CN105906339B - 一种大通流中压ZnO压敏电阻瓷料及其制备方法 - Google Patents

一种大通流中压ZnO压敏电阻瓷料及其制备方法 Download PDF

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CN105906339B
CN105906339B CN201610246644.8A CN201610246644A CN105906339B CN 105906339 B CN105906339 B CN 105906339B CN 201610246644 A CN201610246644 A CN 201610246644A CN 105906339 B CN105906339 B CN 105906339B
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黄欣刚
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Abstract

一种大通流中压ZnO压敏电阻瓷料及其制备方法，将ZnO、Bi2O3、Sb2O3、Co3O4、Cr2O3、Mn3O4、Ni2O3、B2O3和A1(NO3)3·9H2O按比例混合均匀后，采用湿法球磨，得到浆料，将磨好的浆料进行喷雾造粒得到固体瓷料，将固体瓷料过筛后密封陈腐即可制得。本发明通过改变中压ZnO压敏电阻瓷料中的添加剂和配比来提高通流能力，使中压ZnO压敏电阻瓷料的通流由现在的6KA/cm2提高到8KA/cm2。本发明添加物的总量比较少，特别是去掉了价格昂贵的AgNO3，使得成本大幅降低。

Description

一种大通流中压ZnO压敏电阻瓷料及其制备方法
技术领域
本发明属电子材料领域，具体涉及一种大通流中压ZnO压敏电阻瓷料及其制备方法。
背景技术
ZnO压敏电阻是以ZnO粉料为主体，添加多种微量的其他金属化合物添加剂(如Bi2O3、Sb2O3、MnCO3、Co2O3、Cr2O3等)，经混合、成型后在高温下烧结而成的多晶多相半导体陶瓷元件。自它的发明以来，ZnO压敏电阻就以其造价低廉、制造方便、非线性系数大、响应时间快、通流容量大等优良性能，得到了广泛的应用，特别是ZnO压敏电阻具有优良的非线性伏安特性和吸收冲击能量的能力，使得其成为交直流电力系统和电子电路中发展较快且应用十分广泛的电压保护装置，但在ZnO压敏电阻行业依然面临着如何降低压敏电阻的体积和重量，使其更加小型化，如何提高压敏电阻通流能力同时降低生产成本等难题。
发明内容
本发明解决的技术问题：提供一种大通流中压ZnO压敏电阻瓷料及其制备方法，通过改变中压ZnO压敏电阻瓷料中的添加剂和配比来提高通流能力，同时不使用价格昂贵的AgNO3，实现了瓷料生产成本的大幅度降低，并且瓷料性能显著提高。
本发明的设计思路：对ZnO压敏电阻而言，要提高其通流能力不是易事，行业中一般都采用通过提高添加物的量来提高通流，目前ZnO压敏电阻瓷料的通流量可达到7KA/CM2，而本发明是通过减少添加物的量来提高通流，使ZnO压敏电阻瓷料通流量达到了8KA/cm2以上。
本发明的技术解决方案：ZnO压敏电阻瓷料以ZnO为主要成分，添加多种氧化物，使添加物偏析在以ZnO为主晶相的晶界，构成多晶结构，是构成ZnO压敏陶瓷结构并产生相应的非线性电气性能的基础。
根据每一种添加物在体系中所起的作用，添加物的物相组成及相变过程，同时考虑到添加物与添加物之间的影响因素，本发明设计了一系列添加物配比方案，经过试验发现:
1、要想提高ZnO压敏电阻的非线性，必须依靠体系来解决，任何一种添加物都不能改变它。
2、添加物在最终构成的多晶结构中，由于其含量的不同，杂质的成分及含量的不同，以及工艺条件的不同均发生着变化，而且这种变化无规律性，具体表现为电性能的无规律变化。
因此，要想得到一组较佳的配方就十分困难，本发明经过了大量的实验研究，最终确定了一组比较理想的中压大通流ZnO压敏电阻瓷料配方。
本发明的技术解决方案：一种大通流中压ZnO压敏电阻瓷料，由下述重量比的原料制成：ZnO 100kg，Bi2O31.0-2.0kg，Sb2O32.0-3.0kg，Co3O40.5-0.9kg，Cr2O30.4-0.7kg，Mn3O40.3-0.6kg，Ni2O3 0.3-0.6kg，B2O3 0.002-0.006kg，A1(NO3)3·9H2O 0.008-0.012kg。
所述ZnO含量≥99.7％，杂质Na+、Fe2+的含量≤20ppm。
所述Bi2O3含量≥99％；所述Sb2O3含量≥99.8％；所述Co3O4含量在71％-73％之间；所述Cr2O3含量≥99％；所述Mn3O4中锰含量≥71％；所述Ni2O3中镍含量在73-76％之间；所述B2O3含量≥99％；所述A1(NO3)3·9H2O含量≥99％。
一种大通流中压ZnO压敏电阻瓷料的制备方法：
步骤一、将ZnO、Bi2O3、Sb2O3、Co3O4、Cr2O3、Mn3O4、Ni2O3、B2O3和A1(NO3)3·9H2O按所述重量比混合均匀后，加入球磨机中，并采用湿法球磨，加入纯水55-62kg和PVA粘合剂6-10kg，搅拌球磨2.5-4h，得到浆料，其中球占球磨机有效容积的2/3；
步骤二、将步骤一磨好的浆料进行喷雾造粒得到固体瓷料；所述喷雾造粒的工艺参数如下：离心式雾化盘转速7800r/min，喷塔进口温度250℃-300℃，喷塔出口温度80℃-120℃；
步骤三、将固体瓷料过100目筛，密封陈腐20-30h即可。
本发明与现有技术相比具有的优点和效果：
1、本发明通过改变中压ZnO压敏电阻瓷料中的添加剂和配比来提高通流能力，使中压ZnO压敏电阻瓷料的通流由现在的6KA/cm2提高到8KA/cm2；
2、采用本发明生产的中压ZnO压敏电阻瓷料制做的压敏电阻器，同样的通流则体积小，反之，同样体积则通流大，扩大了产品的应用范围。同时，由于本发明添加物的总量比较少，特别是去掉了价格昂贵的AgNO3，使得成本大幅降低；
3、本发明提高了中压ZnO压敏电阻瓷料的性能。经实验主要性能指标为：
具体实施方式
实施例1：
1、配料。首先确定各种材料的质量符合规定要求：ZnO含量≥99.7％，杂质Na+、Fe2+的含量≤20ppm；Bi2O3含量≥99％；Sb2O3含量≥99.8％；Co3O4含量在71％-73％之间；Cr2O3含量≥99％；Mn3O4中锰含量≥71％；Ni2O3中镍含量在73-76％之间；B2O3含量≥99％；A1(NO3)3·9H2O含量≥99％。然后按下述瓷料配方，准确称量配料：ZnO 100kg，Bi2O3 1.43kg，Sb2O3 2.65kg，Co3O4 0.585kg，Cr2O3 0.504kg，Mn3O4 0.458kg，Ni2O3 0.406kg，B2O32.51g，A1(NO3)3·9H2O10g。
2、球磨。将称量好的料加入到搅拌球磨机中，再加纯水58Kg、PVA粘合剂(聚乙烯醇)8kg,搅拌球磨3h(其中球占球磨机的有效容积2/3)。
3、喷雾造粒。将磨好的浆料进行喷雾造粒得到固体瓷料。喷雾造粒的工艺参数如下：离心式雾化盘转速7800r/min，喷塔进口温度280℃，喷塔出口温度100℃。
4、过筛陈腐。将造粒好的固体瓷料过100目筛，再密封陈腐24h，即得到大通流中压ZnO压敏电阻瓷料。
实施例2：工艺步骤与实施例1基本相同，不同之处在于瓷料配方不同：ZnO 100kg，Bi2O3 1.81kg，Sb2O3 2.71kg，Co3O4 0.683kg，Cr2O3 0.650kg，Mn3O4 0.512kg，Ni2O30.453kg，B2O32.58g，A1(NO3)3·9H2O11g。
最后对瓷料进行电性能检测，并对经检测合格的瓷料包装。取制得的瓷料样干压成型后制成Φ25mmX2mm的圆饼胚体，在1230℃保温3h,烧结得到Φ21.06mmX1.6mm的压敏陶瓷片，在其两端面涂80银浆，经氧化还原成银片，焊引线，绝缘漆封装，测得电性能如下表：
本发明生产的瓷料电性能均能达到设计指标，外观一致性好，单、叠装烧结性能一致。
上述实施例只是本发明的较佳实施例，并非用来限制本发明实施范围，故以本发明权利要求所述内容的等同变化，均应包括在本发明权利要求范围之内。

Claims (1)

1.一种大通流中压ZnO压敏电阻瓷料，其特征在于由下述重量比的原料制成：ZnO100kg，Bi2O31.0-2.0kg，Sb2O32.0-3.0kg，Co3O40.5-0.9kg，Cr2O30.4-0.7kg，Mn3O40.3-0.6kg，Ni2O3 0.3-0.6kg，B2O3 0.002-0.006kg，A1(NO3)3·9H2O 0.008-0.012kg；
所述ZnO含量≥99.7％，杂质Na+、Fe2+的含量≤20ppm；
所述Bi2O3含量≥99％；所述Sb2O3含量≥99.8％；所述Co3O4含量在71％-73％之间；所述Cr2O3含量≥99％；所述Mn3O4中锰含量≥71％；所述Ni2O3中镍含量在73-76％之间；所述B2O3含量≥99％；所述A1(NO3)3·9H2O含量≥99％；
所述的大通流中压ZnO压敏电阻瓷料的制备方法如下：
步骤一、将ZnO、Bi2O3、Sb2O3、Co3O4、Cr2O3、Mn3O4、Ni2O3、B2O3和A1(NO3)3·9H2O按所述重量比混合均匀后，加入球磨机中，并采用湿法球磨，加入纯水55-62kg和PVA粘合剂6-10kg，搅拌球磨2.5-4h，得到浆料，其中球占球磨机有效容积的2/3；
步骤二、将步骤一磨好的浆料进行喷雾造粒得到固体瓷料；所述喷雾造粒的工艺参数如下：离心式雾化盘转速7800r/min，喷塔进口温度250℃-300℃，喷塔出口温度80℃-120℃；
步骤三、将固体瓷料过100目筛，密封陈腐20-30h即可。
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CN104150896A (zh) * 2014-08-08 2014-11-19 汕头高新区松田实业有限公司 高通流小型化氧化锌压敏电阻器介质材料及其制备方法
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EP2144256B1 (en) * 2008-07-09 2011-03-16 Kabushiki Kaisha Toshiba Current/voltage nonlinear resistor
CN102617126A (zh) * 2012-03-31 2012-08-01 中国科学院上海硅酸盐研究所 一种低温烧结氧化锌压敏电阻材料及其制备方法
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