CN107140965A - 一种高电阻率、低b值负温度系数热敏材料及其制备方法 - Google Patents

一种高电阻率、低b值负温度系数热敏材料及其制备方法 Download PDF

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CN107140965A
CN107140965A CN201710274618.0A CN201710274618A CN107140965A CN 107140965 A CN107140965 A CN 107140965A CN 201710274618 A CN201710274618 A CN 201710274618A CN 107140965 A CN107140965 A CN 107140965A
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CN107140965B (zh
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李本文
任倜
姜广国
张洪峰
肖立峰
贾伟志
刘倩
朱金鸿
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SHANDONG ZHONGXIA ELECTRONICS TECHNOLOGY Co Ltd
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Abstract

本发明涉及热敏材料及传感器领域，特别公开了一种高电阻率、低B值负温度系数热敏材料及其制备方法。该高电阻率、低B值负温度系数热敏材料，其特征在于：以Ni‑Cu‑Fe系氧化物作为主配方，在主配方中掺入Cr2O3、CaO、ZrO、SiC制成；其中，主配方由重量比为15‑30:45‑60:10‑35的NiO、CuO和Fe2O3组成，Cr2O3、CaO、ZrO、SiC的添加总量为主配方重量的1‑9%。本发明工艺简单、产品可实现批量生产，具有致密性好、稳定性高、导电性能优良等特点，是各种传感器所需的重量材料。

Description

一种高电阻率、低B值负温度系数热敏材料及其制备方法
（一）技术领域
本发明涉及热敏材料及传感器领域，特别涉及一种高电阻率、低B值负温度系数热敏材料及其制备方法。
（二）背景技术
高电阻率、低B值负温度系数热敏材料制备的元件与传感器用于汽车电子、各种半导体器件和传感器的温度补偿以及宽温区测温要求高电阻值/低B值的元件，但由于当前国内外相关高电阻率、低B值产品，相对MEMS数字传感器来说精度偏低，因此能够制造更高精度的高电阻率/低B值的低成本材料成为全球同行业追求的目标。
负温度系数热敏的基本特性决定热敏材料，通常使用的热敏材料是由过度金属Mn、Fe、Co、Ni、Cu的氧化物按不同比例配制而成的，同时掺入一些高价或低价的其他金属化氧化物。目前市场上高电阻率、低B值材料的电阻率500-2000Ωcm，B值（材料系数）在800-1800K范围内；而电阻率10-100KΩcm，B值（材料系数）在1000-2200K范围内，还未见报道，成为当今负温度系数热敏电阻制造的一大难题。
（三）发明内容
本发明为了弥补现有技术的不足，提供了一种工艺简单、产品性能好的高电阻率、低B值负温度系数热敏材料及其制备方法。
本发明是通过如下技术方案实现的：
一种高电阻率、低B值负温度系数热敏材料，其特征在于：以Ni-Cu-Fe系氧化物作为主配方，在主配方中掺入Cr2O3、CaO、ZrO、SiC制成；其中，主配方由重量比为15-30:45-60:10-35的NiO、CuO和Fe2O3组成，Cr2O3、CaO、ZrO、SiC的添加总量为主配方重量的1-9%
其中，所述Cr2O3、CaO、ZrO、SiC的重量配比为10-25:10-20:20-35:20-40。
本发明所述的高电阻率、低B值负温度系数热敏材料的制备方法，其特征在于：在主配方中掺入Cr2O3、CaO、ZrO、SiC后进行18-24h的球磨，然后经100-150℃烘干后加入粘合剂，制成200-300目的颗粒，再制成成形圆片，在900-1200℃高温下烧结2-6h，最后印刷得到成品。
其优选的技术方案为：
所述球磨时，球磨物料、水和球的重量配比为1:1.0-1.3:1.4-1.8。
所述粘合剂为质量浓度为10-20%的聚乙烯醇溶液，其用量为主配方重量的20-30%。
所述成形圆片的直径为5cm，成形密度为2.4-3.6g/cm3。
所述烧结过程为以0.5℃/min的速率由室温升温至500℃，然后恒温2h；再以0.8℃/min的速率由500℃升温至800℃，恒温2h后，以6℃/min的速率升温至烧结温度，烧结2-6h，然后随炉降温。
所述印刷时，在750-850℃的银浆还原温度下还原浆料，还原时间为25-35min。
本发明中配方和烧结为关键工艺，配方决定了材料特性，烧结则是实现这一特性的保证，得到的材料电阻率为10-100KΩcm，B值（材料系数）为1000-2200K。
本发明工艺简单、产品可实现批量生产，具有致密性好、稳定性高、导电性能优良等特点，是各种传感器所需的重量材料。
（四）具体实施方式
实施例1：
（1）配方：以NiO、CuO、Fe2O3为原料，纯度为工业级，取NiO：CuO：Fe2O3=28：55：17（wt%）+5%（添加剂）=25：55：20（wt%）+5%（添加剂）=22：55：23（wt%）+5% （添加剂）=18：55：27（wt%）+5%（添加剂）；添加剂为：Cr2O3：CaO：ZrO：SiC=20:15:30:35wt%,24小时球磨；
（2）将上述比例配方料球磨24小时，料：水：球=1.0:1.2:1.5；
（3）造粒：在粉料中加入浓度为15%的PVA胶溶液24%wt，手工造粒,过200-300目筛；
（4）成形：成形Ф5.4（mm）×1.2（mm）的坯片，压制密度为3.2g/cm3；
（5）将成形的坯片装入陶瓷钵中在1080℃高温下烧结 3小时。烧结曲线为：
室温～500℃ 升温速率为0.5℃/min，
500℃～500℃ 恒温2小时，
500℃～800℃ 升温速率为0.8℃/min，
800℃～800℃ 恒温2小时，
800℃～1080 升温速率为6℃/min，
1080 恒温3小时，
然后随炉降温，200℃以下，出炉。
（6）利用丝网印刷电极；820℃温度下还原30min。
（7）本发明的一种高电阻率、低B值负温度系数热敏材料制成元件测试其电阻率、B值结果如下表(以100支芯片统计)：
结果表明，随着NiO量的减少，电阻率下降，B值随之下降，一种高电阻率、低B值负温度系数热敏材料电阻率、B值与Ni-Cu-Fe系材料相关。
实施例2：
主配方取NiO：CuO：Fe2O3=23：52：25（wt%），添加剂的量分别取为1.0、3.0、5.0、7.0、9.0wt%，按实施例1的工艺制作成样品，其测试结果如下表（以100支芯片统计）：
结果表明，随着添加剂量的增加，电阻率和B值变化很小，一致性以添加剂4%为中心最好，随添加剂增加或减少其一致性变大。
实施例3：
配方取NiO、CuO、Fe2O3=23：52：25（wt%），添加剂的量为5wt%，按实施例1的工艺做成坯片，取不同的烧结温度烧结，样品的测量结果如下表(以100支芯片统计)：
结果表明，随着烧结温度的增加, 电阻率下降，B值随之下降。
本发明的材料配方和制备技术可以批量生产，材料的性能满足温度传感器所需的各种参数，这种材料具有致密性好、稳定性高、导电性能优良等特点，是传感器所需的重要材料。

Claims (8)

1.一种高电阻率、低B值负温度系数热敏材料，其特征在于：以Ni-Cu-Fe系氧化物作为主配方，在主配方中掺入Cr2O3、CaO、ZrO、SiC制成；其中，主配方由重量比为15-30:45-60:10-35的NiO、CuO和Fe2O3组成，Cr2O3、CaO、ZrO、SiC的添加总量为主配方重量的1-9%。
2.根据权利要求1所述的高电阻率、低B值负温度系数热敏材料，其特征在于：所述Cr2O3、CaO、ZrO、SiC的重量配比为10-25:10-20:20-35:20-40。
3.根据权利要求1所述的高电阻率、低B值负温度系数热敏材料的制备方法，其特征在于：在主配方中掺入Cr2O3、CaO、ZrO、SiC后进行18-24h的球磨，然后经100-150℃烘干后加入粘合剂，制成200-300目的颗粒，再制成成形圆片，在900-1200℃高温下烧结2-6h，最后印刷得到成品。
4.根据权利要求3所述的高电阻率、低B值负温度系数热敏材料的制备方法，其特征在于：所述球磨时，球磨物料、水和球的重量配比为1:1.0-1.3:1.4-1.8。
5.根据权利要求3所述的高电阻率、低B值负温度系数热敏材料的制备方法，其特征在于：所述粘合剂为质量浓度为10-20%的聚乙烯醇溶液，其用量为主配方重量的20-30%。
6.根据权利要求3所述的高电阻率、低B值负温度系数热敏材料的制备方法，其特征在于：所述成形圆片的直径为5cm，成形密度为2.4-3.6g/cm3。
7.根据权利要求3所述的高电阻率、低B值负温度系数热敏材料的制备方法，其特征在于：所述烧结过程为以0.5℃/min的速率由室温升温至500℃，然后恒温2h；再以0.8℃/min的速率由500℃升温至800℃，恒温2h后，以6℃/min的速率升温至烧结温度，烧结2-6h，然后随炉降温。
8.根据权利要求3所述的高电阻率、低B值负温度系数热敏材料的制备方法，其特征在于：所述印刷时，在750-850℃的银浆还原温度下还原酱料，还原时间为25-35min。
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