CN106565238B - 一种低温烧结高压陶瓷电容器介质 - Google Patents

一种低温烧结高压陶瓷电容器介质 Download PDF

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CN106565238B
CN106565238B CN201611005233.6A CN201611005233A CN106565238B CN 106565238 B CN106565238 B CN 106565238B CN 201611005233 A CN201611005233 A CN 201611005233A CN 106565238 B CN106565238 B CN 106565238B
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黄新友
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，特指一种低温烧结高压陶瓷电容器介质，介质配方组成，按照重量百分比计算：按照重量百分比：BaTiO360‑91％,SrTiO31‑13％,Li2ZrO3 2‑15％,Nb2O5 0.05‑1％,ZnO 0.1‑1.5％,Co2O3 0.03‑1.0％,ZnB2O4玻璃粉0.5‑6％,Bi2TiSiO7 0.5‑5％。本介质的介电常数较高，为3820左右；耐电压高，直流耐电压可达15kV/mm以上、7.2kV/mm(交流电压，AC)以上；介质损耗小，小于1.3％。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

一种低温烧结高压陶瓷电容器介质
技术领域
本发明涉及无机非金属材料技术领域，特指一种低温烧结(烧结温度为880～900℃)高压陶瓷电容器介质，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、无镉的高介高压陶瓷电容器介质，还能大大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和多层片式陶瓷电容器，能大大降低陶瓷电容器的成本，同时能提高耐电压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1300～1400℃，而本发明的陶瓷电容器介质烧结温度为880～900℃，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，烧结温度低，符合陶瓷电容器的发展趋势,能大大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℃，比本专利高很多，介电常数低于本专利，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，烧结温度最低为1080℃，比本专利高，介质的配方组成也不同于本发明专利。
中国期刊《华南理工大学学报(自然科学版)》1996年第3期在“中温烧结BaTiO3基多相铁电瓷料X7R特性”一文中探讨了BaTiO3基瓷料中温烧结机制，分析了中温烧结BaTiO3基瓷料的组成及不均匀结构分布对介电常数与温度特性的影响，所用的BaTiO3原料是采用化学共沉淀的方法来制备的，这样会增加陶瓷电容器的成本，而本专利所用的BaTiO3、SrTiO3、CaZrO3分别是采用常规的化学原料以固相法合成，组成不同于本专利，组分中含有一定量的铅，并且未涉及耐电压，烧结温度最低为1050℃，比本专利高。
另有专利“高介高性能中温烧结片式多层瓷介电容器瓷料”(专利申请号：97117286.2)，它是采用固相法合成等价和异价离子同时取代(Sr2+,Zr4+,Sn4+,Nb5+)BaTiO3固溶体，加入适量的硼铅锌铜玻璃烧结剂，使瓷料在中温烧结，其性能为：介电常数大于等于16000，耐压为700V/mm，该专利虽然介电常数高，但是所报道的材料的耐压太差，仅为700V/mm,另外其组分含有一定量的铅，该专利烧结温度为1080～1140℃，比本专利高。
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，该专利介质的烧结温度为1080-1330℃，比本专利的高。
还有中国专利“高性能中温烧结片式多层瓷介电容器瓷料”(专利申请号：97117287.0)，它采用独特的配方(重量百分比)(BaTiO393～96％+Nb2O50.8～1.5％+Bi2O31.0～2.2％+助熔剂1.8～3.5％+改性剂0.25～1.0％)得到中温烧结的满足如下性能的电容器陶瓷：介电常数为3000，介质损耗小于1.5％，耐压为860V/mm，该专利的助熔剂含有一定量的铅，该专利的耐电压太差，同时介电常数低，小于本专利，该介质的烧结温度为1100～1140℃，比本专利的高。
还有中国专利“一种中低温烧结高压陶瓷电容器介质”(专利申请号：200410041863.x),它采用独特的配方(重量百分比)(BaTiO3 60-90％，SrTiO3 1-20％CaZrO30.1-10％,Nb2O50.01-1％,MgO0.01-1％,CeO20.01-0.8％,ZnO0.01-0.6％,Co2O30.03-1％,铋锂固溶体0.05-10％)得到中温烧结的满足如下性能的电容器陶瓷：介电常数为2000～3000，耐电压为6kV/mm以上,降低烧结温度的添加物是铋锂固溶体，该专利的介电常数和耐电压没有本专利高，该专利公布的电容器陶瓷烧结温度为1100～1150℃，比本专利高，该专利的配方组成不同于本专利。
还有专利“一种低温烧结的高压陶瓷电容器介质”(专利申请号：201110056685.8)，该专利的介质性能不如本专利的介质的性能，该专利的烧结温度为930-980℃，比本专利的高。该专利的配方组成不同于本专利。
发明内容
本发明的目的是提供一种低温烧结高压陶瓷电容器介质。
本发明的目的是这样来实现的：
低温烧结高压陶瓷电容器介质配方组成，按照重量百分比：BaTiO360-91％,SrTiO31-13％,Li2ZrO3 2-15％,Nb2O5 0.05-1％,ZnO 0.1-1.5％,Co2O3 0.03-1.0％,ZnB2O4玻璃粉0.5-6％,Bi2TiSiO7 0.5-5％；其中BaTiO3、SrTiO3、Li2ZrO3、ZnB2O4玻璃粉、Bi2TiSiO7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ZnB2O4玻璃粉的制备过程包括：将常规的化学原料ZnO、B2O3按1：1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于820℃保温120分钟，在水中急冷后研磨过200目筛，备用。
本发明的介质中所用的Bi2TiSiO7的制备过程包括：将常规的化学原料Bi2O3、TiO2、SiO2按1：1：1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，研磨过200目筛，备用。
本发明的介质中所用的Li2ZrO3的制备过程包括：将常规的化学原料Li2CO3、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830℃保温240分钟，然后冷却，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、Li2ZrO3、ZnB2O4玻璃粉、Bi2TiSiO7,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)：
BaTiO367-82％,SrTiO33-10％,Li2ZrO33-11％,Nb2O50.5-0.8％,ZnO0.3-0.7％，Co2O3 0.3-0.7％，ZnB2O4玻璃粉1-5％，Bi2TiSiO7 1-5％。
BaTiO370-85％,SrTiO33-10％,Li2ZrO33-8％,Nb2O50.5-0.8％,ZnO0.3-0.7％，Co2O3 0.5-0.7％，ZnB2O4玻璃粉2-5％，Bi2TiSiO7 2-5％。
BaTiO373-88％,SrTiO33-10％,Li2ZrO33-8％,Nb2O50.5-0.8％,ZnO0.3-0.7％,Co2O3 0.3-0.7％,ZnB2O4玻璃粉2-5％，Bi2TiSiO7 2-5％。
本发明与现有技术相比，具有如下优点：
1、本专利的介质是低温烧结(烧结温度为880～900℃)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、本介质的介电常数较高，为3820左右；耐电压高，直流耐电压可达15kV/mm以上、7.2kV/mm(交流电压，AC)以上；介质损耗小，小于1.3％。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，符合X7R特性的要求。介质损耗小于1.3％,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、Li2ZrO3、ZnB2O4玻璃粉和Bi2TiSiO7,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，然后在温度为880～900℃下保温1～4小时进行排胶和烧结，再在780～800℃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，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、7.2kV/mm以上(交流电压，AC)以上；介电常数为3820以上；介质损耗小于1.3％；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
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 (8)

1.一种低温烧结高压陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：BaTiO360-91％,SrTiO3 1-13％,Li2ZrO3 2-15％,Nb2O5 0.05-1％,ZnO 0.1-1.5％,Co2O30.03-1.0％,ZnB2O4玻璃粉0.5-6％,Bi2TiSiO7 0.5-5％；其中BaTiO3、SrTiO3、Li2ZrO3、ZnB2O4玻璃粉、Bi2TiSiO7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所述的一种低温烧结高压陶瓷电容器介质，其特征在于，所述的ZnB2O4玻璃粉的制备过程包括：将常规的化学原料ZnO、B2O3按1：1摩尔比配料，研磨混合均匀后放入氧化铝坩埚内于820℃保温120分钟，在水中急冷后研磨过200目筛，备用。
3.如权利要求1所述的一种低温烧结高压陶瓷电容器介质，其特征在于，所述的Bi2TiSiO7的制备过程包括：将常规的化学原料Bi2O3、TiO2、SiO2按1：1：1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，研磨过200目筛，备用。
4.如权利要求1所述的一种低温烧结高压陶瓷电容器介质，其特征在于，所述的Li2ZrO3的制备过程包括：将常规的化学原料Li2CO3、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830℃保温240分钟，然后冷却，研磨过200目筛，备用。
5.如权利要求1所述的一种低温烧结高压陶瓷电容器介质，其特征在于，介质配方组成，按照重量百分比计算：BaTiO367-82％,SrTiO33-10％,Li2ZrO33-11％,Nb2O50.5-0.8％,ZnO0.3-0.7％,Co2O30.3-0.7％，ZnB2O4玻璃粉1-5％，Bi2TiSiO7 1-5％。
6.如权利要求1所述的一种低温烧结高压陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：BaTiO370-85％,SrTiO33-10％,Li2ZrO33-8％,Nb2O50.5-0.8％,ZnO0.3-0.7％,Co2O3 0.5-0.7％,ZnB2O4玻璃粉2-5％，Bi2TiSiO7 2-5％。
7.如权利要求1所述的一种低温烧结高压陶瓷电容器介质，其特征在于：介质配方组成，按照重量百分比计算：BaTiO373-88％，SrTiO33-10％,Li2ZrO33-8％，Nb2O50.5-0.8％,ZnO0.3-0.7％，Co2O3 0.3-0.7％，ZnB2O4玻璃粉2-5％，Bi2TiSiO7 2-5％。
8.如权利要求1所述的一种低温烧结高压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、Li2ZrO3、ZnB2O4玻璃粉和Bi2TiSiO7，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，然后在温度为880～900℃下保温1～4小时进行排胶和烧结，再在780～800℃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。
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