CN107871574A - 一种负温度系数陶瓷热敏电阻的制造方法 - Google Patents
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Abstract
本发明涉及一种负温度系数陶瓷热敏电阻的制造方法。在Mn 3 O 4,Co 3 O 4,Fe 2 O 3中微量掺杂ZnO,混合均匀经过球磨、预烧、喷雾造粒后成型,置于热压炉,通过升温时升压、恒温、恒压1050‑1150℃、10Mpa烧结、降温同时降压;再在瓷体表面用真空蒸发镀膜方式制备表面电极。本发明通过升温时升压、恒温时恒压、降温时降压的热压烧结工艺,烧结恒温温度1050‑1200℃,低于1400℃,大大提高了材料的致密度、热传导系数;采用蒸发镀膜工艺制备陶瓷表面电极,表面金属电极与瓷体结合好,提高了热传导系数,进而提高了负温度系数热敏电阻的耗散系数、伏安特性值;提高了可耐受的最大直流电压,使其避免了在大的工作电压冲击下因为散热不良引起的自热现象,提高了热敏电阻温度测量和控制的准确性。
Description
技术领域
本发明涉及一种负温度系数(NTC)陶瓷热敏电阻的制造方法。
背景技术
在半导体类负温度系数热敏电阻中,常用的负温度系数(NTC)热敏电阻由锰、钴、铁、镍等过渡金属氧化物组成,该种负温度系数热敏电阻(NTC)具有电阻值随着温度上升而呈指数形式下降的特性。由于热敏电阻具备芯片体积小、尺寸与形状的变化灵活、绝对电阻大的特点,在进行温度测量时具有反应灵敏、高精度、低成本的特点,且能够使用很长的连接线和容许较大的接触电阻。由于其独特的特性,在家电、汽车、医疗、航空航天等领域的温度测量控制、温度补偿、间接测量其它参数如液体位置、液体流量、真空度等有广泛应用,
NTC热敏电阻芯片体积小、反应灵敏、组装方是它的优点,它能很快稳定,不会造成热负载。但热敏电阻是一种电阻性器件,需要使用电流源,任何电流源都会在其上因功率而造成发热。为了能够让NTC热敏电阻精确地反映出温度的高低,就必须注意避免因电流过大而引起热敏电阻“自热”的现象。NTC热敏电阻的静态伏安特性即电压-电流特性是NTC热敏电阻基本又重要的特性之一。它表示在热敏电阻器两端的电压和通过它的电流在热敏电阻器和周围介质热平衡时—即加在元件上的电功率和耗散功率相等时的关系。该特性曲线表明了在一定温度的静止介质中,随着通过NTC元件上的电流改变,元件两端电压的变化规律。
在NTC静态伏安特性曲线中,存在一个Im对应的Umax,达到Umax,NTC热敏电阻的电功率和耗散功率达到了平衡状态,由于自热带来的温升影响最小,影响测试精度最小,这个Umax通常也称为最大可耐受直流电压,提高最大可耐受直流电压即可有效避免热敏电阻产生的自热现象,真实的反映环境温度,避免产生测量误差。
传统的NTC热敏电阻材料成型后采用常压高温烧结,烧结温度高达1400℃,耗能极大,由于烧渗传热一致性欠缺,造成瓷体容易开裂,且致密度不高,热敏芯片热传导系数低;表面电极制备采用丝网印刷工艺经高温烧结,表面金属电极与瓷体之间附着力不好,接触电阻大,同样影响了材料的热传导,导致耗散系数低,通过电流时,可耐受最大直流电压低,散热能力不好,导致自热影响测量精度。
发明内容
本发明的目的是针对上述现状,旨在提供一种烧结温度低、耗能小,材料致密度高、表面金属电极与瓷体结合好,热传导性好的负温度系数(NTC)陶瓷热敏电阻的制造方法。
本发明目的的实现方式为,一种负温度系数陶瓷热敏电阻的制造方法,具体步骤如下:
1)制备粉体:将锰、钴、铁元素分别以纳米级分析纯Mn3O4,Co3O4,Fe2O3的形式引入,作为主要原料,各氧化物中Mn、Co、Fe元素比为0.6-0.9:1.0:0.3,微量掺杂ZnO,ZnO掺入量为Mn3O4,Co3O4,Fe2O3总量的2%-10%,混合均匀经过球磨、在900℃下预烧2-4小时后,喷雾,加入PVA溶液造粒,得陶瓷颗粒;
2)制备陶瓷基体:陶瓷颗粒常温等静压成型后,置于热压炉内,温度在由常温升至1050-1150℃的同时,压力由常压升至10MPa烧结6-14小时,而后在降温的同时降压至常温、常压,得热敏陶瓷基体;
3)制备表面电极:在热敏陶瓷基体表面用真空蒸发镀膜方式制备表面电极,所述表面电极为金、银、铜金属中的任意两种金属按一定比例结合,其中银的重量比为80%,金的重量比为20%或80%,铜的重量比为20%。
本发明通过升温同时升压、恒温时恒压、降温同时时降压的热压烧结工艺,烧结恒温温度1050-1150℃,低于1400℃,耗能小,大大提高了材料的致密度、热传导系数;采用蒸发镀膜工艺制备陶瓷表面电极,表面金属电极与瓷体结合好,提高了热传导系数,进而提高了负温度系数热敏电阻的耗散系数、伏安特性值;提高了可耐受的最大直流电压,使其避免了在大的工作电压冲击下因为散热不良引起的自热现象,提高了热敏电阻温度测量和控制的准确性。
具体实施方式
本发明是在纳米级分析纯Mn3O4,Co3O4,Fe2O3中微量掺杂ZnO,混合均匀,经过球磨、预烧、喷雾造粒后,通过升温时升压、恒温、恒压在1050-1150℃、10Mpa烧结、降温,降温同时降压;而后在表面用真空蒸发镀膜方式制备表面电极。
下面用具体实施例说明本发明。
例1、
1)制备粉体:将锰、钴、铁元素分别以纳米级分析纯Mn3O4,Co3O4,Fe2O3的形式引入,作为主要原料,各氧化物中Mn、Co、Fe元素比为0.6:1.0:0.3,微量掺杂ZnO,ZnO掺入量为Mn3O4,Co3O4,Fe2O3总量的2%。混合均匀经过球磨、在900℃下预烧2小时后,喷雾,加入PVA溶液造粒,得陶瓷颗粒;
2)制备陶瓷基体:陶瓷颗粒常温等静压成型后,置于热压炉内,温度在由常温升至1050的同时,压力由常压升至10MPa烧结6小时,而后在降温的同时降压至常温、常压,得热敏陶瓷基体;
3)制备表面电极:在热敏陶瓷基体表面用真空蒸发镀膜方式制备表面电极,表面电极厚度约8μm。所述表面电极为金、银。其中银、金的重量比为80%、20%。
例2、
同例1,不同的是各氧化物中Mn、Co、Fe元素比为0.75:1.0:0.3,ZnO掺入量为Mn3O4,Co3O4,Fe2O3总量的5%。混合均匀经过球磨、在900℃下预烧3小时后,喷雾,加入PVA溶液造粒,得陶瓷颗粒陶瓷,颗粒成型后在1080℃,10MPa烧结8小时。所述表面电极为银、铜,其中银、铜的重量比为80%、20%。
例3、
同例1,不同的是各氧化物中Mn、Co、Fe元素比为0.9:1.0:0.3,ZnO掺入量为Mn3O4,Co3O4,Fe2O3总量的10%。混合均匀经过球磨、在900℃下预烧4小时后,喷雾,加入PVA溶液造粒,得陶瓷颗粒陶瓷,颗粒成型后在1150℃,10MPa下烧结14小时。所述表面电极为金、铜,其中金、铜的重量比为80%、20%。
Claims (2)
1.一种负温度系数陶瓷热敏电阻的制造方法,其特征在于具体步骤如下:
1)制备粉体:将锰、钴、铁元素分别以纳米级分析纯Mn3O4,Co3O4,Fe2O3的形式引入,作为主要原料,各氧化物中Mn、Co、Fe元素比为0.6-0.9:1.0:0.3,微量掺杂ZnO,ZnO掺入量为Mn3O4,Co3O4,Fe2O3总量的2%-10%,混合均匀经过球磨、在900℃下预烧2-4小时后,喷雾,加入PVA溶液造粒,得陶瓷颗粒;
2)制备陶瓷基体:陶瓷颗粒常温等静压成型后,置于热压炉内,温度在由常温升至1050-1150的同时,压力由常压升至10MPa烧结6-14小时,而后在降温的同时降压至常温、常压,得热敏陶瓷基体;
3)制备表面电极:在热敏陶瓷基体表面用真空蒸发镀膜方式制备表面电极,所述表面电极为金、银、铜金属中两种金属按比例结合,其中银的重量比为80%,金的重量比为20%或80%,铜的重量比为20%。
2.根据权利要求1所述的一种负温度系数陶瓷热敏电阻的制造方法,其特征在于在热敏陶瓷基体表面用真空蒸发镀膜方式制备表面电极,表面电极厚度为8μm。
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CN110054488A (zh) * | 2019-05-14 | 2019-07-26 | 中国科学院新疆理化技术研究所 | 一种含有复相添加剂的热敏陶瓷材料及其制备方法 |
CN112366052A (zh) * | 2020-11-09 | 2021-02-12 | 肇庆市金龙宝电子有限公司 | 一种医疗体温测量用高精度热敏电阻芯片及其制备方法 |
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CN110054488A (zh) * | 2019-05-14 | 2019-07-26 | 中国科学院新疆理化技术研究所 | 一种含有复相添加剂的热敏陶瓷材料及其制备方法 |
CN112366052A (zh) * | 2020-11-09 | 2021-02-12 | 肇庆市金龙宝电子有限公司 | 一种医疗体温测量用高精度热敏电阻芯片及其制备方法 |
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