CN107216140A - 一种压敏电阻陶瓷材料及其制备方法 - Google Patents

一种压敏电阻陶瓷材料及其制备方法 Download PDF

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CN107216140A
CN107216140A CN201710620236.9A CN201710620236A CN107216140A CN 107216140 A CN107216140 A CN 107216140A CN 201710620236 A CN201710620236 A CN 201710620236A CN 107216140 A CN107216140 A CN 107216140A
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李丹丹
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Hefei Tong Yu Electronic Technology Co Ltd
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Abstract

本发明公开了一种压敏电阻陶瓷材料及其制备方法，所述陶瓷材料包括如下重量份的组分：氧化锌ZnO 60～80份、二氧化钛TiO2 5～10份、二氧化锰MnO2 3～6份、五氧化二钒V2O5 3～6份、氧化钴Co2O3 1.5～2.8份、氧化铬Cr2O3 1.2～2.2份、五氧化二铌Nb2O5 0.3～0.8份、钛酸锶SrTiO3 0.6～1.8份、钛酸镁Mg2TiO4 0.8～2.0份、碳酸锂Li2CO3 0.1～0.6份。制备方法包括混合制浆、煅烧、球磨压制、粉碎磨粉。本发明的陶瓷材料吸收能力与脉冲冲击耐受能力强，韧性高，不易破碎，再加工性能优越，制备方法简单，能耗低，节约成本。

Description

一种压敏电阻陶瓷材料及其制备方法
技术领域
本发明涉及压敏电阻材料领域，具体涉及一种压敏电阻陶瓷材料及其制备方法。
背景技术
氧化锌压敏陶瓷以其非线性系数高、响应速度快、漏电流小、残压低、制造成本低廉等优势，已成为应用最广、性能最好的压敏电阻材料之一，广泛应用于电力、通信、交通、集成电路、汽车电子、医用设备和家用电器等领域。
现有的压敏电阻以ZnO材料为主，其制备方法是以ZnO粉末为主要原料，添加Bi2O3和其它的一些氧化物，如Sb2O3、Co2O3等，通过高温陶瓷制备工艺得到，高温陶瓷烧结工艺温度为900℃～1300℃，烧结时间为4小时以上。因此现有的压敏电阻为陶瓷型压敏电阻，具有陶瓷材料所具有的共同缺点是机械性能差，脆性强、易碎、再加工困难。
发明内容
本发明的目的在于克服上述现有技术的不足，提供了一种压敏电阻陶瓷材料及其制备方法，该陶瓷材料具有吸收能力与脉冲冲击耐受能力强等良好的电气性能，而且韧性高，不易破碎，再加工性能优越，制备方法简单，能耗低，节约成本。
本发明解决技术问题采用如下技术方案：
一种压敏电阻陶瓷材料，包括如下重量份的组分：氧化锌ZnO 60～80份、二氧化钛TiO25～10份、二氧化锰MnO2 3～6份、五氧化二钒V2O5 3～6份、氧化钴Co2O3 1.5～2.8份、氧化铬Cr2O3 1.2～2.2份、五氧化二铌Nb2O5 0.3～0.8份、钛酸锶SrTiO3 0.6～1.8份、钛酸镁Mg2TiO4 0.8～2.0份、碳酸锂Li2CO3 0.1～0.6份。
优选地，所述陶瓷材料包括如下重量份的组分：氧化锌ZnO 70份、二氧化钛TiO2 6份、二氧化锰MnO2 5份、五氧化二钒V2O5 4份、氧化钴Co2O3 1.9份、氧化铬Cr2O3 1.7份、五氧化二铌Nb2O5 0.5份、钛酸锶SrTiO3 1.2份、钛酸镁Mg2TiO4 1.5份、碳酸锂Li2CO3 0.2份。
上述压敏电阻陶瓷材料的制备方法，包括如下步骤：
（1）按照重量份称取各组分，混合搅拌均匀后过100～200目筛，加入适量水，放入球磨机中球磨制成浆料；
（2）将浆料在100～150℃烘干至含水量2～6%，放入窑炉中，于800～900℃煅烧3～6小时，得到陶瓷主料；
（3）将陶瓷主料放入球磨机中，加入适量水和3～5%的聚乙烯醇水溶液，球磨成浆液，在鼓风烘箱中干燥1～2小时，再用压力机压制成块状物料，置于干燥通风处2～3天；
（4）将通风干燥后的块状物料通入超微粉碎机中粉碎，过200～300目筛，磨粉机磨粉得到颗粒状的瓷料；
（5）将颗粒状的瓷料通入压力机中压制成圆片状陶瓷胚片，放入窑炉中，升温至450～500℃排胶2～3小时，再升温至900～1000℃烧结保温2～3小时，自然冷却至室温得到该压敏电阻陶瓷材料。
优选地，所述步骤（1）加入的水量为各组分混合后总重量的0.6～1.5倍。
优选地，所述步骤（1）球磨机的转速为400～600r/min，球磨时间为10～18小时。
优选地，所述步骤（3）球磨机的转速为800～1000r/min，球磨时间为6～10小时。
优选地，所述步骤（3）压力机的工作压力为5～10MPa。
优选地，所述步骤（5）压力机的工作压力为10～20MPa。
与现有技术相比，本发明具有如下的有益效果：
（1）本发明的压敏电阻陶瓷材料，具有吸收能力与脉冲冲击耐受能力强等良好的电气性能，而且韧性高，不易破碎，再加工性能优越，制备方法简单，能耗低，节约成本。
（2）本发明的压敏电阻陶瓷材料，采用氧化锌ZnO、氧化钴Co2O3、氧化铬Cr2O3、二氧化钛TiO2、二氧化锰MnO2、五氧化二钒V2O5、钛酸锶SrTiO3、钛酸镁Mg2TiO4、碳酸锂Li2CO3几种金属氧化物成分，配比合理，氧化锌和氧化钒、氧化钛反应形成低熔点液相，从而确保陶瓷体可以低温烧结成瓷；同时参与形成液相的掺杂元素及添加的锰、钴掺杂元素在液相的辅助传质机理作用下，完成在ZnO晶粒表面的均匀分布，进而促进在晶界上形成压敏电阻所需的晶界势垒。
（3）本发明的压敏电阻陶瓷材料的制备方法，采用湿法球磨成浆液、烘干煅烧等合理工艺，获取的压敏电阻陶瓷材料，电位梯度可达到500～580V/mm，非线性系数达到45以上，泄漏电流为约1.5μA，吸波能力与耐大电流冲击能力强。
具体实施方式
以下结合具体实施例对发明作进一步详细的描述。
实施例1
一种压敏电阻陶瓷材料，包括如下重量份的组分：氧化锌ZnO 70份、二氧化钛TiO2 6份、二氧化锰MnO2 5份、五氧化二钒V2O5 4份、氧化钴Co2O3 1.9份、氧化铬Cr2O3 1.7份、五氧化二铌Nb2O5 0.5份、钛酸锶SrTiO3 1.2份、钛酸镁Mg2TiO4 1.5份、碳酸锂Li2CO3 0.2份。
上述压敏电阻陶瓷材料的制备方法，包括如下步骤：
（1）按照重量份称取各组分，混合搅拌均匀后过100～200目筛，加入适量水，放入600r/min的球磨机中球磨12小时制成浆料；其中，水的加入量为混合物总质量的1.5倍。
（2）将浆料在150℃烘干至含水量2～6%，放入窑炉中，于900℃煅烧3小时，得到陶瓷主料。
（3）将陶瓷主料放入球磨机中，加入适量水和3～5%的聚乙烯醇水溶液，1000r/min球磨6小时得到浆液，在鼓风烘箱中干燥1小时，再用压力机于10MPa压力下压制成块状物料，置于干燥通风处2～3天。
（4）将通风干燥后的块状物料通入超微粉碎机中粉碎，过200～300目筛，磨粉机磨粉得到颗粒状的瓷料。
（5）将颗粒状的瓷料通入压力机中于20MPa压力下压制成圆片状陶瓷胚片，放入窑炉中，升温至500℃排胶2小时，再升温至900℃烧结保温3小时，自然冷却至室温得到该压敏电阻陶瓷材料。
本实施例的压敏电阻陶瓷材料电位梯度可达到580V/mm，非线性系数达到45以上，泄漏电流为约1.5μA。
实施例2
一种压敏电阻陶瓷材料，包括如下重量份的组分：氧化锌ZnO 66份、二氧化钛TiO2 6份、二氧化锰MnO2 3份、五氧化二钒V2O5 4份、氧化钴Co2O3 1.7份、氧化铬Cr2O3 1.5份、五氧化二铌Nb2O5 0.5份、钛酸锶SrTiO3 0.9份、钛酸镁Mg2TiO4 1.3份、碳酸锂Li2CO3 0.2份。
上述压敏电阻陶瓷材料的制备方法，包括如下步骤：
（1）按照重量份称取各组分，混合搅拌均匀后过100～200目筛，加入适量水，放入600r/min的球磨机中球磨12小时制成浆料；其中，水的加入量为混合物总质量的1.5倍。
（2）将浆料在150℃烘干至含水量2～6%，放入窑炉中，于900℃煅烧3小时，得到陶瓷主料。
（3）将陶瓷主料放入球磨机中，加入适量水和3～5%的聚乙烯醇水溶液，1000r/min球磨6小时得到浆液，在鼓风烘箱中干燥1小时，再用压力机于10MPa压力下压制成块状物料，置于干燥通风处2～3天。
（4）将通风干燥后的块状物料通入超微粉碎机中粉碎，过200～300目筛，磨粉机磨粉得到颗粒状的瓷料。
（5）将颗粒状的瓷料通入压力机中于20MPa压力下压制成圆片状陶瓷胚片，放入窑炉中，升温至500℃排胶2小时，再升温至900℃烧结保温3小时，自然冷却至室温得到该压敏电阻陶瓷材料。
本实施例的压敏电阻陶瓷材料电位梯度可达到572V/mm，非线性系数达到45以上，泄漏电流为约1.5μA。
实施例3
一种压敏电阻陶瓷材料，包括如下重量份的组分：氧化锌ZnO 70份、二氧化钛TiO2 8份、二氧化锰MnO2 3份、五氧化二钒V2O5 5份、氧化钴Co2O3 2.3份、氧化铬Cr2O3 1.8份、五氧化二铌Nb2O5 0.6份、钛酸锶SrTiO3 1.2份、钛酸镁Mg2TiO4 1.5份、碳酸锂Li2CO3 0.5份。
上述压敏电阻陶瓷材料的制备方法，包括如下步骤：
（1）按照重量份称取各组分，混合搅拌均匀后过100～200目筛，加入适量水，放入600r/min的球磨机中球磨12小时制成浆料；其中，水的加入量为混合物总质量的1.5倍。
（2）将浆料在150℃烘干至含水量2～6%，放入窑炉中，于900℃煅烧3小时，得到陶瓷主料。
（3）将陶瓷主料放入球磨机中，加入适量水和3～5%的聚乙烯醇水溶液，1000r/min球磨6小时得到浆液，在鼓风烘箱中干燥1小时，再用压力机于10MPa压力下压制成块状物料，置于干燥通风处2～3天。
（4）将通风干燥后的块状物料通入超微粉碎机中粉碎，过200～300目筛，磨粉机磨粉得到颗粒状的瓷料。
（5）将颗粒状的瓷料通入压力机中于20MPa压力下压制成圆片状陶瓷胚片，放入窑炉中，升温至500℃排胶2小时，再升温至900℃烧结保温3小时，自然冷却至室温得到该压敏电阻陶瓷材料。
本实施例的压敏电阻陶瓷材料电位梯度可达到566V/mm，非线性系数达到45以上，泄漏电流为约1.5μA。
实施例4
一种压敏电阻陶瓷材料，包括如下重量份的组分：氧化锌ZnO 80份、二氧化钛TiO2 8份、二氧化锰MnO2 6份、五氧化二钒V2O5 5份、氧化钴Co2O3 2.5份、氧化铬Cr2O3 2.0份、五氧化二铌Nb2O5 0.7份、钛酸锶SrTiO3 1.6份、钛酸镁Mg2TiO4 1.5份、碳酸锂Li2CO3 0.5份。
上述压敏电阻陶瓷材料的制备方法，包括如下步骤：
（1）按照重量份称取各组分，混合搅拌均匀后过100～200目筛，加入适量水，放入500r/min的球磨机中球磨15小时制成浆料；其中，水的加入量为混合物总质量的0.9倍。
（2）将浆料在120℃烘干至含水量2～6%，放入窑炉中，于820℃煅烧5小时，得到陶瓷主料。
（3）将陶瓷主料放入球磨机中，加入适量水和3～5%的聚乙烯醇水溶液，900r/min球磨8小时得到浆液，在鼓风烘箱中干燥1.8小时，再用压力机于10MPa压力下压制成块状物料，置于干燥通风处2～3天。
（4）将通风干燥后的块状物料通入超微粉碎机中粉碎，过200～300目筛，磨粉机磨粉得到颗粒状的瓷料。
（5）将颗粒状的瓷料通入压力机中于16MPa压力下压制成圆片状陶瓷胚片，放入窑炉中，升温至480℃排胶2.2小时，再升温至960℃烧结保温2.5小时，自然冷却至室温得到该压敏电阻陶瓷材料。
本实施例的压敏电阻陶瓷材料电位梯度可达到559V/mm，非线性系数达到45以上，泄漏电流为约1.5μA。
实施例5
一种压敏电阻陶瓷材料，包括如下重量份的组分：氧化锌ZnO 80份、二氧化钛TiO2 10份、二氧化锰MnO2 6份、五氧化二钒V2O5 6份、氧化钴Co2O3 2.8份、氧化铬Cr2O3 2.2份、五氧化二铌Nb2O5 0.6份、钛酸锶SrTiO3 1.6份、钛酸镁Mg2TiO4 1.8份、碳酸锂Li2CO3 0.6份。
上述压敏电阻陶瓷材料的制备方法，包括如下步骤：
（1）按照重量份称取各组分，混合搅拌均匀后过100～200目筛，加入适量水，放入400r/min的球磨机中球磨18小时制成浆料；其中，水的加入量为混合物总质量的1.3倍。
（2）将浆料在135℃烘干至含水量2～6%，放入窑炉中，于860℃煅烧5小时，得到陶瓷主料。
（3）将陶瓷主料放入球磨机中，加入适量水和3～5%的聚乙烯醇水溶液，1000r/min球磨6小时得到浆液，在鼓风烘箱中干燥1小时，再用压力机于8MPa压力下压制成块状物料，置于干燥通风处2～3天。
（4）将通风干燥后的块状物料通入超微粉碎机中粉碎，过200～300目筛，磨粉机磨粉得到颗粒状的瓷料。
（5）将颗粒状的瓷料通入压力机中于16MPa压力下压制成圆片状陶瓷胚片，放入窑炉中，升温至480℃排胶2.2小时，再升温至920℃烧结保温2.3小时，自然冷却至室温得到该压敏电阻陶瓷材料。
本实施例的压敏电阻陶瓷材料电位梯度可达到560V/mm，非线性系数达到45以上，泄漏电流为约1.5μA。
以上所述仅是本发明的优选实施方式，本发明的保护范围并不仅局限于上述实施例，凡属于本发明思路下的技术方案均属于本发明的保护范围。应当指出，对于本技术领域的普通技术人员来说，在不脱离本发明原理前提下的若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。

Claims (8)

1.一种压敏电阻陶瓷材料，其特征在于，包括如下重量份的组分：氧化锌ZnO 60～80份、二氧化钛TiO2 5～10份、二氧化锰MnO2 3～6份、五氧化二钒V2O5 3～6份、氧化钴Co2O3 1.5～2.8份、氧化铬Cr2O3 1.2～2.2份、五氧化二铌Nb2O5 0.3～0.8份、钛酸锶SrTiO3 0.6～1.8份、钛酸镁Mg2TiO4 0.8～2.0份、碳酸锂Li2CO3 0.1～0.6份。
2.根据权利要求1所述的压敏电阻陶瓷材料，其特征在于，所述陶瓷材料包括如下重量份的组分：氧化锌ZnO 70份、二氧化钛TiO2 6份、二氧化锰MnO2 5份、五氧化二钒V2O5 4份、氧化钴Co2O3 1.9份、氧化铬Cr2O3 1.7份、五氧化二铌Nb2O5 0.5份、钛酸锶SrTiO3 1.2份、钛酸镁Mg2TiO4 1.5份、碳酸锂Li2CO3 0.2份。
3.根据权利要求1或2所述的压敏电阻陶瓷材料的制备方法，其特征在于，包括如下步骤：
（1）按照重量份称取各组分，混合搅拌均匀后过100～200目筛，加入适量水，放入球磨机中球磨制成浆料；
（2）将浆料在100～150℃烘干至含水量2～6%，放入窑炉中，于800～900℃煅烧3～6小时，得到陶瓷主料；
（3）将陶瓷主料放入球磨机中，加入适量水和3～5%的聚乙烯醇水溶液，球磨成浆液，在鼓风烘箱中干燥1～2小时，再用压力机压制成块状物料，置于干燥通风处2～3天；
（4）将通风干燥后的块状物料通入超微粉碎机中粉碎，过200～300目筛，磨粉机磨粉得到颗粒状的瓷料；
（5）将颗粒状的瓷料通入压力机中压制成圆片状陶瓷胚片，放入窑炉中，升温至450～500℃排胶2～3小时，再升温至900～1000℃烧结保温2～3小时，自然冷却至室温得到该压敏电阻陶瓷材料。
4.根据权利要求3所述的压敏电阻陶瓷材料的制备方法，其特征在于，所述步骤（1）加入的水量为各组分混合后总重量的0.6～1.5倍。
5.根据权利要求3所述的压敏电阻陶瓷材料的制备方法，其特征在于，所述步骤（1）球磨机的转速为400～600r/min，球磨时间为10～18小时。
6.根据权利要求3所述的压敏电阻陶瓷材料的制备方法，其特征在于，所述步骤（3）球磨机的转速为800～1000r/min，球磨时间为6～10小时。
7.根据权利要求3所述的压敏电阻陶瓷材料的制备方法，其特征在于，所述步骤（3）压力机的工作压力为5～10MPa。
8.根据权利要求3所述的压敏电阻陶瓷材料的制备方法，其特征在于，所述步骤（5）压力机的工作压力为10～20MPa。
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