CN106631005A - 中温烧结的无铅高压电容器介质瓷料及制备方法 - Google Patents

中温烧结的无铅高压电容器介质瓷料及制备方法 Download PDF

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CN106631005A
CN106631005A CN201710018252.0A CN201710018252A CN106631005A CN 106631005 A CN106631005 A CN 106631005A CN 201710018252 A CN201710018252 A CN 201710018252A CN 106631005 A CN106631005 A CN 106631005A
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dielectric ceramic
ceramic composition
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voltage capacitor
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程华容
杜红炎
杨魁勇
宋蓓蓓
孙淑英
王金生
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Yuanliuhongyuan (Suzhou) Electronic Technology Co.,Ltd.
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Abstract

本发明公开了中温烧结的无铅高压电容器介质瓷料及制备方法，由以下原料组分(重量份)制备而成：100份Sr0.78Ca0.20Ba0.02TiO3、8～20份Bi2O3·2TiO2、0.05～0.35份MnCO3、0.05～0.30份Co2O3、0.01～0.08份MgTiO3、0～0.20份Al2O3、0～0.10份Nb2O5、0～0.08份HfO2、1～2份烧结助剂；通过球磨、干燥、研磨及过筛制得。本发明主要通过改变Bi2O3·2TiO2的含量来调整该电容器介质瓷料的介电常数及绝缘电阻，及选择不同掺杂改性元素改善介质瓷料的综合性能，最终获得的介质瓷料具备高介电常数、低损耗、高绝缘电阻率和很高的击穿强度。该介质瓷料实现中温烧结且不含铅，可用于制备高压多层瓷介电容器(MLCC)，具有重大的实用价值及市场价值。

Description

中温烧结的无铅高压电容器介质瓷料及制备方法
技术领域
本发明涉及电子信息材料与元器件技术领域，尤其涉及中温烧结的无铅高压电容器介质瓷料及制备方法，该瓷料不含铅、符合环保要求，中温烧结因采用低钯内浆可降低多层瓷介电容器成本，适合开发单层和多层瓷介电容器。
背景技术
高压陶瓷电容器具有高击穿电压、大容量、高稳定、高储能、交流高频等优点，有隔直流和分离各种频率分量的作用，是电视机、激光器、雷达、电子显微镜、X光机及各种测试仪器的倍压电源电路、交流电断路器等高压电源和高压线路的关键元件之一，广泛应用于送电、配电系统的电力设备和处理脉冲能量的设备。
随着材料、电极和制造技术的进步，高压电容器有了长足的发展，在大功率、高压领域使用的高压电容器要求具有小型、高耐压和频率特性好等特点，因此要求使用的瓷料介电常数高、损耗低、击穿强度高、容量频率特性温度随外电场变化相对稳定等。
目前常用作高压陶瓷电容器的介质材料有三种，即钛酸钡系、钛酸锶系和反铁电介质陶瓷，其中后两种非铁电相材料体系均含铅，如钛酸锶系大多都掺杂钛酸铅以保障高介电常数、反铁电体瓷主要是锆钛酸铅体系改性。通常，钛酸钡陶瓷因其铁电体结构具有介电常数高、介电损耗偏大(1％～2％)且击穿电压低(<100kV/cm)的特点，此外还存在电致伸缩现象，因此限制了其在高压电容器领域的应用。另一种可用的高压电容器材料是二氧化钛，它具有击穿电压高(≈350kV/cm)、介电损耗低(≈0.05％)但介电常数低(≈110)，因此作为高压储能介质陶瓷其介电常数偏低。
发明内容
针对上述问题中存在的不足之处，本发明提供中温烧结的无铅高压电容器介质瓷料及制备方法，采用该瓷料可实现电容器的中温烧结，并保持高介电常数、低损耗、高绝缘电阻和很高的击穿电压等特点。
为实现上述目的，本发明提供一种中温烧结的无铅高压电容器介质瓷料，该介质瓷料由主料、副料、改性剂和烧结助剂组成，其中：
所述主料为Sr0.78Ca0.20Ba0.02TiO3；
所述副料为Bi2O3·2TiO2；
所述改性剂为MnCO3、Co2O3、MgTiO3、Al2O3、Nb2O5、HfO2中的五种或五种以上；
所述烧结助剂ZCBS由ZnO、CaCO3、H3BO3和SiO2组成。
作为本发明的进一步改进，该介质瓷料以100重量份的Sr0.78Ca0.20Ba0.02TiO3为基材，各成分及相对含量如下：
主料Sr0.78Ca0.20Ba0.02TiO3为100份；
副料Bi2O3·2TiO2为8-20份；
烧结助剂ZCBS为1～2份；
改性剂MnCO3为0.05～0.35份；
改性剂Co2O3为0.05～0.30份；
改性剂MgTiO3为0.01～0.08份；
改性剂Al2O3为0～0.20份；
改性剂Nb2O5为0～0.10份；
改性剂HfO2为0～0.08份。
本发明还提供一种中温烧结的无铅高压电容器介质瓷料的制备方法，包括：
步骤1、采用低温液相法制备前驱体结合水热处理工艺合成主料Sr0.78Ca0.20Ba0.02TiO3；
步骤2、采用湿法混料、固相法合成副料Bi2O3·2TiO2；
步骤3、按照瓷料各成分的重量份称取各成分，放入装有氧化锆球的球磨罐中，加上去离子水球磨、烘干、研磨过筛，装袋备用，制备介质瓷料。
作为本发明的进一步改进，所述步骤1包括：
(1)配制溶液：采用分析纯原料包括SrCl2、CaCl2、BaCl2、TiCl4、NaOH及去离子水，根据配比称量后分别配制TiCl4冰水溶液、锶钙钡混合溶液、NaOH溶液；
(2)低温液相反应：将锶钙钡混合溶液与TiCl4冰水溶液按比例量取、混合后加热至60℃，将NaOH溶液加热至80℃，再把加热好的两种溶液均匀注入到反应釜中搅拌20分钟，得到前驱体为混合悬浊液；
(3)水热处理：将上述混合悬浊液移至水热釜中，于180～220℃水热3～5小时，然后过滤、去离子水洗涤、干燥、过40目筛，得到主料Sr0.78Ca0.20Ba0.02TiO3。
作为本发明的进一步改进，所述步骤2包括：
(1)称量：称取原料Bi2O3和TiO2，Bi2O3与TiO2的摩尔比为1：2；
(2)球磨：将原料Bi2O3和TiO2进行球磨，球磨介质为二氧化锆球和去离子水，球磨时间为5～8小时；
(3)烘干：将球磨后的原料进行烘干，烘干温度为100～120℃，烘干时间为6～8小时；
(4)过筛：采用玛瑙研钵对烘干后的块状料进行研磨，过筛目数为100目；
(5)煅烧：将过筛后的粉末置于刚玉坩埚中，于700～800℃煅烧3～6小时，之后随炉自然冷却；
(6)过筛：煅烧后的粉末经研磨，再过40目筛，得到副料Bi2O3·2TiO2。
作为本发明的进一步改进，在步骤3中，球磨8～15小时、于120℃烘5～8小时至干燥、研磨过40目筛，装袋备用。
本发明还提供一种中温烧结的无铅高压电容器介质瓷料的应用，向介质瓷料中加PVA溶液造粒压片，于1120℃±20℃烧结成瓷料圆片；
瓷料圆片性能如下：介电常数238-298、损耗≤0.07％、绝缘电阻率＞1013Ω·cm、击穿强度高达352kV/cm，储能密度高达1.62J/cm3。
与现有技术相比，本发明的有益效果为：
本发明实现了高压介质瓷料的中温烧结，该介质瓷料有粒度小且分布窄、分散性好的特点，同时具备高介电常数、低损耗、高绝缘电阻率和很高击穿强度等特点，该介质瓷料不含铅、镉、汞、六价铬等有毒元素，符合环保要求。
具体实施方式
为使本发明实施例的目的、技术方案和优点更加清楚，下面对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例是本发明的一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动的前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明所选原料如无特殊说明，均可通过商业渠道采购。
钛酸锶(SrTiO3)介质陶瓷具有典型的钙钛矿结构，具有介电常数高(≈250)、高频损耗低、热稳定性好等优点。因其常温下为顺电体结构，既不同于普通的线性介质、又与铁电体有所区别。钛酸锶介质不会因施加一定的外电场而导致电畴转动、引起电致应变使介质破坏，从而提高电容器的可靠性和使用寿命。本发明提供一种高介电常数、低损耗、高绝缘电阻、高击穿强度的高压介质瓷料，同时提供一种该介质瓷料的制备方法；其以钛酸锶为基材，先制备高纯Sr0.78Ca0.20Ba0.02TiO3钛酸锶基固溶体，添加Bi2O3·2TiO2提高绝缘电阻和调节介电常数，再通过Mn、Co、Nb、Al、Hf等成份及用量控制进行掺杂改性。该材料体系在高的外电场下介电常数及绝缘电阻变化不大，可望在高压电容器领域得到广泛应用。
本发明提供一种中温烧结的无铅高压电容器介质瓷料，该介质瓷料由主料、副料、改性剂和烧结助剂组成，其中：
主料为Sr0.78Ca0.20Ba0.02TiO3；
副料为Bi2O3·2TiO2；
改性剂为MnCO3、Co2O3、MgTiO3、Al2O3、Nb2O5、HfO2中的五种或五种以上；
烧结助剂ZCBS由ZnO、CaCO3、H3BO3和SiO2组成。
主料占总成份重量的81wt％-90wt％、副料占总成份重量的7wt％-16wt％该介质瓷料以100重量份的Sr0.78Ca0.20Ba0.02TiO3为基材，各成分及相对含量如下：
主料Sr0.78Ca0.20Ba0.02TiO3为100份；
副料Bi2O3·2TiO2为8-20份；
烧结助剂ZCBS为1～2份；
改性剂MnCO3为0.05～0.35份；
改性剂Co2O3为0.05～0.30份；
改性剂MgTiO3为0.01～0.08份；
改性剂Al2O3为0～0.20份；
改性剂Nb2O5为0～0.10份；
改性剂HfO2为0～0.08份。
本发明提供一种中温烧结的无铅高压电容器介质瓷料的制备方法，包括：
步骤1、采用低温液相法制备前驱体结合水热处理工艺合成主料Sr0.78Ca0.20Ba0.02TiO3；
(1)先采用原料及去离子水配制TiCl4冰水溶液、钙锶钡混合溶液、NaOH溶液三种水溶液，其中钙锶钡混合溶液中Sr:Ca:Ba摩尔比为78:20:2；(2)按摩尔比TiCl4：(SrCl2+CaCl2+BaCl2)：NaOH＝1：1：6的比例量取溶液；(3)将TiCl4溶液与钙锶钡溶液混合并加热至60℃，NaOH溶液加热至80℃，再把加热好的两种溶液均匀注入到反应釜中搅拌20分钟，得到前驱体为混合悬浊液；(4)将上述混合悬浊液移至水热釜中，于180～220℃水热3～5小时(优选于200℃水热4小时)，然后过滤、去离子水洗涤、干燥、过40目筛，得到Sr0.78Ca0.20Ba0.02TiO3粉末。
采用低温液相反应结合水热处理的主料制备方法，可以保证锶、钙和钡元素离子级别的混合反应，可制得高纯的Sr0.78Ca0.20Ba0.02TiO3固溶体材料。
步骤2、采用湿法混料、固相法合成副料Bi2O3·2TiO2；
(1)按照摩尔比1：2称量原料Bi2O3和TiO2，将其放入加有二氧化锆球的球磨罐中，加上去离子水，球磨时间为5～8小时(优选6小时)；(2)将球磨后浆料在100～120℃(优选120℃)烘6～8小时(优选6小时)至干燥，采用玛瑙研钵对研磨烘干的块料，再过100目筛；(3)过筛后干粉放入刚玉坩埚中，于700～800℃煅烧3～6小时(优选750℃煅烧4小时)，之后随炉自然冷却，煅烧后的粉末经研磨再过40目筛，得到副料Bi2O3·2TiO2粉末。
步骤3、制备烧结助剂ZCBS；
(1)按照重量比30:1:8:1分别称取原料ZnO、CaCO3、H3BO3和SiO2，放入装有氧化锆球的球磨罐中，加上适量的去离子水球磨8小时；(2)混合浆料于80℃烘12小时至干燥、研磨过100目筛；(3)将过筛的粉末置于刚玉坩埚中，650±30℃煅烧3小时，研磨过100目筛，再装袋备用。本发明的ZnO、CaCO3、H3BO3和SiO2的具体加入量可根据实际成分的加入量进行相应的调整。
步骤4、按照表1所设计的质量比例称取主料、副料、改性剂和烧结助剂放入球磨罐中，加上一定的氧化锆球及去离子水进行混合球磨12小时；然后在120℃烘6小时至干燥；采用玛瑙研钵处理后过40目筛，得到这种中温烧结的无铅高压电容器介质瓷料(表1中SCBT是Sr0.78Ca0.20Ba0.02TiO3粉末的简称)。
采用湿法混料将更加高效、均匀混合物料，制备可用的副料及高压电容器介质瓷料。
表1介质瓷料配方列表
将上述介质瓷料粉末样品按照如下步骤进行造粒压片、烧结及处理，并测试相关性能：(1)造粒压片：将介质瓷料加PVA溶液进行造粒、压片，制成直径10mm、厚约1mm的陶瓷生坯圆片；(2)烧结成瓷：将生坯圆片放入电阻炉中，以2℃/min由室温升高到600℃保温4小时排胶，然后5℃/min升至1100-1140℃，保温3小时，随炉冷却至室温，烧制成陶瓷圆片；(3)样品处理：将圆片表面打磨后测量厚度和直径，然后在圆片两面被银、烧银，形成简单的圆片电容；(4)测试：测试圆片电容的容量、损耗、绝缘电阻和击穿电压，并计算得出相对介电常数、绝缘电阻率和击穿场强，其性能参数见表2。
由于介质瓷料属于线性介质材料，其圆片电容的储能密度按照如下公式计算(其中ε0为真空介电常数、其值为8.85×10-12F/m，εr和Eb分别是介质瓷料的相对介电常数和击穿强度)：
表2介质瓷料圆片性能列表
本发明实现了高压介质瓷料的中温烧结，该介质瓷料有粒度小且分布窄、分散性好的特点，同时具备高介电常数、低损耗、高绝缘电阻率和很高击穿强度等特点，该介质瓷料不含铅、镉、汞、六价铬等有毒元素，符合环保要求。
以上仅为本发明的优选实施例而已，并不用于限制本发明，对于本领域的技术人员来说，本发明可以有各种更改和变化。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 (7)

1.一种中温烧结的无铅高压电容器介质瓷料，其特征在于，该介质瓷料由主料、副料、改性剂和烧结助剂组成，其中：
所述主料为Sr0.78Ca0.20Ba0.02TiO3；
所述副料为Bi2O3·2TiO2；
所述改性剂为MnCO3、Co2O3、MgTiO3、Al2O3、Nb2O5、HfO2中的五种或五种以上；
所述烧结助剂ZCBS由ZnO、CaCO3、H3BO3和SiO2组成。
2.如权利要求1所述的中温烧结的无铅高压电容器介质瓷料，其特征在于，该介质瓷料以100重量份的Sr0.78Ca0.20Ba0.02TiO3为基材，各成分及相对含量如下：
主料Sr0.78Ca0.20Ba0.02TiO3为100份；
副料Bi2O3·2TiO2为8-20份；
烧结助剂ZCBS为1～2份；
改性剂MnCO3为0.05～0.35份；
改性剂Co2O3为0.05～0.30份；
改性剂MgTiO3为0.01～0.08份；
改性剂Al2O3为0～0.20份；
改性剂Nb2O5为0～0.10份；
改性剂HfO2为0～0.08份。
3.一种如权利要求1～2中任一项所述的中温烧结的无铅高压电容器介质瓷料的制备方法，其特征在于，包括：
步骤1、采用低温液相法制备前驱体结合水热处理工艺合成主料Sr0.78Ca0.20Ba0.02TiO3；
步骤2、采用湿法混料、固相法合成副料Bi2O3·2TiO2；
步骤3、按照权利要求2所述的重量份称取各成分，放入装有氧化锆球的球磨罐中，加上去离子水球磨、烘干、研磨过筛，装袋备用，制备介质瓷料。
4.如权利要求3所述的中温烧结的无铅高压电容器介质瓷料的制备方法，其特征在于，所述步骤1包括：
(1)配制溶液：采用分析纯原料包括SrCl2、CaCl2、BaCl2、TiCl4、NaOH及去离子水，根据配比称量后分别配制TiCl4冰水溶液、锶钙钡混合溶液、NaOH溶液；
(2)低温液相反应：将锶钙钡混合溶液与TiCl4冰水溶液按比例量取、混合后加热至60℃，将NaOH溶液加热至80℃，再把加热好的两种溶液均匀注入到反应釜中搅拌20分钟，得到前驱体为混合悬浊液；
(3)水热处理：将上述混合悬浊液移至水热釜中，于180～220℃水热3～5小时，然后过滤、去离子水洗涤、干燥、过40目筛，得到主料Sr0.78Ca0.20Ba0.02TiO3。
5.如权利要求3所述的中温烧结的无铅高压电容器介质瓷料的制备方法，其特征在于，所述步骤2包括：
(1)称量：称取原料Bi2O3和TiO2，Bi2O3与TiO2的摩尔比为1：2；
(2)球磨：将原料Bi2O3和TiO2进行球磨，球磨介质为二氧化锆球和去离子水，球磨时间为5～8小时；
(3)烘干：将球磨后的原料进行烘干，烘干温度为100～120℃，烘干时间为6～8小时；
(4)过筛：采用玛瑙研钵对烘干后的块状料进行研磨，过筛目数为100目；
(5)煅烧：将过筛后的粉末置于刚玉坩埚中，于700～800℃煅烧3～6小时，之后随炉自然冷却；
(6)过筛：煅烧后的粉末经研磨，再过40目筛，得到副料Bi2O3·2TiO2。
6.如权利要求3所述的中温烧结的无铅高压电容器介质瓷料的制备方法，其特征在于，在步骤3中，球磨8～15小时、于120℃烘5～8小时至干燥、研磨过40目筛，装袋备用。
7.一种如权利要求1～2中任一项所述的中温烧结的无铅高压电容器介质瓷料的应用，其特征在于，向介质瓷料中加PVA溶液造粒压片，于1120℃±20℃烧结成瓷料圆片；
瓷料圆片性能如下：介电常数238-298、损耗≤0.07％、绝缘电阻率＞1013Ω·cm、击穿强度高达352kV/cm，储能密度高达1.62J/cm3。
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CN109020499A (zh) * 2018-10-10 2018-12-18 贵州大学 一种高性能压电陶瓷的制备工艺
CN109970446A (zh) * 2019-04-24 2019-07-05 北京元六鸿远电子科技股份有限公司 一种用于中温烧结的锶铋钛基储能介质材料及制备方法
CN109970446B (zh) * 2019-04-24 2021-12-24 北京元六鸿远电子科技股份有限公司 一种用于中温烧结的锶铋钛基储能介质材料及制备方法
CN110078495A (zh) * 2019-04-25 2019-08-02 北京元六鸿远电子科技股份有限公司 介电常数可调的宽温域介质陶瓷材料
CN110078495B (zh) * 2019-04-25 2022-05-10 北京元六鸿远电子科技股份有限公司 介电常数可调的宽温域介质陶瓷材料
CN111533554A (zh) * 2020-04-30 2020-08-14 福建火炬电子科技股份有限公司 一种高压陶瓷脉冲电容器、介质材料及其制备方法
CN112645708A (zh) * 2020-12-24 2021-04-13 福建火炬电子科技股份有限公司 一种抗还原bme瓷介电容器及电容器用陶瓷材料

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