CN107324799B - 一种类钙钛矿型高温热敏电阻材料及其制备方法 - Google Patents
一种类钙钛矿型高温热敏电阻材料及其制备方法 Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 56
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 229910010293 ceramic material Inorganic materials 0.000 claims abstract description 20
- 239000010936 titanium Substances 0.000 claims abstract description 19
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000011572 manganese Substances 0.000 claims abstract description 18
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 18
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 16
- 239000011575 calcium Substances 0.000 claims abstract description 14
- 238000000227 grinding Methods 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000005751 Copper oxide Substances 0.000 claims abstract description 9
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 9
- 239000004408 titanium dioxide Substances 0.000 claims abstract description 9
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 8
- 239000011248 coating agent Substances 0.000 claims abstract description 8
- 238000000576 coating method Methods 0.000 claims abstract description 8
- 238000009694 cold isostatic pressing Methods 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 22
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 21
- 229910052697 platinum Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 8
- 239000002002 slurry Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000000137 annealing Methods 0.000 claims description 5
- 239000004570 mortar (masonry) Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
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- RUDFQVOCFDJEEF-UHFFFAOYSA-N oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims 1
- 238000005245 sintering Methods 0.000 abstract description 5
- 239000010408 film Substances 0.000 description 3
- 229910004247 CaCu Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000000523 sample Substances 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 235000012431 wafers Nutrition 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
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- 229910018553 Ni—O Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
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- 238000001514 detection method Methods 0.000 description 1
- -1 i.e. Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
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- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种类钙钛矿型高温热敏电阻材料及其制备方法，该材料以分析纯碳酸钙，氧化铜，二氧化锰，二氧化钛，三氧化二钇原料，经混合研磨、煅烧、冷等静压成型、高温烧结、涂烧电极，即可得到类钙钛矿结构的Ca1‑ xYxCu2.5Mn0.5Ti4O12(0≤x≤0.1)热敏陶瓷材料，材料常数为B300℃/500℃＝6800K‑7700K，温度25℃电阻率为1.09×107Ωcm‑3.60×107Ωcm。采用本发明制备的热敏电阻材料在25℃‑800℃范围具有明显的负温度系数特性，材料体系电性能稳定，一致性好，适合制造高温热敏电阻器。
Description
技术领域
本发明涉及一种类钙钛矿型高温热敏电阻材料及其制备方法，该热敏电阻材料在温度25℃-800℃范围具有明显的负温度系数特性，是一种适用于制造高温热敏电阻器的新型热敏电阻材料。
背景技术
目前，国内外用于高温检测的主要为铂电阻。铂电阻温度探测器用于测量温度低于600℃的情况已有很长的历史，目前的发展主要集中在薄型和厚型铂膜上，即在陶瓷物质上带一层薄膜的膜型电阻温度探测器。经最新改进后，它的测量温度最高可达850℃。铂膜电阻温度传感器依靠电阻－温度的线性化特性实现温度测量，在低于500℃时，可充分呈线性化，但由于铂金属材料自身的特性，高温下的线性化很难实现。另外，欲提高灵敏度须采用制造技术手段增加元件尺寸，这使传感器的响应时间随尺寸增加而增大，造成了性能改进的矛盾。
负温度系数热敏电阻器具有灵敏度高、响应快的特点，然而，传统的Mn-Co-Ni-O系尖晶石型热敏电阻材料主要用于300℃以下，这就给新型高温热敏电阻材料的开发提出了新的挑战性课题。
本发明对氧化物固相法制备的CaCu2.5Mn0.5Ti4O12热敏电阻材料电学性能进行了初步研究，其材料常数为6400K，有望用于制造高温热敏电阻器。考虑到Y2O3的耐高温性能，且Y3+与Ca2+具有相近的离子半径，Y3+取代Ca2+可调节CaCu2.5Mn0.5Ti4O12热敏电阻材料电学性能，制造不同电性能参数的高温热敏电阻器。
本发明从CaCu2.5Mn0.5Ti4O12的半导体特性出发，通过Y2O3掺杂设计合成了类钙钛矿型Ca1-xYxCu2.5Mn0.5Ti4O12(0≤x≤0.1)高温25℃-800℃的热敏电阻材料。
发明内容
本发明的目的在于，提供一种类钙钛矿型高温热敏电阻材料及其制备方法，该材料以碳酸钙，氧化铜，二氧化锰，二氧化钛，三氧化二钇为原料，经混合研磨、煅烧、冷等静压成型、高温烧结、涂烧电极，即可得到类钙钛矿型高温热敏电阻材料，材料常数为B300℃/500℃＝6800K—7700K，温度25℃电阻率为1.09×107Ωcm-3.60×107Ωcm。采用本发明制备的热敏电阻材料在25℃-800℃范围具有明显的负温度系数特性，材料体系电性能稳定，一致性好，适合制造高温热敏电阻器。
本发明所述的一种类钙钛矿型高温热敏电阻材料，该热敏电阻材料以碳酸钙，氧化铜，二氧化锰，二氧化钛，三氧化二钇为原料，结构为体心立方的类钙钛矿结构，其化学组成为Ca1-xYxCu2.5Mn0.5Ti4O12，其中0≤x≤0.1。
所述的一种类钙钛矿型高温热敏电阻材料的制备方法，按下列步骤进行：
a、按Ca1-xYxCu2.5Mn0.5Ti4O12分别称取碳酸钙，氧化铜，二氧化锰，二氧化钛，三氧化二钇进行混合，将混合的原料置于玛瑙研钵中研磨5-10小时，得到粉体；
b、将步骤a中研磨好的粉体在温度800℃-1000℃煅烧4-8小时，研磨5-10小时后即得Ca1-xYxCu2.5Mn0.5Ti4O12粉体；
c、将步骤b得到的粉体材料以10-20Kg/cm2的压力进行压块成型，时间为0.5-2分钟，将成型的块体材料进行冷等静压，在压强为300—400MPa下保压1-3分钟，然后于温度1000℃-1200℃烧结4-8小时，制得高温热敏陶瓷材料；
d、将步骤c烧结的陶瓷材料正反两面涂覆铂浆电极，然后于温度900℃下退火30分钟，即得到温度范围为25℃-800℃，材料常数为B300℃/500℃＝6800K-7700K，温度25℃电阻率为1.09×107Ωcm-3.60×107Ωcm的高温热敏电阻材料。
本发明所述的一种类钙钛矿型高温热敏电阻材料及其制备方法，采用固相法将钙、铜、锰、钛、钇的氧化物进行混和研磨、煅烧、混合、再研磨即得负温度系数热敏电阻粉体材料，再将该粉体材料片式冷等静压成型，高温烧结后正反两面涂烧铂浆电极获得热敏电阻圆片，该圆片热敏电阻为类钙钛结构的Ca1-xYxCu2.5Mn0.5Ti4O12的陶瓷材料，其材料常数为B300℃/500℃＝6800K-7700K，温度25℃电阻率为1.09×107Ωcm-3.60×107Ωcm。采用本发明所述方法制备的类钙钛矿型高温热敏电阻材料性能稳定，一致性好，该热敏电阻材料在温度25℃-800℃范围具有明显的负温度系数特性，适合制造高温热敏电阻器。
附图说明
图1为本发明的热敏陶瓷材料的X射线衍射图谱。
具体实施方式
实施例1
a、首先按CaCu2.5Mn0.5Ti4O12分别称取分析纯碳酸钙，氧化铜，二氧化锰，二氧化钛进行混合，将混合的原料置于玛瑙研钵中研磨5小时，得到粉体；
b、将步骤a中研磨好的粉体在温度800℃煅烧4小时，研磨5小时后即得CaCu2.5Mn0.5Ti4O12粉体；
c、将步骤b得到的粉体材料以20Kg/cm2的压力进行压块成型，时间为1分钟，将成型的块体材料进行冷等静压，在压强为300MPa下保压2分钟，然后于温度1000℃烧结8小时，制得高温热敏陶瓷材料；
d、将步骤c烧结的陶瓷材料正反两面涂覆铂浆电极，然后于900℃下退火30分钟，即可得到温度范围为25℃-800℃，材料常数为B300℃/500℃＝7110K，温度25℃电阻率为1.09×107Ωcm的高温热敏电阻材料。
实施例2
a、按Ca0.95Y0.05Cu2.5Mn0.5Ti4O12分别称取碳酸钙，氧化铜，二氧化锰，二氧化钛，三氧化二钇进行混合，将混合的原料置于玛瑙研钵中研磨10小时，得到粉体；
b、将步骤a中研磨好的粉体在温度900℃煅烧6小时，研磨8小时后即得Ca0.95Y0.05Cu2.5Mn0.5Ti4O12粉体；
c、将步骤b得到的粉体材料以15Kg/cm2的压力进行压块成型，时间为0.5分钟，将成型的块体材料进行冷等静压，在压强为400MPa下保压1分钟，然后于温度1100℃烧结6小时，制得高温热敏陶瓷材料；
d、将步骤c烧结的陶瓷材料正反两面涂覆铂浆电极，然后于温度900℃下退火30分钟，即可得到温度范围为25℃-800℃，材料常数为B300℃/500℃＝6800K，温度25℃电阻率为2.01×107Ωcm的高温热敏电阻材料。
实施例3
a、按Ca0.9Y0.1Cu2.5Mn0.5Ti4O12分别称取碳酸钙，氧化铜，二氧化锰，二氧化钛，三氧化二钇进行混合，将混合的原料置于玛瑙研钵中研磨8小时，得到粉体；
b、将步骤a中研磨好的粉体在温度1000℃煅烧8小时，研磨10小时后即得Ca0.9Y0.1Cu2.5Mn0.5Ti4O12粉体；
c、将步骤b得到的粉体材料以10Kg/cm2的压力进行压块成型，时间为2分钟，将成型的块体材料进行冷等静压，在压强为350MPa下保压3分钟，然后于温度1200℃烧结4小时，制得高温热敏陶瓷材料；
d、将步骤c烧结的陶瓷材料正反两面涂覆铂浆电极，然后于温度900℃下退火30分钟，即可得到温度范围为25℃-800℃，材料常数为B300℃/500℃＝7700K，温度25℃电阻率为3.60×107Ωcm的高温热敏电阻材料。
Claims (1)
1.一种类钙钛矿型高温热敏电阻材料的制备方法，其特征在于该热敏电阻材料以碳酸钙，氧化铜，二氧化锰，二氧化钛，三氧化二钇为原料，其化学组成为Ca1-x Y x Cu2.5Mn0.5Ti4O12，结构为体心立方的类钙钛矿结构，其中0＜x≤0.1，具体操作按下列步骤进行：
a、按Ca1-x Y x Cu2.5Mn0.5Ti4O12分别称取碳酸钙，氧化铜，二氧化锰，二氧化钛，三氧化二钇进行混合，将混合的原料置于玛瑙研钵中研磨5-10小时，得到粉体；
b、将步骤a中研磨好的粉体在温度800℃-1000℃煅烧4-8小时，研磨5-10小时后即得Ca1-x Y x Cu2.5Mn0.5Ti4O12粉体；
c、将步骤b得到的粉体材料以10-20Kg/cm2的压力进行压块成型，时间为0.5-2分钟，将成型的块体材料进行冷等静压，在压强为300-400MPa下保压1-3分钟，然后于温度1000℃-1200℃烧结4-8小时，制得高温热敏陶瓷材料；
d、将步骤c烧结的陶瓷材料正反两面涂覆铂浆电极，然后于温度900℃下退火30分钟，即得到温度范围为25℃-800℃，材料常数为B 300℃/500℃=6800K-7700K，温度25℃电阻率为1.09×107Ωcm-3.60×107Ωcm的高温热敏电阻材料。
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| CN111620689A (zh) * | 2020-06-08 | 2020-09-04 | 中国科学院新疆理化技术研究所 | 一种不同a位元素的类钙钛矿型高温热敏电阻材料及其制备方法 |
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| CN112830770B (zh) * | 2021-01-19 | 2023-03-21 | 中国科学院新疆理化技术研究所 | 一种高温复合热敏电阻材料及其制备方法 |
| CN113004039B (zh) * | 2021-04-26 | 2023-03-21 | 中国科学院新疆理化技术研究所 | 一种钨青铜型高温热敏电阻材料及其制备方法 |
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