CN106587988A - 一种高温度稳定陶瓷电容器介质 - Google Patents

一种高温度稳定陶瓷电容器介质 Download PDF

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CN106587988A
CN106587988A CN201610998071.4A CN201610998071A CN106587988A CN 106587988 A CN106587988 A CN 106587988A CN 201610998071 A CN201610998071 A CN 201610998071A CN 106587988 A CN106587988 A CN 106587988A
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ceramic capacitor
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capacitor dielectric
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CN106587988B (zh
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黄新友
陈磊
高春华
李军
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Jiangsu University
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Abstract

本发明涉及无机非金属材料技术领域，特指一种高温度稳定陶瓷电容器介质。介质配方组成，按照重量百分比计算：BaTiO3 55‑90％，SrTiO3 2‑25％，CaZrO32‑15％，BiLiTiSiO6 0.5‑6％，(Li1/2La1/2)TiO3 0.1‑8.5％，WO30.1‑0.8％，MnO20.03‑1.0％。本介质的介电常数高，为5800以上；耐电压高，直流耐电压可达15kV/mm以上；介质损耗小，小于0.4％；本介质的介电常数较高，能实现陶瓷电容器的小型化和大容量,同样能降低成本。

Description

一种高温度稳定陶瓷电容器介质
技术领域
本发明涉及无机非金属材料技术领域，特指一种高温度稳定陶瓷电容器介质；它采用常规的陶瓷电容器介质制备方法，利用电容器陶瓷普通化学原料，制备得到无铅、无镉的高介高温度稳定陶瓷电容器介质，还能降低电容器陶瓷的烧结温度，该介质适合于制备单片陶瓷电容器，能大大降低陶瓷电容器的成本,同时能提高温度稳定性以扩大陶瓷电容器的应用范围，并且在制备和使用过程中不污染环境。
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、温度稳定性好、可靠性高、小型化、大容量的陶瓷电容器。一般单片高压陶瓷电容器介质的烧结温度为1350～1430℃，而本发明的陶瓷电容器介质烧结温度为1200～1230℃，这样能大大降低高压陶瓷电容器的成本，同时本专利电容器陶瓷介质不含铅和镉，电容器陶瓷在制备和使用过程中不污染环境；另外，本发明的电容器陶瓷的介电常数较高，这样会提高陶瓷电容器的容量并且小型化，符合陶瓷电容器的发展趋势,同样也会降低陶瓷电容器的成本。
通常用于生产高压陶瓷电容器的介质中含有一定量的铅，这不仅在生产、使用和废弃过程中对人体和环境造成危害，而且对性能稳定性也有不良影响。
中国期刊《电子元件与材料》1989年第5期在“高介高压2B4介质陶瓷”一文中公开了一种高压陶瓷电容器介质材料，该介质材料采用97.8wt.％BaTiO3+0.8wt.％Bi2O3+0.7wt.％Nb2O5+0.5wt.％CeO2+0.2wt.％MnO2的配方，以常规的工艺制备试样，其介电常数ε＝2500～2600，tgδ＝0.5-1.4％,直流耐压强度为7KV/mm。该介质虽属无铅介质材料，但它存在耐压性较差，介电常数太小。配方组成不同于本专利。
中国专利“一种高压陶瓷电容器介质”(专利号ZL00112050.6)公开的电容器陶瓷介质虽属无铅介质材料，但介电常数为1860-3300，耐电压可以达到10kV/mm以上(直流)，烧结温度为1260-1400℃，比本专利高。介电常数太小，远低于本专利，而且配方组成不同于本专利。
中国期刊《江苏陶瓷》1999年第2期在“BaTiO3系低温烧成高介X7R电容器瓷料”一文中公开了一种BaTiO3中低温烧成高介满足X7R特性的电容器瓷料，该介质材料的配方组成为(质量百分数)：(BaTiO3+Nd2O3)89％～92％+Bi2O3·2TiO27.5～10％+低熔点玻璃料0.8％+50％Mn(NO3)2(水溶液)0.205％。其中，所用的低熔点玻璃料是硼硅酸铅低熔点玻璃，介质是含铅的，并且未涉及耐电压,介电常数小于3500,远小于本专利的介电常数,介质的配方组成也不同于本发明专利。
另有专利“一种低损耗高压陶瓷电容器介质”(专利申请号：201010588021.1)，该专利的介质虽然介电损耗低，但是容量温度特性较差，不符合X7R特性，介电常数比本专利的低，配方不同于本专利。
另有专利“高压陶瓷电容器介质的制造方法”(专利号：91101958.8),其采用非常规工艺制备介质,即流延成型膜,然后叠层介质体,将多层介质体进行真空加热匀压、冲片、然后进行排胶、烧成而得。该专利的缺点是制备工艺方法复杂、导致产品制造成本增加，按其介质配方制造所得的高压电容器陶瓷的介电常数为1800-7200，介电常数太小，容量温度特性不符合X7R特性，配方不同于本专利。
还有专利“一种陶瓷电容器的电介质及其制备方法”(专利申请号：201010538725.8)，该专利的介质虽然介电常数很高，但容温特性较差，不符合X7R特性，配方不同于本专利。
发明内容
本发明的目的是提供一种高温度稳定陶瓷电容器介质。
本发明的目的是这样来实现的：
高温度稳定陶瓷电容器介质配方组成，按照重量百分比计算：BaTiO3 55-90％，SrTiO3 2-25％，CaZrO3 2-15％，BiLiTiSiO6 0.5-6％，(Li1/2La1/2)TiO3 0.1-8.5％，WO30.1-0.8％，MnO2 0.03-1.0％；其中BaTiO3、SrTiO3、CaZrO3、BiLiTiSiO6、(Li1/2La1/2)TiO3分别是采用常规的化学原料以固相法合成。
本发明的介质中所用的BiLiTiSiO6是采用如下工艺制备的：将常规的化学原料Bi2O3、Li2CO3、TiO2、SiO2按1/2：1/2：1：1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于810℃保温240分钟，然后冷却，固相反应合成BiLiTiSiO6，冷却后研磨过200目筛，备用。
本发明的介质中所用的(Li1/2La1/2)TiO3的制备过程如下：将常规的化学原料Li2CO3和La2O3和TiO2按1/4：1/4：1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于1000℃-1030℃保温120分钟，固相反应合成(Li1/2La1/2)TiO3，冷却后研磨过200目筛，备用。
本发明采用常规的高压陶瓷电容器介质制备工艺，即首先采用常规的化学原料用固相法分别合成BaTiO3、SrTiO3、CaZrO3、BiLiTiSiO6、(Li1/2La1/2)TiO3，然后按配方配料，将配合料球磨、粉碎、混合，进行烘干后，加入粘合剂造粒，再压制成生坯片，然后在空气中进行排胶和烧结，经保温并自然冷却后，获得陶瓷电容器介质，在介质上被电极即成。
上述陶瓷介质的配方最好采用下列三种方案(重量百分比)：
BaTiO360-86％,SrTiO33-22％,CaZrO33-12％,BiLiTiSiO60.5-6％,(Li1/2La1/2)TiO30.2-6.7％,WO30.1-0.8％,MnO20.03-1.0％。
BaTiO3 65-83％,SrTiO3 3-19％,CaZrO3 4-10％,BiLiTiSiO6 1-6％,(Li1/2La1/2)TiO30.2-5.2％,WO30.1-0.8％,MnO20.03-1.0％。
BaTiO370-81％,SrTiO34-17％,CaZrO33-8％,BiLiTiSiO6 1-5％,(Li1/2La1/2)TiO30.2-4.7％,WO3 0.1-0.8％,MnO20.03-1.0％。
本发明与现有技术相比，具有如下优点：
1、本专利的介质是烧结温度较低(烧结温度1200～1230℃)钛酸钡锶基电容器陶瓷，这样能大大降低高压陶瓷电容器的成本，本专利的介质组分中不含铅和镉，对环境无污染。
2、本介质的介电常数高，为5800以上；耐电压高，直流耐电压可达15kV/mm以上；介质损耗小，小于0.4％；本介质的介电常数较高，能实现陶瓷电容器的小型化和大容量,同样能降低成本。
3、本介质的电容温度变化率小，容温特性符合X7R特性的要求；介质损耗小于0.4％,使用过程中性能稳定性好，安全性高。
4、主要原料采用陶瓷电容器级纯即可制造出本发明的陶瓷介质。
5、本介质采用常规的固相法陶瓷电容器介质制备工艺即可进行制备。
具体实施方式
现在结合实施例对本发明作进一步的描述。表1给出本发明的实施例共9个试样的配方。
本发明的实施例共9个试样的配方的主要原料采用陶瓷电容器级纯，在制备时首先采用常规的化学原料用固相法分别合成BaTiO3、SrTiO3、CaZrO3、BiLiTiSiO6、(Li1/2La1/2)TiO3，然后按上述配方配料,将配好的料用蒸馏水或去离子水采用行星球磨机球磨混合，料:球:水＝1:3:(0.6～1.0)(质量比)，球磨4～8小时后，烘干得干粉料，在干粉料中加入占其重量8～10％的浓度为10wt％的聚乙烯醇溶液，进行造粒，混研后过40目筛，再在20～30Mpa压力下进行干压成生坯片，然后在烧结温度为1200～1230℃下保温1～4小时进行排胶和烧结，再在780～870℃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，测试其介电性能。上述各配方试样的介电性能列于表2。从表2可以看出所制备的电容器陶瓷耐电压高，可达15kV/mm(直流电压,DC)以上；介电常数为5800以上；介质损耗小于0.4％；电容温度变化率小，符合X7R特性的要求。
表1本发明的实施例共9个试样的配方(重量百分比)
表2各配方试样的介电性能
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，凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明的保护范围之内。

Claims (7)

1.一种高温度稳定陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：BaTiO3 55-90％，SrTiO3 2-25％，CaZrO3 2-15％，BiLiTiSiO6 0.5-6％，(Li1/2La1/2)TiO30.1-8.5％，WO30.1-0.8％，MnO2 0.03-1.0％；其中BaTiO3、SrTiO3、CaZrO3、BiLiTiSiO6、(Li1/2La1/2)TiO3分别是采用常规的化学原料以固相法合成。
2.如权利要求1所述的一种高温度稳定陶瓷电容器介质，其特征在于：所述的BiLiTiSiO6是采用如下工艺制备的：将常规的化学原料Bi2O3、Li2CO3、TiO2、SiO2按1/2：1/2：1：1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于810℃保温240分钟，然后冷却，固相反应合成BiLiTiSiO6，冷却后研磨过200目筛，备用。
3.如权利要求1所述的一种高温度稳定陶瓷电容器介质，其特征在于：所述的(Li1/ 2La1/2)TiO3的制备过程如下：将常规的化学原料Li2CO3和La2O3和TiO2按1/4：1/4：1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于1000℃-1030℃保温120分钟，固相反应合成(Li1/ 2La1/2)TiO3，冷却后研磨过200目筛，备用。
4.如权利要求1所述的一种高温度稳定陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：BaTiO360-86％,SrTiO33-22％,CaZrO33-12％,BiLiTiSiO60.5-6％,(Li1/2La1/2)TiO30.2-6.7％,WO30.1-0.8％,MnO20.03-1.0％。
5.如权利要求1所述的一种高温度稳定陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：BaTiO3 65-83％,SrTiO3 3-19％,CaZrO3 4-10％,BiLiTiSiO6 1-6％,(Li1/2La1/2)TiO30.2-5.2％,WO30.1-0.8％,MnO20.03-1.0％。
6.如权利要求1所述的一种高温度稳定陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：BaTiO370-81％,SrTiO34-17％,CaZrO33-8％,BiLiTiSiO6 1-5％,(Li1/2La1/2)TiO3 0.2-4.7％,WO3 0.1-0.8％,MnO20.03-1.0％。
7.如权利要求1所述的一种高温度稳定陶瓷电容器介质的制备方法，其特征在于：首先采用常规的化学原料用固相法分别合成BaTiO3、SrTiO3、CaZrO3、BiLiTiSiO6、(Li1/2La1/2)TiO3，然后按上述配方配料,将配好的料用蒸馏水或去离子水采用行星球磨机球磨混合，料、球和水的质量比＝1:3:(0.6～1.0)，球磨4～8小时后，烘干得干粉料，在干粉料中加入占其重量8～10％的浓度为10wt％的聚乙烯醇溶液，进行造粒，混研后过40目筛，再在20～30Mpa压力下进行干压成生坯片，然后在烧结温度为1200～1230℃下保温1～4小时进行排胶和烧结，再在780～870℃下保温15分钟进行烧银，形成银电极，再焊引线，进行包封，即得陶瓷电容器介质。
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