,ZnO 0.8%,MnCO3 0.3%,La2O3 1.8%,W2O3 1.2%;
(2)将步骤(1)所配备的BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3混合并采用球磨机进行球磨,然后将球磨获得的料浆转移至砂磨机进行砂磨;
本步骤(2)中,采用行星球磨机对配备好的原料进行球磨,被球磨的原料、所用球、所用水的重量比例为:原料:球:水=1:3:0.5,球磨过程持续5小时;
本步骤(2)中,进行球磨前向球磨机中加入分散剂(分散剂采用铵盐分散剂),分散剂的用量为步骤(1)所配备原料总重的0.1%;
(3)步骤(2)砂磨至料浆中物料粒度D50达到1.0μm时,将料浆转移至搅拌罐中,再加入粘结剂,搅拌均匀后进行烘干造粒,得到粉料;
本步骤(3)的粘结剂采用重量百分比浓度为10%的聚乙烯醇溶液,所加入的聚乙烯醇溶液的重量为料浆干重的30%(即粘结剂所含聚乙烯醇的重量为步骤(1)所配备原料总重的3%);
(4)将步骤(3)得到的粉料压制成生坯片(对粉料进行干压成型,得到生坯片);
(5)将生坯片置于1350℃下保温2.5小时,使生坯片排出粘结剂并烧结,得到所述高压低损陶瓷电容器介质。
得到的高压低损陶瓷电容器介质为陶瓷片,涂刷银电极浆料后在800℃下保温15分钟进行烧银,形成银电极,再焊引线,进行包封,即得陶瓷电容器。
实施例2
首先,以固相法合成BaTiO3、BaZrO3
本实施例中BaTiO3、BaZrO3的制备工艺与实施例1相同。
然后,按下述步骤制备高压低损陶瓷电容器介质:
(1)按比例配备BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3
本实施例中配备的各种原料的重量百分比如下:BaTiO3 89%,BaZrO3 6%, CeO20.6%,ZnO 1%,MnCO3 0.4%,La2O3 2%,W2O3 1%;
(2)将步骤(1)所配备的BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3混合并采用球磨机进行球磨,然后将球磨获得的料浆转移至砂磨机进行砂磨;
本步骤(2)中,采用行星球磨机对配备好的原料进行球磨,被球磨的原料、所用球、所用水的重量比例为:原料:球:水=1:3:0.5,球磨过程持续6小时;
本步骤(2)中,进行球磨前向球磨机中加入分散剂(分散剂采用铵盐分散剂),分散剂的用量为步骤(1)所配备原料总重的0.1%;
(3)步骤(2)砂磨至料浆中物料粒度D50达到1.0μm时,将料浆转移至搅拌罐中,再加入粘结剂,搅拌均匀后进行烘干造粒,得到粉料;
本步骤(3)的粘结剂采用重量百分比浓度为10%的聚乙烯醇溶液,所加入的聚乙烯醇溶液的重量为料浆干重的30%(即粘结剂所含聚乙烯醇的重量为步骤(1)所配备原料总重的3%);
(4)将步骤(3)得到的粉料压制成生坯片(对粉料进行干压成型,得到生坯片);
(5)将生坯片置于1330℃下保温3小时,使生坯片排出粘结剂并烧结,得到所述高压低损陶瓷电容器介质。
得到的高压低损陶瓷电容器介质为陶瓷片,在820℃下保温15分钟进行烧银,形成银电极,再焊引线,进行包封,即得陶瓷电容器。
实施例3
首先,以固相法合成BaTiO3、BaZrO3
本实施例中BaTiO3、BaZrO3的制备工艺与实施例1相同。
然后,按下述步骤制备高压低损陶瓷电容器介质:
(1)按比例配备BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3
本实施例中配备的各种原料的重量百分比如下:BaTiO88.2%,BaZrO3 7%, CeO20.5%,ZnO 1.2%,MnCO3 0.5%,La2O3 1.8%,W2O3 0.8%;
(2)将步骤(1)所配备的BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3混合并采用球磨机进行球磨,然后将球磨获得的料浆转移至砂磨机进行砂磨;
本步骤(2)中,采用行星球磨机对配备好的原料进行球磨,被球磨的原料、所用球、所用水的重量比例为:原料:球:水=1:3:0.5,球磨过程持续5.5小时;
本步骤(2)中,进行球磨前向球磨机中加入分散剂(分散剂采用铵盐分散剂),分散剂的用量为步骤(1)所配备原料总重的0.1%;
(3)步骤(2)砂磨至料浆中物料粒度D50达到1.0μm时,将料浆转移至搅拌罐中,再加入粘结剂,搅拌均匀后进行烘干造粒,得到粉料;
本步骤(3)的粘结剂采用重量百分比浓度为10%的聚乙烯醇溶液,所加入的聚乙烯醇溶液的重量为料浆干重的30%(即粘结剂所含聚乙烯醇的重量为步骤(1)所配备原料总重的3%);
(4)将步骤(3)得到的粉料压制成生坯片(对粉料进行干压成型,得到生坯片);
(5)将生坯片置于1320℃下保温4小时,使生坯片排出粘结剂并烧结,得到所述高压低损陶瓷电容器介质。
得到的高压低损陶瓷电容器介质为陶瓷片,在850℃下保温15分钟进行烧银,形成银电极,再焊引线,进行包封,即得陶瓷电容器。
以上各实施例制得陶瓷电容器后,测试其性能,各实施例陶瓷电容器介质的性能如表1所示。从表1可以看出,所制备的电容器陶瓷耐电压高(直流耐电压可达7kV/mm以上,交流耐压可达5kV/mm以上),介电常数为3400以上,介质损耗小于0.8%,制得的陶瓷电容器的温度特性符合Y5P特性的要求。其中实施例2综合性能最优(主要是耐电压高)。
表1本发明各实施例制得的陶瓷电容器介质的性能

Claims (10)

1.一种高压低损陶瓷电容器介质,其特征在于由下述重量配比的原料制成: BaZrO3 5-7%, CeO2 0.5-0.7%,ZnO 0.8-1.2%,MnCO3 0.3-0.5%,La2O3 1.5-2.5%,W2O3 0.8-1.2%,余量为BaTiO3
2.根据权利要求1所述的高压低损陶瓷电容器介质,其特征在于所述高压低损陶瓷电容器介质由下述重量配比的原料制成:BaTiO3 89%,BaZrO3 6%, CeO2 0.6%,ZnO 1%,MnCO30.4%,La2O3 2%,W2O3 1%。
3.根据权利要求1或2所述的高压低损陶瓷电容器介质,其特征在于所述BaTiO3采用如下工艺制备:按1:1的摩尔比配备BaCO3和TiO2,然后对BaCO3和TiO2进行研磨并混合均匀,再将BaCO3和TiO2的混合物料放入氧化铝坩埚内,于1260℃下保温180分钟,得到BaTiO3
4.根据权利要求1或2所述的高压低损陶瓷电容器介质,其特征在于所述BaZrO3采用如下工艺制备:按1:1的摩尔比配备BaCO3和ZrO2,然后对BaCO3和ZrO2进行研磨并混合均匀,再将BaCO3和ZrO2的混合物料放入氧化铝坩埚内,于1330℃下保温180分钟,得到BaZrO3
5.权利要求1或2所述的高压低损陶瓷电容器介质的制备方法,其特征在于包括下述步骤:
(1)按比例配备BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3
(2)将步骤(1)所配备的BaTiO3、BaZrO3、CeO2、ZnO、MnCO3、La2O3和W2O3混合并采用球磨机进行球磨,然后将球磨获得的料浆转移至砂磨机进行砂磨;
(3)步骤(2)砂磨至料浆中物料粒度D50达到1.0μm时,将料浆转移至搅拌罐中,再加入粘结剂,搅拌均匀后进行烘干造粒,得到粉料;
(4)将步骤(3)得到的粉料压制成生坯片;
(5)将生坯片置于1320-1350℃下保温2-4小时,使生坯片排出粘结剂并烧结,得到所述高压低损陶瓷电容器介质。
6.根据权利要求5所述的高压低损陶瓷电容器介质的制备方法,其特征是:步骤(2)中,采用行星球磨机对配备好的原料进行球磨,被球磨的原料、所用球、所用水的重量比例为:原料:球:水=1:3:0.5,球磨过程持续5-8小时。
7.根据权利要求6所述的高压低损陶瓷电容器介质的制备方法,其特征是:步骤(2)中,进行球磨前向球磨机中加入分散剂,分散剂的用量为步骤(1)所配备原料总重的0.1%。
8.根据权利要求7所述的高压低损陶瓷电容器介质的制备方法,其特征是:所述分散剂采用铵盐分散剂。
9.根据权利要求5所述的高压低损陶瓷电容器介质的制备方法,其特征是:步骤(3)的粘结剂采用重量百分比浓度为10%的聚乙烯醇溶液,所加入的聚乙烯醇溶液的重量为料浆干重的30%。
10.根据权利要求5所述的高压低损陶瓷电容器介质的制备方法,其特征是:步骤(4)中,对粉料进行干压成型,得到生坯片。
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0865052A2 (en) * 1997-02-25 1998-09-16 TDK Corporation High dielectric-constant ceramic composition, and its fabrication process
JP2003277137A (ja) * 2002-03-26 2003-10-02 Tdk Corp 高誘電率誘電体磁器組成物
CN101265087A (zh) * 2007-03-14 2008-09-17 Tdk株式会社 电介质陶瓷组合物以及电子部件
CN103803969A (zh) * 2013-12-15 2014-05-21 赵华 一种y5u组别电子陶瓷介质材料及制备方法
JP2016216270A (ja) * 2015-05-14 2016-12-22 サムソン エレクトロ−メカニックス カンパニーリミテッド. 誘電体磁器組成物およびその製造方法、ならびにセラミック電子部品
TW201704187A (zh) * 2015-07-16 2017-02-01 國立臺北科技大學 陶瓷電容介電材料

Family Cites Families (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH06102573B2 (ja) * 1988-07-01 1994-12-14 日本油脂株式会社 還元再酸化型半導体セラミックコンデンサ用組成物
DE4130438C2 (de) * 1991-09-13 1999-12-09 Philips Patentverwaltung Verfahren zur Herstellung verformter Dielektrika auf Basis keramischer Massen des Systems BaTiO¶3¶-ZrO¶2¶-CeO¶2¶
KR100250228B1 (ko) * 1997-12-17 2000-04-01 김충환 세라믹 콘덴서용 유전체 조성물 및 그 제조방법
CN1762899A (zh) * 2004-10-21 2006-04-26 天津大学 温度稳定型高介电常数陶瓷介质材料及其制造方法
JP4967963B2 (ja) * 2007-09-28 2012-07-04 Tdk株式会社 誘電体磁器組成物および電子部品
JP4710908B2 (ja) * 2008-01-10 2011-06-29 Tdk株式会社 誘電体磁器組成物および電子部品
JP5018604B2 (ja) * 2008-03-31 2012-09-05 Tdk株式会社 誘電体磁器組成物および電子部品
CN102101775B (zh) * 2010-12-08 2013-03-13 汕头高新区松田实业有限公司 一种低损耗高压陶瓷电容器介质
CN102531592B (zh) * 2011-11-10 2014-10-29 厦门万明电子有限公司 一种抗还原的y5p陶瓷电容器介质瓷料
JP6091881B2 (ja) * 2012-03-19 2017-03-08 セイコーインスツル株式会社 BaTi2O5系複合酸化物の製造方法
CN104496465B (zh) * 2014-12-02 2016-09-07 佛山铭乾科技有限公司 一种微波介质陶瓷材料及其制备方法
CN106518067A (zh) * 2016-10-27 2017-03-22 盐城工学院 一种陶瓷组合物、陶瓷及其制备方法和应用
CN108585834A (zh) * 2018-06-21 2018-09-28 江苏田字格新材料科技有限公司 高介电常数陶瓷粉料及所制得的陶瓷电容器及制造方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0865052A2 (en) * 1997-02-25 1998-09-16 TDK Corporation High dielectric-constant ceramic composition, and its fabrication process
JP2003277137A (ja) * 2002-03-26 2003-10-02 Tdk Corp 高誘電率誘電体磁器組成物
CN101265087A (zh) * 2007-03-14 2008-09-17 Tdk株式会社 电介质陶瓷组合物以及电子部件
CN103803969A (zh) * 2013-12-15 2014-05-21 赵华 一种y5u组别电子陶瓷介质材料及制备方法
JP2016216270A (ja) * 2015-05-14 2016-12-22 サムソン エレクトロ−メカニックス カンパニーリミテッド. 誘電体磁器組成物およびその製造方法、ならびにセラミック電子部品
TW201704187A (zh) * 2015-07-16 2017-02-01 國立臺北科技大學 陶瓷電容介電材料

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