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CN106145933A - 一种高居里温度（Tc > 190℃）低铅PTCR陶瓷材料制备方法 - Google Patents

一种高居里温度（Tc > 190℃）低铅PTCR陶瓷材料制备方法 Download PDF

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CN106145933A
CN106145933A CN201610406748.0A CN201610406748A CN106145933A CN 106145933 A CN106145933 A CN 106145933A CN 201610406748 A CN201610406748 A CN 201610406748A CN 106145933 A CN106145933 A CN 106145933A
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ptcr
ceramic material
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朱兴文
任慧茹
卢胤
牛伟鉴
李晨
钟史伟
周晓
姜文中
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University of Shanghai for Science and Technology
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Abstract

本发明涉及一种高居里温度(Tc>190℃)低铅PTCR陶瓷材料制备方法，该方法采用以下材料：x(Bi1/2Na1/2)TiO3‑yPbTiO3‑(1‑x‑y)BaTiO3粉体；Nb2O5、La2O3、Sb2O3、Sm2O3、Nd2O3化合物中的一种或多种为半导化剂；MnO2、MnCO3或Mn(NO3)2中的一种或多种为PTCR效应调节剂；Li2CO3、Al2O3和TiO2为烧结助剂，采用的工艺是：将上述所列材料压制的圆片在N2气氛中1200‑1350℃下保温15～120分钟烧结，使其充分烧结和实现固相反应；对烧结后的圆片表面进行研磨，上电极，制得PTCR陶瓷材料。该陶瓷材料，其室温电阻率低至1×103Ω·cm，居里温度Tc在190～260℃，其居里温度和室温电阻率性能不仅能达到实用化要求，而且该材料中含铅量是传统的相同性能的PTCR陶瓷材料的15～25％，减少了其对人体和环境的危害。

Description

一种高居里温度（Tc > 190℃）低铅PTCR陶瓷材料制备方法
技术领域
本发明涉及一种高居里温度（Tc > 190℃）低铅正温度系数热敏电阻（PTCR）陶瓷材料制备方法，属于电子陶瓷材料技术领域。
背景技术
目前广泛使用的高居里温度PTCR陶瓷均采用BaTiO3－PbTiO3体系，居里温度Tc越高，PTCR陶瓷材料中的铅含量越多。在空调中的加热元件采用PTCR陶瓷热敏元件，其居里温度Tc为250℃，元件中的铅的含量超过30wt%，铅对人体和环境有严重的危害。
PTCR陶瓷材料的无铅化研究始于上世纪80年代末，以铁电(Na,Bi)TiO3与BaTiO3固溶，获得(Ba,Bi,Na)TiO3高温PTCR陶瓷材料。(Na,Bi)TiO3是一种具有复合钙钛矿结构的驰豫型铁电体，其居里温度Tc为320℃，可与BaTiO3以任意比例固溶。当用(Na,Bi)TiO3取代PbTiO3来制备PTCR材料时，(Na,Bi)TiO3固溶量从10mol%上升至45mol%，材料的居里温度Tc从180℃升至209℃，如果(Na,Bi)TiO3固溶量为80mol%，其居里温度为220℃左右，该材料的室温电阻率增大，PTC效应差，因此BNT-BaTiO3体系的无铅PTCR材料遭遇了一定的发展瓶颈，无法达到实用化的要求。本发明的方法采用(Na,Bi)TiO3—PbTiO3，制备PTCR材料，其居里温度和室温电阻率性能不仅能达到实用化要求，而且PTCR材料中含铅低，减少其对环境的危害。
发明内容
本发明的目的在于提供一种高居里温度（Tc > 190℃）低铅PTCR陶瓷材料制备方法，该方法制备的材料含铅量低，能减少环境的危害。
为达到上述目的，本发明采用下述技术方案：
本发明提出的一种高居里温度（Tc > 190℃）低铅PTCR陶瓷材料制备方法，该方法采用以下材料：x(Bi1/2Na1/2)TiO3- yPbTiO3-(1-x-y) BaTiO3粉体；Nb2O5、La2O3、Sb2O3、Sm2O3、Nd2O3化合物中的一种或多种为半导化剂； MnO2、MnCO3或Mn(NO3)2中的一种或多种为PTCR效应调节剂； Li2CO3、Al2O3和TiO2为烧结助剂，然后通过掺杂，烧结，压制，固相反应制得高居里温度（Tc > 190℃）低铅PTCR陶瓷材料，其特征在于具有以下的配方和工艺步骤：
A.取材料x(Bi1/2Na1/2)TiO3- yPbTiO3-(1-x-y)BaTiO 3，其中x =0.05～0.50, y =0.01～0.15 ；然后向材料中掺入半导化剂和PTCR效应调节剂，所述的半导化剂为Nb2O5、La2O3、Sb2O3、Sm2O3、Nd2O3化合物中的一种或多种，所述的PTCR效应调节剂为MnO2、MnCO3或Mn(NO3)2中的一种或多种，所述的PTCR效应调节剂掺入量为上述材料的0.05～0.80 atom% ；再向上述预合成的粉体加入烧结助剂，所述的烧结助剂为0～0.5 atom%Li2CO3、0～0.50 atom%Al2O3和0～3.5 atom% TiO2；
B.按原子比Bi2O3：Na2O：TiO2＝0.5：0.5：1.0和按原子比PbO：TiO2＝1.0：1.0的比例称取上述两种分析纯的原料，以玛瑙球和酒精为介质，将上述原料混合，在磨机中球磨3～72小时，将烘干后混合料分别放在950℃和1000℃温度下充分煅烧，实现固相反应，煅烧时间为0.5～4.0小时，分别获得(Bi1/2Na1/2)TiO3和PbTiO3粉体；
C. 称取上述步骤A所列材料和上述步骤B中获得(Bi1/2Na1/2)TiO3和PbTiO3粉体，以玛瑙球和酒精为介质，在磨机中球磨12～72小时，得到烘干后的粉末；再加入烘干后的粉末重量的3.0～12.0wt% 的浓度为10wt%的PVA，造粒，再以5～15 MPa的压力压制成Φ10×2.0mm的圆片；
D.将压制好的圆片在N2气氛中1200-1350℃下保温15～120分钟烧结，使其充分烧结；对烧结后的的圆片表面进行研磨，上电极，制得高居里温度低铅（Tc > 190℃）PTCR陶瓷材料。
与现有技术相比，本发明的有益效果是:本发明的方法采用(Na,Bi)TiO3－PbTiO3制备高居里温度（Tc > 190℃）低铅PTCR陶瓷材料，其室温电阻率低至1×103Ω·cm，居里温度Tc在190～260℃，升阻比最高达5×104，非线性系数α 达5～15％，其居里温度和室温电阻率性能不仅能达到实用化要求，而且PTCR材料中含铅低，以高居里温度Tc = 250℃的材料为例，本发明的材料的铅含量比传统的PTCR材料降低约80%，减少其对人体和环境的危害。
具体实施方式
结合以下具体实施实例，对本发明作进一步详细说明。
实施例1
本实施例1按x(Bi1/2Na1/2)TiO3-0.07PbTiO3-(0.93-x)BaTiO3+0.0005Nb2O5+0.00167Al2O3 +0.01TiO2+0.001 Li2CO3进行配料，其中x =0.05～0.50，换算出所需各粉料的质量，然后准确称量，称量质量如下表1：
以玛瑙球和去离子水为介质，在行星磨上以225转/分的转速球磨（料：玛瑙球：去离子水水＝1：2.5：1.5）24小时，得到烘干后的粉末，再加入烘干后的粉末质量的8wt%的浓度为10wt%的PVA，造粒，以10MPa的压力压制Φ10×2.0mm的圆片。所压制的圆片在N2气氛中1300℃下保温60分钟烧结，经充分烧结，实现固相反应，对烧结后的的圆片表面进行研磨，上电极，制得高居里温度（Tc > 190℃）低铅PTCR陶瓷材料。
以1℃/min的升温速率加热上述陶瓷材料，测试其电阻－温度特性，所得结果如表2所示：
由上述表1和表2看出，本发明的PTCR材料的居里温度随BNT含量的增加而上升。
实施例2
本实施例2按0.30(Bi1/2Na1/2)TiO3—yPbTiO3—(0.7-y)BaTiO3+0.0005Nb2O5+0.00167Al2O3 +0.01 TiO2+0.001 L2CO3进行配料，其中y =0.01～0.15，换算出所需各粉料的质量，然后准确称量，称量质量如下表3：
以玛瑙球和去离子水为介质，在行星磨上以225转/分的转速球磨（料：玛瑙球：去离子水＝1：2.5：1.5）24小时，得到烘干后的粉末，再加入烘干后的粉末重量的8wt%的浓度为10wt%的PVA，造粒，以10MPa的压力压制Φ10×2.0mm的圆片；将压制的圆片在N2气氛中1300℃下保温60分钟烧结，经充分烧结，实现固相反应，对烧结后的的圆片表面进行研磨，上电极，制得高居里温度（Tc > 190℃）低铅PTCR陶瓷材料。
以1℃/min的升温速率加热上述陶瓷材料，测试其电阻－温度特性，所得结果如表4所示：
由上述表3和表4看出，在BNT含量为30 mol%、PbTiO3固溶量为7 mol%时，本发明的PTCR材料的Tc温度接近230℃，且材料的PTC性能无明显恶化，而传统的PTCR材料要达到此性能，PbTiO3的固溶量高达30 mol%。
实施例3
本实施例按0.30(Bi1/2Na1/2)TiO3-0.07PbTiO3-0.63BaTiO3+0.0005Nb2O5+0.00167Al2O3 +0.01TiO2 +0.001Li2CO3+m MnO2进行配料，其中m =0.0002～0.0015，换算出所需各粉料的质量，然后准确称量，称量质量如下表5：
以玛瑙球和去离子水为介质，在行星磨上以225转/分的转速球（料：玛瑙球：去离子水水＝1：2.5：1.5）24小时，得到烘干后的粉末，再加入烘干后的粉末质量的8wt%的浓度为10wt%的PVA，造粒，以10MPa的压力压制Φ10×2.0mm的圆片。所压制的圆片在N2气氛中1300℃下保温60分钟烧结，经充分烧结，实现固相反应，对烧结后的的圆片表面进行研磨，上电极，制得高居里温度（Tc > 190℃）低铅PTCR陶瓷材料。
以1℃/min的升温速率加热上述陶瓷材料，测试其电阻－温度特性，所得结果如表6所示：
由上述表5和表6看出，本发明的PTCR材料中添加适量的MnO2可以提高该材料的PTC效应。

Claims (1)

1. 一种高居里温度（Tc > 190℃）低铅PTCR陶瓷材料制备方法，该方法采用以下材料：x(Bi1/2Na1/2)TiO3- yPbTiO3-(1-x-y) BaTiO3粉体；Nb2O5、La2O3、Sb2O3、Sm2O3、Nd2O3化合物中的一种或多种为半导化剂； MnO2、MnCO3或Mn(NO3)2中的一种或多种为PTCR效应调节剂；Li2CO3、Al2O3和TiO2为烧结助剂，然后通过掺杂，烧结，压制，固相反应制得高居里温度（Tc >190℃）低铅PTCR陶瓷材料，其特征在于具有以下步骤：
A.取材料x(Bi1/2Na1/2)TiO3- yPbTiO3-(1-x-y)BaTiO 3，其中x =0.05～0.50, y =0.01～0.15 ；然后向材料中掺入半导化剂和PTCR效应调节剂，所述的半导化剂为Nb2O5、La2O3、Sb2O3、Sm2O3、Nd2O3化合物中的一种或多种，所述的PTCR效应调节剂为MnO2、MnCO3或Mn(NO3)2中的一种或多种，所述的PTCR效应调节剂掺入量为上述材料的0.05～0.80 atom%；再向上述预合成的粉体加入烧结助剂，所述的烧结助剂为0～0.5 atom%Li2CO3、0～0.50 atom%Al2O3和0～3.5 atom% TiO2；
B.按原子比Bi2O3：Na2O：TiO2＝0.5：0.5：1.0和按原子比PbO：TiO2＝1.0：1.0的比例称取上述两种分析纯的原料，以玛瑙球和酒精为介质，将上述原料混合，在磨机中球磨，球磨3～72小时，将烘干后混合料分别放在950℃和1100℃温度下充分煅烧，以实现固相反应，煅烧时间为0.5～4.0小时，分别获得(Bi1/2Na1/2)TiO3和PbTiO3粉体；
C. 称取上述步骤A所列材料和上述步骤B中获得(Bi1/2Na1/2)TiO3和PbTiO3粉体，以玛瑙球和酒精或去离子水为介质，在磨机中球磨12～72小时，得到烘干后的粉末；再加入烘干后的粉末重量的3.0～12.0wt% 的浓度为10wt%的PVA，造粒，再以5～15 MPa的压力压制成Φ10×2.0mm的圆片；
D.将压制好的压制的圆片在N2气氛中1200-1350℃下保温15～120分钟烧结，使其充分烧结和实现固相反应；对烧结后的的圆片表面进行研磨，上电极，制得高居里温度（Tc >190℃）低铅PTCR陶瓷材料。
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CN113475755A (zh) * 2021-08-06 2021-10-08 深圳市基克纳科技有限公司 发热体及其制备方法和雾化器、雾化装置

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