CN112028623A - 杂原子改性钛酸盐热敏电阻材料的制备方法 - Google Patents
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Abstract
本发明公开了一种杂原子改性钛酸盐热敏电阻材料的制备方法。本发明调整结炉升降温速率、最高温度、保温时间;降低了800℃以前用的升温速率,有助于在造粒时加入的粘合剂完全排出,防止未排出的粘合剂由于缺氧碳化在瓷体内,造成耐压降低;提升了800℃之后的升温速率,降低了烧结的最高温度,防止升温过慢造成晶粒异常生长;缩短保温时间可防止瓷体在高温下变形,晶粒异常生长;降低降温速率,有助于产品在降温时改善晶粒结构、使其均匀,提高材料阻温特性,提高材料B值常数,增强耐电压Vb。
Description
技术领域
本发明涉及材料技术领域,尤其是一种杂原子改性钛酸盐热敏电阻材料的制备方法。
背景技术
现有陶瓷热敏电阻PTC元件再制作时,一般都是直接进料BaTiO3 材料再加入CaCO3,SrCO3以及施主原材料及受主原材料经过球磨→混合→造粒制备而出,或者进料BaCO3、SrCO3、CaCO3、施主原材料及受主原材料一起球磨→混合→预烧→二次球磨→造粒制备而出,前者工艺制备出陶瓷热敏电阻PTC元件晶粒结构不均匀、材料B值常数低、耐电压Vb低;后者制备陶瓷热敏电阻PTC元件工艺复杂,生产周期较长,不能及时应对订单。
于是,有鉴于此,针对现有的工艺流程,提供一种杂原子改性钛酸盐热敏电阻材料的制备工艺,以期达到更具有更加经济实用价值性的目的。
发明内容
本发明的目的在于,提供一种杂原子改性钛酸盐热敏电阻材料的制备方法,它能解决晶粒结构不均匀、材料B值常数低、耐电压Vb 低、生产工艺复杂、生产周期长等不利因素等问题。
本发明是这样实现的:杂原子改性钛酸盐热敏电阻材料的制备方法,包括如下步骤:
1)将钛酸盐体系中加入微量元素与掺杂过渡元素进行球磨、混合,并加入PVA胶进行造粒;
2)将经过球磨后的物料进行烧结,烧结炉升温在800℃以前的降温速率为200℃/小时,到达800℃后按照升温速率为300℃/小时,将温度升高至1320-1330℃,然后保温1小时,再按照200℃/小时的降温速率进行降温,直至室温。
所述的钛酸盐体系为BaTiO3、CaTiO3及SrTiO3质量比 70-80∶10-20∶5-15。
所述的微量元素的载体是SiO2,掺杂过渡元素的载体是TiO2,其中,每1mol钛酸盐体系中加入0.005mol微量元素的载体和0.03mol 掺杂过渡元素的载体。
PVA胶的加入量为材料净重量的10-15%,造粒的粒度大小为150 目
所述的BaTiO3、CaTiO3及SrTiO3分别是采用BaCO3与TiO2、CaCO3与TiO2、SrCO3与TiO2反应获得,参与反应的BaCO3与TiO2、CaCO3与 TiO2、SrCO3与TiO2的摩尔比均是1∶1.01-1.03。本发明中,在生成钛酸盐的体系中,使TiO2过量,最终是以Ti的形式存在于晶界中,TiO2过量可以改善晶粒结构,结果是可以增加耐压。
如果需要不同参数(如居里温度)的产品,可以调整SrTiO3的量改变居里温度,增加SrTiO3的量,减少BaTiO3的量,可以降低居里温度,反之,增加居里温度。
由于采用了上述技术方案,与现有技术相比,本发明调整结炉升降温速率、最高温度、保温时间;降低了800℃以前用的升温速率,有助于在造粒时加入的粘合剂完全排出,防止未排出的粘合剂由于缺氧碳化在瓷体内,造成耐压降低;提升了800℃之后的升温速率,降低了烧结的最高温度,防止升温过慢造成晶粒异常生长;缩短保温时间可防止瓷体在高温下变形,晶粒异常生长;降低降温速率,有助于产品在降温时改善晶粒结构、使其均匀,提高材料阻温特性,提高材料B值常数,增强耐电压Vb。
附图说明
图1为本发明的示例的性能对比。
具体实施方式
本发明的实施例:杂原子改性钛酸盐热敏电阻材料的制备方法,本实施例要制备的材料为一居里温度(开关温度)100℃,产品尺寸D=12mm*T=2.5mm,阻值80Ω,耐压Vb大于800V的陶瓷热敏电阻(PTC) 材料,包括如下步骤:
1)按摩尔比1:1.02分别配制BaCO3及TiO2、CaCO3及TiO2、SrCO3及TiO2,经过预烧后生成BaTiO3、CaTiO3、SrTiO3备用;
2)将BaTiO3、CaTiO3及SrTiO3按照75∶15∶10的比例配置成钛酸盐体系,每1mol钛酸盐体系中加入0.005mol SiO2和0.03mol TiO2。后进行球磨、混合,并加入13%的PVA胶进行造粒;
2)将经过球磨后的物料进行烧结,烧结炉升温在800℃以前的降温速率为200℃/小时,到达800℃后按照升温速率为300℃/小时,将温度升高至1320-1330℃,然后保温1小时,再按照200℃/小时的降温速率进行降温,直至室温。
将获得的产品进行检测
本试验以加入微量元素提高耐压为例:
原配比 BaxSr0.08Ca0.12Ti1.01Y0.002
现配比 BaxSr0.08Ca0.12Ti1.01Y0.002Si0.005
R25(常温电阻值)及Vb(破坏电压)与原配比对比Vb提升22.1%。
Claims (5)
1.一种杂原子改性钛酸盐热敏电阻材料的制备方法,其特征在于,包括如下步骤:
1)将钛酸盐体系中加入微量元素与掺杂过渡元素,进行球磨、混合,并加入PVA胶进行造粒;
2)将经过球磨后的物料进行烧结,烧结炉升温在800℃以前的降温速率为200℃/小时,到达800℃后按照升温速率为300℃/小时,将温度升高至1320-1330℃,然后保温1小时,再按照200℃/小时的降温速率进行降温,直至室温。
2.根据权利要求1所述的杂原子改性钛酸盐热敏电阻材料的制备方法,其特征在于:所述的钛酸盐体系为BaTiO3、CaTiO3及SrTiO3质量比70-80∶10-20∶5-15。
3.根据权利要求1所述的杂原子改性钛酸盐热敏电阻材料的制备方法,其特征在于:所述的微量元素的载体是SiO2,掺杂过渡元素的载体是TiO2,其中,每1mol钛酸盐体系中加入0.005mol微量元素的载体和0.03mol掺杂过渡元素的载体。
4.根据权利要求1所述的杂原子改性钛酸盐热敏电阻材料的制备方法,其特征在于:PVA胶的加入量为材料净重量的10-15%,造粒的粒度大小为150目。
5.根据权利要求1或2所述的杂原子改性钛酸盐热敏电阻材料的制备方法,其特征在于:所述的BaTiO3、CaTiO3及SrTiO3分别是采用BaCO3与TiO2、CaCO3与TiO2、SrCO3与TiO2反应获得,参与反应的BaCO3与TiO2、CaCO3与TiO2、SrCO3与TiO2的摩尔比均是1∶1.01-1.03。
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CN112608146A (zh) * | 2020-12-31 | 2021-04-06 | 马鞍山巨华电子科技有限公司 | 一种具有耐高压性能的新型环保ptc热敏电阻 |
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