CN112759391A - 一种镱掺杂ntc型高温热敏电阻陶瓷材料及其制备方法和应用 - Google Patents
一种镱掺杂ntc型高温热敏电阻陶瓷材料及其制备方法和应用 Download PDFInfo
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- 229910010293 ceramic material Inorganic materials 0.000 title claims abstract description 66
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 70
- 238000004519 manufacturing process Methods 0.000 claims abstract description 8
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 27
- 239000011575 calcium Substances 0.000 claims description 23
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 18
- 229910052593 corundum Inorganic materials 0.000 claims description 18
- 239000010431 corundum Substances 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- ZNOKGRXACCSDPY-UHFFFAOYSA-N tungsten trioxide Chemical compound O=[W](=O)=O ZNOKGRXACCSDPY-UHFFFAOYSA-N 0.000 claims description 18
- 238000001816 cooling Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 14
- 229910052697 platinum Inorganic materials 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 10
- 238000005245 sintering Methods 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 9
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 9
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- 238000009694 cold isostatic pressing Methods 0.000 claims description 9
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 9
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 9
- UZLYXNNZYFBAQO-UHFFFAOYSA-N oxygen(2-);ytterbium(3+) Chemical compound [O-2].[O-2].[O-2].[Yb+3].[Yb+3] UZLYXNNZYFBAQO-UHFFFAOYSA-N 0.000 claims description 8
- 238000000137 annealing Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000000465 moulding Methods 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 2
- 239000013590 bulk material Substances 0.000 claims 1
- 238000011161 development Methods 0.000 description 7
- 229910052769 Ytterbium Inorganic materials 0.000 description 4
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 3
- 229910052684 Cerium Inorganic materials 0.000 description 3
- 229910052791 calcium Inorganic materials 0.000 description 3
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 239000010955 niobium Substances 0.000 description 3
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- 229910052721 tungsten Inorganic materials 0.000 description 3
- 239000010937 tungsten Substances 0.000 description 3
- 229910004829 CaWO4 Inorganic materials 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000035945 sensitivity Effects 0.000 description 2
- 229910018553 Ni—O Inorganic materials 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- -1 i.e. Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 239000011029 spinel Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- FIXNOXLJNSSSLJ-UHFFFAOYSA-N ytterbium(III) oxide Inorganic materials O=[Yb]O[Yb]=O FIXNOXLJNSSSLJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明涉及一种镱掺杂NTC型高温热敏电阻陶瓷材料及其制备方法和应用,该材料以碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱为原料,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NTC(负温度系数)型高温热敏电阻陶瓷材料,材料常数为B300℃/600℃=6465K—6732K,在温度25℃时,电阻率为4.06×107Ωcm—8.63×107Ωcm。采用本发明制备的热敏电阻材料性能稳定,一致性好,该热敏电阻材料在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
本发明属于热敏材料,具体涉及一种镱掺杂NTC型高温热敏电阻陶瓷材料及其制备方法和应用。
背景技术
随着当今科学技术的快速发展,NTC热敏电阻器已经在很多领域应用,与人们的生活息息相关,NTC热敏陶瓷材料是热敏电阻器的核心,工业的发展和市场的需求已经促进着NTC热敏材料的发展,尤其汽车领域的发展,促使NTC热敏电阻材料从低温应用领域向高温应用领域转变成为工业发展的需要。所以研发应用于高温领域的NTC热敏陶瓷材料具有重要的意义。
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,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。其测量温度最高可达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,在500℃以上的高温下,电阻-温度关系的线性化不稳定。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(NTC)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。
发明内容
发明目的:针对现有技术存在的问题,本发明提供镱掺杂NTC型高温热敏电阻陶瓷材料,采用本发明制备的热敏电阻陶瓷材料性能稳定,一致性好,该热敏电阻材料在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的新型热敏电阻材料。
本发明还提供了所述的镱掺杂NTC型高温热敏电阻陶瓷材料的制备方法和应用。
技术方案:为实现上述发明目的,本发明所述一种镱掺杂NTC型高温热敏电阻陶瓷材料,该热敏电阻陶瓷材料主要以碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱为原料制备而成。
其中,所述镱掺杂NTC型高温热敏电阻陶瓷材料的化学组成为Ca1-xYbxCeNbWO8,其中0<x≤0.2,x代表元素Yb的摩尔数,1-x代表元素Ca的摩尔数。所述镱掺杂NTC型高温热敏电阻陶瓷材料为白钨矿结构CaWO4。
作为优选,所述镱掺杂NTC型高温热敏电阻陶瓷材料中使用的钙、镱、铈、铌、钨的摩尔比为(0.8-1):(0.05-0.2):1:1:1。
更优选地,所述中x=0.2,所述镱掺杂NTC型高温热敏电阻陶瓷材料中使用的钙、镱、铈、铌、钨的摩尔比为0.8:0.2:1:1:1。
其中,所述热敏电阻陶瓷材料在温度25℃—800℃范围具有明显的负温度系数特性。
本发明所述的镱掺杂NTC型高温热敏电阻陶瓷材料的制备方法,包括如下步骤:
a、按Ca1-xYbxCeNbWO8的组成,分别称取碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱原料,将其置于玛瑙研钵中混合研磨,得到混合粉体;
b、将步骤a中得到的混合粉体,高温煅烧,再研磨,即得到Ca1-xYbxCeNbWO8粉体材料;
c、将步骤b得到的粉体材料用压片机,进行压块成型,得到块体材料;
d、将步骤c得到的块体材料进行冷等静压,高温烧结,冷却至室温,得到块体陶瓷材料;
e、将步骤d烧结的块体陶瓷材料正反两面涂覆铂浆电极,退火,冷却至室温,即得到NTC型热敏电阻陶瓷材料。
其中,步骤b中将步骤a中得到的混合粉体,置于刚玉干锅,在1000℃—1200℃温度下煅烧2—6小时,再研磨6—10小时,即得到Ca1-xYbxCeNbWO8粉体材料。
其中,步骤c中将步骤b得到的粉体材料用压片机,以5-10Kg/cm2的压力进行压块成型,保压时间为0.2-0.5分钟,得到块体材料。
其中,步骤d中将步骤c得到的块体材料进行冷等静压,在200—300MPa压强下保压1—3分钟,然后置于刚玉盖板上,在1200℃—1400℃温度下烧结2—6小时,冷却至室温,得到块体陶瓷材料。
作为优选,步骤d中的煅烧温度为1350℃,煅烧时长为4h。
其中,步骤e中将步骤d烧结的块体陶瓷材料正反两面涂覆铂浆电极,电极厚度约0.1mm,后置于刚玉盖板上,在800-900℃温度下退火30-60分钟,冷却至室温,即得到NTC型热敏电阻陶瓷材料。
本发明所述的热敏电阻陶瓷材料在制造高温热敏电阻器中的应用。
本发明提出一种全新的镱掺杂NTC型高温热敏电阻陶瓷材料,以碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱为原料,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NTC型高温热敏电阻陶瓷材料,材料常数为B300℃/600℃=6465K—6732K,在温度25℃时,电阻率为4.06×107Ωcm—8.63×107Ωcm。采用本发明制备的热敏电阻陶瓷材料性能稳定,一致性好,该热敏电阻材料在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。
本发明从Ca1-xYbxCeNbWO8的半导体特性出发,通过Yb2O3掺杂改性优化Ca1- xYbxCeNbWO8热敏陶瓷材料电学性能,其中0<x≤0.2,实现高温条件下(25℃—800℃)此热敏电阻陶瓷材料性能稳定,有望成为制造高温热敏电阻器的新材料。
有益效果:与现有技术相比,本发明具有如下优点:
本发明制备的镱掺杂NTC型高温热敏电阻陶瓷材料,采用固相法将钙、铈、铌、钨、镱的氧化物进行混合研磨、煅烧、再研磨即得热敏电阻前驱体粉体材料,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,该圆片形热敏电阻为白钨矿结构的Ca1-xYbxCeNbWO8的陶瓷材料,其材料常数为B300℃/600℃=6465K—6732K,在温度25℃时,电阻率为4.06×107Ωcm—8.63×107Ωcm。采用本发明所述方法制备的高温热敏电阻陶瓷材料性能稳定,一致性好,该热敏电阻陶瓷材料在温度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(白钨矿结构CaWO4);
图2为本发明的热敏陶瓷材料的阻温特性曲线。
具体实施方式
下面对本发明技术方案进行详细说明,但是本发明的保护范围不局限于所述实施例。
实施例1
a、按Ca0.95Yb0.05CeNbWO8的组成,分别称取碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱原料,将其置于玛瑙研钵中混合研磨6小时,得到混合粉体;
b、将步骤a中得到的混合粉体,置于刚玉干锅,在1200℃温度下煅烧2小时,再研磨6小时,即得到Ca0.95Yb0.05CeNbWO8粉体材料;
c、将步骤b得到的粉体材料用压片机,以10Kg/cm2的压力进行压块成型,保压时间为0.2分钟,得到块体材料;
d、将步骤c得到的块体材料进行冷等静压,在200MPa压强下保压3分钟,然后置于刚玉盖板上,在1400℃温度下烧结2小时,冷却至室温,得到块体陶瓷材料;
e、将步骤d烧结的块体陶瓷材料正反两面涂覆铂浆电极,电极厚度约0.1mm,然后置于刚玉盖板上,在900℃温度下退火30分钟,冷却至室温,即得到NTC型热敏电阻陶瓷材料。其材料常数为B300℃/600℃=6465K,在温度25℃时,电阻率为4.06×107Ωcm。
实施例2
a、按Ca0.9Yb0.1CeNbWO8的组成,分别称取碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱原料,将其置于玛瑙研钵中混合研磨8小时,得到混合粉体;
b、将步骤a中得到的混合粉体,置于刚玉干锅,在1100℃温度下煅烧4小时,再研磨4小时,即得到Ca0.9Yb0.1CeNbWO8粉体材料;
c、将步骤b得到的粉体材料用压片机,以5Kg/cm2的压力进行压块成型,保压时间为0.5分钟,得到块体材料;
d、将步骤c得到的块体材料进行冷等静压,在250MPa压强下保压2分钟,然后置于刚玉盖板上,在1300℃温度下烧结4小时,冷却至室温,得到块体陶瓷材料;
e、将步骤d烧结的块体陶瓷材料正反两面涂覆铂浆电极,电极厚度约0.1mm,然后置于刚玉盖板上,在900℃温度下退火30分钟,冷却至室温,即得到NTC型热敏电阻陶瓷材料。其材料常数为B300℃/600℃=6470K,在温度25℃时,电阻率为4.39×107Ωcm。
实施例3
a、按Ca0.85Yb0.15CeNbWO8的组成,分别称取碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱原料,将其置于玛瑙研钵中混合研磨6小时,得到混合粉体;
b、将步骤a中得到的混合粉体,置于刚玉干锅,在1000℃温度下煅烧6小时,再研磨10小时,即得到Ca0.85Yb0.15CeNbWO8粉体材料;
c、将步骤b得到的粉体材料用压片机,以8Kg/cm2的压力进行压块成型,保压时间为0.3分钟,得到块体材料;
d、将步骤c得到的块体材料进行冷等静压,在200MPa压强下保压3分钟,然后置于刚玉盖板上,在1200℃温度下烧结6小时,冷却至室温,得到块体陶瓷材料;
e、将步骤d烧结的块体陶瓷材料正反两面涂覆铂浆电极,电极厚度约0.1mm,然后置于刚玉盖板上,在900℃温度下退火30分钟,冷却至室温,即得到NTC型热敏电阻陶瓷材料。其材料常数为B300℃/600℃=6580K,在温度25℃时,电阻率为6.33×107Ωcm。
实施例4
a、按Ca0.8Yb0.2CeNbWO8的组成,分别称取碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱原料,将其置于玛瑙研钵中混合研磨8小时,得到混合粉体;
b、将步骤a中得到的混合粉体,置于刚玉干锅,在1100℃温度下煅烧3小时,再研磨8小时,即得到Ca0.8Yb0.2CeNbWO8粉体材料;
c、将步骤b得到的粉体材料用压片机,以10Kg/cm2的压力进行压块成型,保压时间为0.5分钟,得到块体材料;
d、将步骤c得到的块体材料进行冷等静压,在300MPa压强下保压3分钟,然后置于刚玉盖板上,在1350℃温度下烧结4小时,冷却至室温,得到块体陶瓷材料;
e、将步骤d烧结的块体陶瓷材料正反两面涂覆铂浆电极,电极厚度约0.1mm,然后置于刚玉盖板上,在900℃温度下退火30分钟,冷却至室温,即得到NTC型热敏电阻陶瓷材料。其材料常数为B300℃/600℃=6732K,在温度25℃时,电阻率为8.63×107Ωcm。
对比例1
对比例1与实施例4的制备方法相同,不同之处在于:x=0,制得产品其材料常数为B300℃/600℃=6707K,在温度25℃时,电阻率为4.28×107Ωcm。
本发明实施例制备的NTC型热敏电阻陶瓷材料的X射线衍射图谱,如图1所示,本发明制备的材料为固溶体,XRD中无其他杂峰,为白钨矿结构CaWO4。
采用实施例1-4制备得到NTC型热敏电阻陶瓷材料其电阻率随温度变化如图2所示,可以说明本发明制备的材料在温度25℃—800℃范围具有明显的负温度系数特性,一致性好,性能稳定。
Claims (9)
1.一种镱掺杂NTC型高温热敏电阻陶瓷材料,其特征在于,该热敏电阻陶瓷材料主要以碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱为原料制备而成。
2.根据权利要求1所述的镱掺杂NTC型高温热敏电阻陶瓷材料,其特征在于,所述镱掺杂NTC型高温热敏电阻陶瓷材料的化学组成为Ca1-xYbxCeNbWO8,其中0<x≤0.2,为白钨矿结构。
3.根据权利要求1所述的镱掺杂NTC型高温热敏电阻陶瓷材料,其特征在于,所述热敏电阻陶瓷材料在温度25℃—800℃范围具有明显的负温度系数特性。
4.一种权利要求1所述的镱掺杂NTC型高温热敏电阻陶瓷材料的制备方法,其特征在于,包括如下步骤:
a、按Ca1-xYbxCeNbWO8的组成,分别称取碳酸钙,二氧化铈,五氧化二铌,三氧化钨,三氧化二镱原料,将其置于玛瑙研钵中混合研磨,得到混合粉体;
b、将步骤a中得到的混合粉体,高温煅烧,再研磨,即得到Ca1-xYbxCeNbWO8粉体材料;
c、将步骤b得到的粉体材料用压片机,进行压块成型,得到块体材料;
d、将步骤c得到的块体材料进行冷等静压,,高温烧结,冷却至室温,得到块体陶瓷材料;
e、将步骤d烧结的块体陶瓷材料正反两面涂覆铂浆电极,退火,冷却至室温,即得到NTC型热敏电阻陶瓷材料。
5.根据权利要求4所述的镱掺杂NTC型高温热敏电阻陶瓷材料的制备方法,其特征在于,步骤b中优选将步骤a中得到的混合粉体,置于刚玉干锅,在1000℃—1200℃温度下煅烧2—6小时,再研磨6—10小时,即得到Ca1-xYbxCeNbWO8粉体材料。
6.根据权利要求4所述的镱掺杂NTC型高温热敏电阻陶瓷材料的制备方法,其特征在于,步骤c中将步骤b得到的粉体材料用压片机,以5-10Kg/cm2的压力进行压块成型,保压时间为0.2-0.5分钟,得到块体材料。
7.根据权利要求4所述的镱掺杂NTC型高温热敏电阻陶瓷材料的制备方法,其特征在于,步骤d中将步骤c得到的块体材料进行冷等静压,在200—300MPa压强下保压1—3分钟,然后置于刚玉盖板上,在1200℃—1400℃温度下烧结2—6小时,冷却至室温,得到块体陶瓷材料。
8.根据权利要求4所述的镱掺杂NTC型高温热敏电阻陶瓷材料的制备方法,其特征在于,步骤e中将步骤d烧结的块体陶瓷材料正反两面涂覆铂浆电极,然后置于刚玉盖板上,在800-900℃温度下退火30-60分钟,冷却至室温,即得到NTC型热敏电阻陶瓷材料。
9.一种权利要求1所述的热敏电阻陶瓷材料在制造高温热敏电阻器中的应用。
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