CN110698189A - 一种镧离子掺杂的深低温热敏电阻材料及制备方法 - Google Patents

一种镧离子掺杂的深低温热敏电阻材料及制备方法 Download PDF

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CN110698189A
CN110698189A CN201911117201.9A CN201911117201A CN110698189A CN 110698189 A CN110698189 A CN 110698189A CN 201911117201 A CN201911117201 A CN 201911117201A CN 110698189 A CN110698189 A CN 110698189A
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张惠敏
常爱民
范庆梅
孙家林
王强
刘思学
代树武
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

本发明公开了一种镧离子掺杂的深低温热敏电阻材料及制备方法，该电阻材料以锰、镍、铁、镧的氧化物为原料，采用固相法进行制备，将混合后的粉体经过煅烧、研磨、烧结制得。与市面上现有的NTC热敏电阻相比，该电阻材料可以在15 K条件下工作。其电性能参数为：R70K=160 KΩ∙cm，R90K=680 KΩ∙cm。测温区间在15 K‑280 K之间，解决了低温热敏电阻测温范围较窄，应用范围不够广泛的问题。由该材料制得的热敏电阻期间可以应用于航空航天等深低温领域。

Description

一种镧离子掺杂的深低温热敏电阻材料及制备方法
技术领域
本发明涉及一种镧离子掺杂的深低温热敏电阻材料及制备方法，基于该新型材料电性能参数，其适用于深低温、航天、外太空温度探测领域。
背景技术
负温度系数(NTC)热敏电阻按照实际医用温区可以分为以下三种：低温区(0-213.15K)，常温区(213.15-623.15K)和高温区(623.15-1273.15K)。目前市面上绝大部分所售卖的负温度系数(NTC)热敏电阻为常温型，至于低温型的电阻器少之又少，即便有那么几种产品具有低温探测功能仍然不能够满足航空航天以及深海测温的需求，其根本原因在于，当外部温度环境极低时大部分电阻器中阻值趋于无穷大，难以实现电学信号的传输。
发明内容
本发明目的在于，提供一种镧离子掺杂的深低温热敏电阻材料及制备方法，该材料是由MnO2，NiO，Fe2O3和La2O3为原料进行混合，通过球磨、煅烧、研磨、成型、高温烧结制成La离子掺杂的深低温热敏电阻材料，通过增加La离子含量，降低电阻器件的低温电阻以及低温测温范围内的B值。当La离子含量达到最大时，测试温度可低至15K，R77K＝160KΩ·cm，B77/90＝290.38K，由此实现了测量温度，阻值，B值的最低值。同时制得的热敏电阻测温区间可从15K到280K，从而解决了MF5602型产品测温区间较窄，应用范围较小的核心问题。该材料B值波动范围小，即B77/90＝290.38-311.63K，材料体系十分稳定，与军工需求相一致。
本发明所述的一种镧离子掺杂的深低温热敏电阻材料，该材料是由MnO2、NiO、Fe2O3和La2O3为原料，按摩尔比MnO2:NiO:Fe2O3:La2O3＝0.45-2:0.8-3:0.1-0.6:1-4.15，通过球磨、煅烧、研磨、成型、高温烧结制成。
所述一种镧离子掺杂的深低温热敏电阻材料的制备方法，按下列步骤进行：
a、粉体配比：以MnO2、NiO、Fe2O3和La2O3为原料，按摩尔比MnO2:NiO:Fe2O3:La2O3＝0.45-2:0.8-3:0.1-0.6:1-4.15分别进行称量，置入聚四氟乙烯罐中进行球磨，时间8h-12h，于温度100℃-150℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中聚四氟乙烯罐中的玛瑙球、粉体、分散剂丙酮与乙醚的混合质量比为1-4:1:1，分散剂丙酮与乙醚混合体积比为1:9-9:1；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度900℃-1100℃下煅烧1-4h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨2-6h；
d、成型：将步骤c复合后的粉体于280MP-350MP下冷等静压140s-175s后成型；
e、烧结：将步骤d成型块体置入含有MnO2、Fe2O3、La2O3中一种或两种或三种的Al2O3粉体中，于温度1150-1300℃下烧结1-4h，得到镧离子掺杂的深低温热敏电阻材料。
本发明所述的一种镧离子掺杂的深低温热敏电阻材料及制备方法，该材料具有以下特点：
1、最低测试温度可达15K；
2、温度测试适用范围广：15-280K；
3、B77/90值及其波动范围小：B77/90＝290.38-311.63K，材料体系稳定；
4、低温下阻值较低R77K＝160KΩ·cm。
具体实施方式
以下结合实施例对本发明作进一步详细说明，在不仅限于所给出的实施例。
实施例1
a、粉体配比：按摩尔比MnO2:NiO:Fe2O3:La2O3＝1.15:1.3:0.55:3分别进行称量，置入聚四氟乙烯罐中，控制玛瑙球、粉体、分散剂丙酮与乙醚混合质量比为1:1:1，进行球磨，时间8h，，于温度100℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中分散剂丙酮与乙醚混合体积比为1:9；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度900℃下煅烧4h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨2h；
d、成型：将步骤c复合后的粉体于280MP下冷等静压140s后成型；
e、烧结：将步骤d成型块体置入含有MnO2的Al2O3粉体中，于温度1150℃下烧结4h，得到La离子掺杂的深低温热敏电阻材料；
电极制备：将银浆涂覆于镧离子掺杂的深低温热敏电阻材料正反两面，置入钟罩炉中在温度800℃下烧结60min；将经过电极制备的镧离子掺杂的深低温热敏电阻材料进行电学性能测试，电学参数为：R90K＝680KΩ·cm，R77K＝1.2MΩ·cm，B77/90＝302.78K。
实施例2
a、粉体配比：按摩尔比MnO2:NiO:Fe2O3:La2O3＝2:1.9:0.1:2.5分别进行称量，置入聚四氟乙烯罐中，控制玛瑙球、粉体、分散剂丙酮与乙醚混合质量比为1.5:1:1，进行球磨，时间9h，于温度110℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中分散剂丙酮与乙醚混合体积比为2:8；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度950℃下煅烧3.5h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨2.5h；
d、成型：将步骤c复合后的粉体于290MP下冷等静压145s后成型；
e、烧结：将步骤d成型块体置入含有Fe2O3的Al2O3粉体中，于温度1175℃下烧结3.5h，得到La离子掺杂的深低温热敏电阻材料；
电极制备：将银浆涂覆于镧离子掺杂的深低温热敏电阻材料正反两面，置入钟罩炉中在温度800℃下烧结60min；将经过电极制备的镧离子掺杂的深低温热敏电阻材料进行电学性能测试，电学参数为：R90K＝1.3MΩ·cm，R77K＝2.3MΩ·cm，B77/90＝303.21K。
实施例3
a、粉体配比：按摩尔比MnO2:NiO:Fe2O3:La2O3＝1:1:0.6:4分别进行称量，置入聚四氟乙烯罐中，控制玛瑙球、粉体、分散剂丙酮与乙醚混合质量比为2:1:1，进行球磨，时间9h，于温度110℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中分散剂丙酮与乙醚混合体积比为3:7；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度950℃下煅烧3h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨3h；
d、成型：将步骤c复合后的粉体于300MP下冷等静压150s后成型；
e、烧结：将步骤d成型块体置入含有La2O3的Al2O3粉体中，于温度1225℃下烧结3h，得到La离子掺杂的深低温热敏电阻材料；
电极制备：将银浆涂覆于镧离子掺杂的深低温热敏电阻材料正反两面，置入钟罩炉中在温度800℃下烧结60min；将经过电极制备的镧离子掺杂的深低温热敏电阻材料进行电学性能测试，电学参数为：R90K＝160.69KΩ·cm，R77K＝280.35KΩ·cm，B77/90＝296.7K。
实施例4
a、粉体配比：按摩尔比MnO2:NiO:Fe2O3:La2O3＝0.45:1.3:0.55:3.5分别进行称量，置入聚四氟乙烯罐中，控制玛瑙球、粉体、分散剂丙酮与乙醚混合质量比为2.5:1:1，进行球磨，时间10h，于温度125℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中分散剂丙酮与乙醚混合体积比为5:5；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度1000℃下煅烧2.5h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨4h；
d、成型：将步骤c复合后的粉体于315MP下冷等静压160s后成型；
e、烧结：将步骤d成型块体置入含有Fe2O3和La2O3的Al2O3粉体中，于温度1200℃下烧结2.5h，得到La离子掺杂的深低温热敏电阻材料；
电极制备：将银浆涂覆于镧离子掺杂的深低温热敏电阻材料正反两面，置入钟罩炉中在温度800℃下烧结60min；将经过电极制备的镧离子掺杂的深低温热敏电阻材料进行电学性能测试，电学参数为：R90K＝543.66KΩ·cm，R77K＝953.4KΩ·cm，B77/90＝299.43K。
实施例5
a、粉体配比：按摩尔比MnO2:NiO:Fe2O3:La2O3＝1:3:0.3:1分别进行称量，置入聚四氟乙烯罐中，控制玛瑙球、粉体、分散剂丙酮与乙醚混合质量比为3:1:1，进行球磨，时间11h，于温度140℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中分散剂丙酮与乙醚混合体积比为7:3；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度1050℃下煅烧2h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨5h；
d、成型：将步骤c复合后的粉体于330MP下冷等静压165s后成型；
e、烧结：将步骤d成型块体置入含有MnO2和Fe2O3的Al2O3粉体中，于温度1250℃下烧结2h，得到La离子掺杂的深低温热敏电阻材料；
电极制备：将银浆涂覆于镧离子掺杂的深低温热敏电阻材料正反两面，置入钟罩炉中在温度800℃下烧结60min；将经过电极制备的镧离子掺杂的深低温热敏电阻材料进行电学性能测试，电学参数为：R90K＝6.34MΩ·cm，R77K＝11.38MΩ·cm，B77/90＝311.63K。
实施例6
a、粉体配比：按摩尔比MnO2:NiO:Fe2O3:La2O3＝1.7:2.3:0.1:2分别进行称量，置入聚四氟乙烯罐中，控制玛瑙球、粉体、分散剂丙酮与乙醚混合质量比为3.5:1:1，进行球磨，时间11h，于温度140℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中分散剂丙酮与乙醚混合体积比为8:2；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度1050℃下煅烧1.5h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨5.5h；
d、成型：将步骤c复合后的粉体于340MP下冷等静压170s后成型；
e、烧结：将步骤d成型块体置入含有MnO2和La2O3的Al2O3粉体中，于温度1275℃下烧结1.5h，得到La离子掺杂的深低温热敏电阻材料；
电极制备：将银浆涂覆于镧离子掺杂的深低温热敏电阻材料正反两面，置入钟罩炉中在温度800℃下烧结60min；将经过电极制备的镧离子掺杂的深低温热敏电阻材料进行电学性能测试，电学参数为：R90K＝3.03MΩ·cm，R77K＝5.4MΩ·cm，B77/90＝308.58K。
实施例7
a、粉体配比：按摩尔比MnO2:NiO:Fe2O3:La2O3＝0.55:0.8:0.55:4.15分别进行称量，置入聚四氟乙烯罐中，控制玛瑙球、粉体、分散剂丙酮与乙醚混合质量比为4:1:1，进行球磨，时间12h，于温度150℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中分散剂丙酮与乙醚混合体积比为9:1；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度1100℃下煅烧1h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨6h；
d、成型：将步骤c复合后的粉体于350MP下冷等静压175s后成型；
e、烧结：将步骤d成型块体置入含有MnO2、Fe2O3和Fe2O3的Al2O3粉体中，于温度1300℃下烧结1h，得到La离子掺杂的深低温热敏电阻材料。
电极制备：将银浆涂覆于镧离子掺杂的深低温热敏电阻材料正反两面，置入钟罩炉中在温度800℃下烧结60min；将经过电极制备的镧离子掺杂的深低温热敏电阻材料进行电学性能测试，电学参数为：R77K＝160KΩ·cm，R90K＝92.8KΩ·cm，B77/90＝290.38K。
实施例1-7得到的任意一种La离子掺杂的深低温热敏电阻材料均为尖晶石结构，所有陶瓷片微观形貌均显示出良好的致密性，成瓷、一致性与复现性较好，低温测量温区较广。

Claims (2)

1.一种镧离子掺杂的深低温热敏电阻材料，其特征在于该材料是由MnO2、NiO、Fe2O3和La2O3为原料，按摩尔比MnO2:NiO: Fe2O3: La2O3=0.45-2:0.8-3:0.1-0.6:1-4.15，通过球磨、煅烧、研磨、成型、高温烧结制成。
2.根据权利要求1所述的一种镧离子掺杂的深低温热敏电阻材料的制备方法，其特征在于按下列步骤进行：
a、粉体配比：以MnO2、NiO、Fe2O3和La2O3为原料，按摩尔比MnO2:NiO: Fe2O3: La2O3=0.45-2:0.8-3:0.1-0.6:1-4.15分别进行称量，置入聚四氟乙烯罐中进行球磨，时间8h-12h，于温度100℃-150℃下干燥，得到Mn-Ni-Fe-La-O混合粉体，其中聚四氟乙烯罐中的玛瑙球、粉体、分散剂丙酮与乙醚的混合质量比为1-4:1:1，分散剂丙酮与乙醚混合体积比为1:9-9:1；
b、煅烧：将步骤a中得到的Mn-Ni-Fe-La-O混合粉体置于温度900℃-1100℃下煅烧1-4h，得到尖晶石结构的Mn-Ni-Fe-La-O粉体；
c、混合研磨：将步骤b煅烧后的尖晶石Mn-Ni-Fe-La-O粉体置入玛瑙研钵中研磨2-6h；
d、成型：将步骤c复合后的粉体于280MP-350MP下冷等静压140s-175s后成型；
e、烧结：将步骤d成型块体置入含有MnO2、Fe2O3、La2O3中一种或两种或三种的Al2O3粉体中，于温度1150-1300℃下烧结1-4h，得到镧离子掺杂的深低温热敏电阻材料。
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