CN109293354A - 一种ptc陶瓷材料及其制备方法 - Google Patents

一种ptc陶瓷材料及其制备方法 Download PDF

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CN109293354A
CN109293354A CN201811206111.2A CN201811206111A CN109293354A CN 109293354 A CN109293354 A CN 109293354A CN 201811206111 A CN201811206111 A CN 201811206111A CN 109293354 A CN109293354 A CN 109293354A
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ptc
temperature
rate
warming
ceramic material
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CN109293354B (zh
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欧志文
黎何华
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FOSHAN CITY GAOMING OUYI ELECTRONIC MANUFACTURE Co Ltd
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Abstract

本发明公开了一种PTC陶瓷材料及其制备方法，其由以下质量百分比的原料制成：BaTiO355‑60％、PbTiO3 25‑30％、Cr 5‑8％、Ni 3‑6％、MoSi2 2‑3％、ZrB2 1‑2％、CaCO3 0.5‑1％、SiO2 0.4‑0.8％、Al2O3 0.2‑0.4％、Nb2O5 0.1‑0.2％、MnCO3 0.03‑0.05％。本发明加入的MoSi2和ZrB2，提高了BaTiO3基PTC陶瓷材料的居里温度，最高达260℃，本发明通过添加Cr、Ni以及合理科学的制备工艺以达到PTC陶瓷材料的低室温电阻率和优良PTC效应；本发明采用的原料和工艺条件容易实现，材料性能的重复性好，性能优异，应用范围广。

Description

一种PTC陶瓷材料及其制备方法
技术领域
本发明涉及一种PTC陶瓷材料及其制备方法，特别涉及一种BaTiO3基高居里温度PTC陶瓷材料及其制备方法。
背景技术
PTC材料是一种温度敏感性的导电材料，PTC(Positive TemperatureCoefficient)即正温度系数，是指材料电阻率随自身温度升高而增大的一种特性。PTC陶瓷材料在自控温加热和限流等方面应用广泛，但是目前该材料的室温电阻率较高和居里温度较低，一定程度上限制了它的发展，因此，亟需开发一种低室温电阻率和高居里温度的PTC陶瓷材料。
发明内容
本发明的目的在于提供一种PTC陶瓷材料及其制备方法。本发明制得的PTC陶瓷材料不仅具有较高的居里温度，还具有较低的室温电阻率。
为实现上述目的，本发明采用如下的技术方案：
本发明提供了一种PTC陶瓷材料，由以下质量百分比的原料制成：BaTiO3 55-60％、PbTiO3 25-30％、Cr 5-8％、Ni 3-6％、MoSi2 2-3％、ZrB2 1-2％、CaCO3 0.5-1％、SiO20.4-0.8％、Al2O3 0.2-0.4％、Nb2O5 0.1-0.2％、MnCO3 0.03-0.05％。
优选地，所述Cr的纯度为98％以上，粒度为100目。
优选地，所述Ni的纯度为99％以上，粒度为120目。
本发明还提供了一种PTC陶瓷材料的制备方法，包括以下步骤：
(1)按照上述配方配比称取BaTiO3、PbTiO3、Cr、Ni、MoSi2、ZrB2、CaCO3、SiO2、Al2O3、Nb2O5、MnCO3；
(2)将BaTiO3、MoSi2、CaCO3、Al2O3、MnCO3混合，采用料：球：水＝1:1:2-3的质量比将混合料在5000-6000r/min的转速下湿法球磨18-24h，105-125℃下干燥4-8h，即得球磨料A；
(3)将PbTiO3、ZrB2、SiO2、Nb2O5混合，采用料：球：水＝1:1:1.5-2.5的质量比将混合料在4000-5000r/min的转速下湿法球磨24-36h，100-120℃下干燥5-10h，即得球磨料B；
(4)将球磨料A、球磨料B以及Cr、Ni混合，双频超声波交替振荡处理0.5-1h，即得全配料；
(5)取相当于全配料质量7-9％的聚乙烯醇水溶液和0.5-1％的甘油与全配料混合均匀，造粒，过60-90目筛，即得造粒料；
(6)将造粒料在100-150MPa下压制成型，即得素坯；
(7)将素坯在50vt％N2+30％vtAr+20vt％H2气氛下先以2-4℃/min的速率升温至160-220℃，保温20-40min，再以1-3℃/h的速率升温至480-520℃，保温1.5-2.5h，再以2-4℃/h的速率升温至790-830℃，保温1-2h，然后在60vt％N2+20％vtAr+20vt％CO气氛下先以3-5℃/min的速率升温至1120-1180℃，保温20-40min，再以1-3℃/min的速率升温至1330-1390℃，保温1-2h，最后在70vt％N2+20％vtH2+10vt％CO气氛下先以0.5-1.5℃/min的速率降温至1250-1300℃，保温0.5-1.5h，再以0.5-1.5℃/min的速率降温至1200-1250℃，保温0.5-1.5h，再以1-2℃/min的速率降温至1110-1140℃，保温2-3h，自然冷却至室温；
(8)清洗步骤(7)烧结好的瓷片后，在其正反两面均匀涂覆欧姆接触银电极浆料，在440-470℃下烧渗10-15min即可。
优选地，所述聚乙烯醇水溶液的浓度为5-10％。
优选地，所述双频超声波交替振荡处理的条件为：双频超声波交替频率为30-50KHz/80-100KHz，双频超声波交替工作时间为4-6s，超声波功率为150-200W。
本发明的有益效果：
本发明加入的MoSi2和ZrB2，提高了BaTiO3基PTC陶瓷材料的居里温度，最高达260℃，本发明通过添加Cr、Ni以及合理科学的制备工艺以达到PTC陶瓷材料的低室温电阻率和优良PTC效应；本发明采用的原料和工艺条件容易实现，材料性能的重复性好，性能优异，应用范围广。
具体实施方式
实施例1
本实施例提供了一种PTC陶瓷材料，由以下质量百分比的原料制成：BaTiO3 55％、PbTiO3 26％、Cr 8％、Ni 6％、MoSi2 2.5％、ZrB2 1.2％、CaCO3 0.5％、SiO2 0.4％、Al2O30.27％、Nb2O5 0.1％、MnCO3 0.03％。
上述Cr的纯度为98％以上，粒度为100目。
上述Ni的纯度为99％以上，粒度为120目。
本实施例还提供了一种PTC陶瓷材料的制备方法，包括以下步骤：
(1)按照上述配方配比称取BaTiO3、PbTiO3、Cr、Ni、MoSi2、ZrB2、CaCO3、SiO2、Al2O3、Nb2O5、MnCO3；
(2)将BaTiO3、MoSi2、CaCO3、Al2O3、MnCO3混合，采用料：球：水＝1:1:2的质量比将混合料在5000r/min的转速下湿法球磨24h，105℃下干燥8h，即得球磨料A；
(3)将PbTiO3、ZrB2、SiO2、Nb2O5混合，采用料：球：水＝1:1:1.5的质量比将混合料在4000r/min的转速下湿法球磨36h，100℃下干燥10h，即得球磨料B；
(4)将球磨料A、球磨料B以及Cr、Ni混合，在双频超声波交替频率为30KHz/80KHz，双频超声波交替工作时间为4s，超声波功率为150W的条件下双频超声波交替振荡处理1h，即得全配料；
(5)取相当于全配料质量7％的浓度为5％的聚乙烯醇水溶液和0.5％的甘油与全配料混合均匀，造粒，过60目筛，即得造粒料；
(6)将造粒料在100MPa下压制成型，即得素坯；
(7)将素坯在50vt％N2+30％vtAr+20vt％H2气氛下先以2℃/min的速率升温至160℃，保温40min，再以1℃/h的速率升温至480℃，保温2.5h，再以2℃/h的速率升温至790℃，保温2h，然后在60vt％N2+20％vtAr+20vt％CO气氛下先以3℃/min的速率升温至1120℃，保温40min，再以1℃/min的速率升温至1330℃，保温2h，最后在70vt％N2+20％vtH2+10vt％CO气氛下先以0.5℃/min的速率降温至1250℃，保温1.5h，再以0.5℃/min的速率降温至1200℃，保温1.5h，再以1℃/min的速率降温至1110℃，保温3h，自然冷却至室温；
(8)清洗步骤(7)烧结好的瓷片后，在其正反两面均匀涂覆欧姆接触银电极浆料，在440℃下烧渗15min即可。
上述实施例制得的PTC陶瓷材料经测试居里温度为245℃，室温电阻率为68Ω·cm。
实施例2
本实施例提供了一种PTC陶瓷材料，由以下质量百分比的原料制成：BaTiO3 58％、PbTiO3 27％、Cr 6％、Ni 4％、MoSi2 2％、ZrB2 1.5％、CaCO3 0.6％、SiO2 0.5％、Al2O30.2％、Nb2O5 0.16％、MnCO3 0.04％。
上述Cr的纯度为98％以上，粒度为100目。
上述Ni的纯度为99％以上，粒度为120目。
本实施例还提供了一种PTC陶瓷材料的制备方法，包括以下步骤：
(1)按照上述配方配比称取BaTiO3、PbTiO3、Cr、Ni、MoSi2、ZrB2、CaCO3、SiO2、Al2O3、Nb2O5、MnCO3；
(2)将BaTiO3、MoSi2、CaCO3、Al2O3、MnCO3混合，采用料：球：水＝1:1:2.5的质量比将混合料在5500r/min的转速下湿法球磨21h，115℃下干燥6h，即得球磨料A；
(3)将PbTiO3、ZrB2、SiO2、Nb2O5混合，采用料：球：水＝1:1:2的质量比将混合料在4500r/min的转速下湿法球磨30h，110℃下干燥8h，即得球磨料B；
(4)将球磨料A、球磨料B以及Cr、Ni混合，在双频超声波交替频率为40KHz/90KHz，双频超声波交替工作时间为5s，超声波功率为180W的条件下双频超声波交替振荡处理45min，即得全配料；
(5)取相当于全配料质量8％的浓度为7％的聚乙烯醇水溶液和0.6％的甘油与全配料混合均匀，造粒，过80目筛，即得造粒料；
(6)将造粒料在120MPa下压制成型，即得素坯；
(7)将素坯在50vt％N2+30％vtAr+20vt％H2气氛下先以3℃/min的速率升温至190℃，保温30min，再以2℃/h的速率升温至500℃，保温2h，再以3℃/h的速率升温至810℃，保温1.5h，然后在60vt％N2+20％vtAr+20vt％CO气氛下先以4℃/min的速率升温至1150℃，保温30min，再以2℃/min的速率升温至1360℃，保温1.5h，最后在70vt％N2+20％vtH2+10vt％CO气氛下先以1℃/min的速率降温至1280℃，保温1h，再以1℃/min的速率降温至1230℃，保温1h，再以1.5℃/min的速率降温至1120℃，保温2.5h，自然冷却至室温；
(8)清洗步骤(7)烧结好的瓷片后，在其正反两面均匀涂覆欧姆接触银电极浆料，在450℃下烧渗12min即可。
上述实施例制得的PTC陶瓷材料经测试居里温度为260℃，室温电阻率为55Ω·cm。
实施例3
本实施例提供了一种PTC陶瓷材料，由以下质量百分比的原料制成：BaTiO3 60％、PbTiO3 25％、Cr 5％、Ni 5％、MoSi2 2％、ZrB2 1％、CaCO3 0.8％、SiO2 0.6％、Al2O30.4％、Nb2O5 0.15％、MnCO3 0.05％。
上述Cr的纯度为98％以上，粒度为100目。
上述Ni的纯度为99％以上，粒度为120目。
本实施例还提供了一种PTC陶瓷材料的制备方法，包括以下步骤：
(1)按照上述配方配比称取BaTiO3、PbTiO3、Cr、Ni、MoSi2、ZrB2、CaCO3、SiO2、Al2O3、Nb2O5、MnCO3；
(2)将BaTiO3、MoSi2、CaCO3、Al2O3、MnCO3混合，采用料：球：水＝1:1:3的质量比将混合料在6000r/min的转速下湿法球磨18h，125℃下干燥4h，即得球磨料A；
(3)将PbTiO3、ZrB2、SiO2、Nb2O5混合，采用料：球：水＝1:1:2.5的质量比将混合料在5000r/min的转速下湿法球磨24h，120℃下干燥5h，即得球磨料B；
(4)将球磨料A、球磨料B以及Cr、Ni混合，在双频超声波交替频率为50KHz/100KHz，双频超声波交替工作时间为6s，超声波功率为200W的条件下双频超声波交替振荡处理0.5h，即得全配料；
(5)取相当于全配料质量9％的浓度为10％的聚乙烯醇水溶液和1％的甘油与全配料混合均匀，造粒，过90目筛，即得造粒料；
(6)将造粒料在150MPa下压制成型，即得素坯；
(7)将素坯在50vt％N2+30％vtAr+20vt％H2气氛下先以4℃/min的速率升温至220℃，保温20min，再以3℃/h的速率升温至520℃，保温1.5h，再以4℃/h的速率升温至830℃，保温1h，然后在60vt％N2+20％vtAr+20vt％CO气氛下先以5℃/min的速率升温至1180℃，保温20min，再以3℃/min的速率升温至1390℃，保温1h，最后在70vt％N2+20％vtH2+10vt％CO气氛下先以1.5℃/min的速率降温至1300℃，保温0.5h，再以1.5℃/min的速率降温至1250℃，保温0.5h，再以2℃/min的速率降温至1140℃，保温2h，自然冷却至室温；
(8)清洗步骤(7)烧结好的瓷片后，在其正反两面均匀涂覆欧姆接触银电极浆料，在470℃下烧渗10min即可。
上述实施例制得的PTC陶瓷材料经测试居里温度为250℃，室温电阻率为61Ω·cm。

Claims (6)

1.一种PTC陶瓷材料，其特征在于，由以下质量百分比的原料制成：BaTiO3 55-60％、PbTiO3 25-30％、Cr 5-8％、Ni 3-6％、MoSi2 2-3％、ZrB2 1-2％、CaCO3 0.5-1％、SiO2 0.4-0.8％、Al2O3 0.2-0.4％、Nb2O5 0.1-0.2％、MnCO3 0.03-0.05％。
2.根据权利要求1所述的一种PTC陶瓷材料，其特征在于，所述Cr的纯度为98％以上，粒度为100目。
3.根据权利要求1所述的一种PTC陶瓷材料，其特征在于，所述Ni的纯度为99％以上，粒度为120目。
4.一种如权利要求1-3任一项所述的PTC陶瓷材料的制备方法，其特征在于，包括以下步骤：
(1)按照上述配方配比称取BaTiO3、PbTiO3、Cr、Ni、MoSi2、ZrB2、CaCO3、SiO2、Al2O3、Nb2O5、MnCO3；
(2)将BaTiO3、MoSi2、CaCO3、Al2O3、MnCO3混合，采用料：球：水＝1:1:2-3的质量比将混合料在5000-6000r/min的转速下湿法球磨18-24h，105-125℃下干燥4-8h，即得球磨料A；
(3)将PbTiO3、ZrB2、SiO2、Nb2O5混合，采用料：球：水＝1:1:1.5-2.5的质量比将混合料在4000-5000r/min的转速下湿法球磨24-36h，100-120℃下干燥5-10h，即得球磨料B；
(4)将球磨料A、球磨料B以及Cr、Ni混合，双频超声波交替振荡处理0.5-1h，即得全配料；
(5)取相当于全配料质量7-9％的聚乙烯醇水溶液和0.5-1％的甘油与全配料混合均匀，造粒，过60-90目筛，即得造粒料；
(6)将造粒料在100-150MPa下压制成型，即得素坯；
(7)将素坯在50vt％N2+30％vtAr+20vt％H2气氛下先以2-4℃/min的速率升温至160-220℃，保温20-40min，再以1-3℃/h的速率升温至480-520℃，保温1.5-2.5h，再以2-4℃/h的速率升温至790-830℃，保温1-2h，然后在60vt％N2+20％vtAr+20vt％CO气氛下先以3-5℃/min的速率升温至1120-1180℃，保温20-40min，再以1-3℃/min的速率升温至1330-1390℃，保温1-2h，最后在70vt％N2+20％vtH2+10vt％CO气氛下先以0.5-1.5℃/min的速率降温至1250-1300℃，保温0.5-1.5h，再以0.5-1.5℃/min的速率降温至1200-1250℃，保温0.5-1.5h，再以1-2℃/min的速率降温至1110-1140℃，保温2-3h，自然冷却至室温；
(8)清洗步骤(7)烧结好的瓷片后，在其正反两面均匀涂覆欧姆接触银电极浆料，在440-470℃下烧渗10-15min即可。
5.根据权利要求4所述的PTC陶瓷材料的制备方法，其特征在于，所述聚乙烯醇水溶液的浓度为5-10％。
6.根据权利要求4所述的PTC陶瓷材料的制备方法，其特征在于，所述双频超声波交替振荡处理的条件为：双频超声波交替频率为30-50KHz/80-100KHz，双频超声波交替工作时间为4-6s，超声波功率为150-200W。
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