CN105967678B - 一种巨介陶瓷电容器介质及其制备方法 - Google Patents
一种巨介陶瓷电容器介质及其制备方法 Download PDFInfo
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- 239000003985 ceramic capacitor Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims description 11
- 229910010252 TiO3 Inorganic materials 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 8
- UPWOEMHINGJHOB-UHFFFAOYSA-N cobalt(III) oxide Inorganic materials O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000005245 sintering Methods 0.000 claims abstract description 7
- 239000013064 chemical raw material Substances 0.000 claims description 9
- 239000004615 ingredient Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 238000010532 solid phase synthesis reaction Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000000498 ball milling Methods 0.000 claims description 4
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 238000003746 solid phase reaction Methods 0.000 claims description 4
- 238000010671 solid-state reaction Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(III) oxide Inorganic materials O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims description 2
- 238000010304 firing Methods 0.000 claims description 2
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 229940068984 polyvinyl alcohol Drugs 0.000 claims description 2
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 2
- 238000003825 pressing Methods 0.000 claims description 2
- 229910000679 solder Inorganic materials 0.000 claims description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 2
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 claims description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims 2
- 239000004411 aluminium Substances 0.000 claims 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 229910000019 calcium carbonate Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000000919 ceramic Substances 0.000 abstract description 19
- 239000002994 raw material Substances 0.000 abstract description 5
- 229910052793 cadmium Inorganic materials 0.000 abstract description 2
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 abstract description 2
- 238000011160 research Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910004247 CaCu Inorganic materials 0.000 description 1
- 229910002966 CaCu3Ti4O12 Inorganic materials 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Abstract
本发明涉及无机非金属材料技术领域,特指一种巨介、电容温度变化率小的陶瓷电容器介质。配方组成包括:Ca0.925Y0.05Cu3Ti4O1291~98wt.%,(Ba0.65Sr0.35)TiO30.1~7.0wt.%,Bi2WO30.01~1wt.%,Ba(Yb1/2Nb1/2)O30.1~4wt.%,Co2O30.01~1.8wt.%。它采用电容器陶瓷普通化学原料,制备得到无铅、无镉的巨介、电容温度变化率小的陶瓷电容器介质,还能大大降低电容器陶瓷的烧结温度。
Description
技术领域
本发明涉及无机非金属材料技术领域,特指一种巨介、电容温度变化率小的陶瓷电容器介质。它采用电容器陶瓷普通化学原料,制备得到无铅、无镉的巨介、电容温度变化率小的陶瓷电容器介质,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和单层片式陶瓷电容器,能大大降低陶瓷电容器的成本,该介质介电常数巨高,容易实现陶瓷电容器的小型化,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
高介电常数为电容性器件的体积微型化提供了可能性。随着电子器件微型化的发展,高介电常数材料在微电子技术中起着越来越重要的作用。钛酸铜钙(CaCu3Ti4O12,简称CCTO)陶瓷是其中一种最具代表性的高介电常数材料。CCTO陶瓷不论单晶还是多晶形态都呈现出异常高的介电常数,近年受到越来越多的关注。CCTO陶瓷具有很多优点,例如介电常数非常大(εr为104)、在比较宽的频率范围和相当广的温度范围内介电常数随频率和温度的变化很小、制备工艺也相当简单,而且介电常数的大小可以通过改变烧结条件来调节,在谐振器、滤波器、存储器等重要电子器件方面具有很大的应用潜力,因此特别引人注目。然而,通常制备的CCTO陶瓷的介质损耗(tanδ值)很大,在实际应用中会导致器件或电路的发热、工作不稳定或信号衰减等问题,不利于其作为电子材料的应用。为了解决CCTO陶瓷介质损耗大的问题,研究者进行了一些研究,但这些研究的结果不是很成功,最终都没有获得综合介电性能指标满足实际应用要求的改性CCTO陶瓷。具体讲,这些尝试不是没有达到足够程度降低介质损耗的目的,就是明显损害了CCTO陶瓷原有的高介电常数特性,致使改性后介电常数很低,或者破坏了CCTO陶瓷原有的低频段介电常数基本不随频率发生变化的优点。因此,寻找出一种既可以保持CCTO陶瓷所具有高介电常数的优点又能显著地降低介质损耗的有效方法,是一个重要的研究课题。
发明内容
本发明的目的是提供一种巨介低容温变化率的陶瓷电容器介质。
本发明的目的是这样来实现的:
巨介低容温变化率的陶瓷电容器介质配方组成包括:Ca0.925Y0.05Cu3Ti4O1291~98wt.%,(Ba0.65Sr0.35)TiO30.1~7.0wt.%,Bi2WO60.01~1wt.%,Ba(Yb1/2Nb1/2)O30.1~4wt.%,Co2O3 0.01~1.8wt.%;其中Ca0.925Y0.05Cu3Ti4O12、(Ba0.65Sr0.35)TiO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3分别是采用常规的化学原料以固相法合成的。
本发明的介质中所用的Ca0.925Y0.05Cu3Ti4O12是采用如下工艺制备的:将常规的化学原料CaCO3、Y2O3、CuO和TiO2按0.925:0.025:3:4摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于900-950℃保温360-540分钟,固相反应合成Ca0.925Y0.05Cu3Ti4O12,冷却后研磨过200目筛,备用。
本发明的介质中所用的Bi2WO6是采用如下工艺制备的:将常规的化学原料Bi2O3和WO3按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于850℃保温120分钟,冷却后得到Bi2WO6,研磨过200目筛,备用。
本发明的介质中所用的Ba(Yb1/2Nb1/2)O3的制备过程包括:将常规的化学原料BaCO3、Yb2O3、Nb2O5按1:1/4:1/4摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1250-1280℃保温120-180分钟,固相反应合成Ba(Yb1/2Nb1/2)O3,冷却后研磨过200目筛,备用。
本发明采用如下的陶瓷介质制备工艺:首先采用常规的化学原料用固相法分别合成Ca0.925Y0.05Cu3Ti4O12、(Ba0.65Sr0.35)TiO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3,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,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二种方案:
Ca0.925Y0.05Cu3Ti4O1292~96wt.%,(Ba0.65Sr0.35)TiO30.1~5.0wt.%,Bi2WO60.01~0.8wt.%,Ba(Yb1/2Nb1/2)O30.1~3.8wt.%,Co2O3 0.03~1.6wt.%。
Ca0.925Y0.05Cu3Ti4O1292~95wt.%,(Ba0.65Sr0.35)TiO30.1~5.5wt.%,Bi2WO60.01~0.8wt.%,Ba(Yb1/2Nb1/2)O30.1~3.5wt.%,Co2O3 0.03~1.5wt.%。
本发明与现有技术相比,具有如下优点:
1、本介质的介电常数高,可以达到205000以上;耐电压高,直流耐电压可达3.5kV/mm以上;介质损耗小,小于0.08,本介质的介电常数高,能实现陶瓷电容器的小型化和大容量,同样能降低成本。
2、本介质的温度系数低,电容温度变化率小,符合X8R特性的要求,介质损耗小于0.08,使用过程中性能稳定性好,安全性高,对环境无污染。
3、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。
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4个试样的配方。
本发明的实施例共4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Ca0.925Y0.05Cu3Ti4O12、(Ba0.6Sr0.4)TiO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3,然后按配方配料,将配好的料用无水乙醇采用行星球磨机球磨混合,料:球:无水乙醇=1:3:(0.6~1.3)(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,然后在温度为1040~1100℃下保温6~10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,即得巨介陶瓷电容器,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较高,直流耐电压可达3.5kV/mm以上;介电常数高,可以达到205000以上;介质损耗小于0.08;电容温度变化率小,符合X8R特性的要求。
表1本发明的实施例共4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 (9)
1.一种巨介陶瓷电容器介质,其特征在于,所述巨介陶瓷电容器介质配方组成为:Ca0.925Y0.05Cu3Ti4O1291~98wt.%,(Ba0.65Sr0.35)TiO30.1~7.0wt.%,Bi2WO60.01~1wt.%,Ba(Yb1/2Nb1/2)O30.1~4wt.%,Co2O3 0.01~1.8wt.%。
2.如权利要求1所述的一种巨介陶瓷电容器介质,其特征在于:所述Ca0.925Y0.05Cu3Ti4O12、(Ba0.65Sr0.35)TiO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3分别是采用常规的化学原料以固相法合成的。
3.如权利要求1或2所述的一种巨介陶瓷电容器介质,其特征在于,所述Ca0.925Y0.05Cu3Ti4O12是采用如下工艺制备的:将常规的化学原料CaCO3、Y2O3、CuO和TiO2按0.925:0.025:3:4摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于900-950℃保温360-540分钟,固相反应合成Ca0.925Y0.05Cu3Ti4O12,冷却后研磨过200目筛,备用。
4.如权利要求1或2所述的一种巨介陶瓷电容器介质,其特征在于,所述的Bi2WO6是采用如下工艺制备的:将常规的化学原料Bi2O3和WO3按1:1摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于850℃保温120分钟,冷却后得到Bi2WO6,研磨过200目筛,备用。
5.如权利要求1或2所述的一种巨介陶瓷电容器介质,其特征在于,所述的Ba(Yb1/ 2Nb1/2)O3的制备过程包括:将常规的化学原料BaCO3、Yb2O3、Nb2O5按1:1/4:1/4摩尔比配料,研磨混合均匀后放入氧化铝坩埚内于1250-1280℃保温120-180分钟,固相反应合成Ba(Yb1/2Nb1/2)O3,冷却后研磨过200目筛,备用。
6.如权利要求1所述的一种巨介陶瓷电容器介质,其特征在于:所述巨介陶瓷电容器介质直流耐电压达3.5kV/mm以上;介电常数高,达205000以上;介质损耗小于0.08;电容温度变化率小,符合X8R特性的要求;烧结温度低,为1040~1100℃。
7.如权利要求1所述的一种巨介陶瓷电容器介质,其特征在于,所述巨介陶瓷电容器介质配方组成为:Ca0.925Y0.05Cu3Ti4O1292~96wt.%,(Ba0.65Sr0.35)TiO30.1~5.0wt.%,Bi2WO60.01~0.8wt.%,Ba(Yb1/2Nb1/2)O30.1~3.8wt.%,Co2O3 0.03~1.6wt.%。
8.如权利要求1所述的一种巨介陶瓷电容器介质,其特征在于,所述巨介陶瓷电容器介质配方组成为:Ca0.925Y0.05Cu3Ti4O1292~95wt.%,(Ba0.65Sr0.35)TiO30.1~5.5wt.%,Bi2WO60.01~0.8wt.%,Ba(Yb1/2Nb1/2)O30.1~3.5wt.%,Co2O3 0.03~1.5wt.%。
9.如权利要求1所述的一种巨介陶瓷电容器介质的制备方法,其特征在于:在制备时首先采用常规的化学原料用固相法分别合成Ca0.925Y0.05Cu3Ti4O12、(Ba0.65Sr0.35)TiO3、Bi2WO6、Ba(Yb1/2Nb1/2)O3,然后按配方配料,将配好的料用无水乙醇采用行星球磨机球磨混合,料、球和无水乙醇的质量比为1:3:0.6~1.3,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1040~1100℃下保温6~10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,即得巨介陶瓷电容器介质。
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