CN112960979A - 一种锆酸盐体系高温负温度系数热敏电阻材料及制备方法 - Google Patents
一种锆酸盐体系高温负温度系数热敏电阻材料及制备方法 Download PDFInfo
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Abstract
本发明涉及一种锆酸盐体系高温负温度系数热敏电阻材料及制备方法,该热敏电阻材料是将二氧化锆分别与三氧化二钬或三氧化二镧按照化学计量比混合,经过湿法球磨、冷等静压成型、高温烧结,即可得到锆酸盐体系高温负温度系数热敏电阻材料,该材料电性能参数为B500℃/1500℃=11281‑16706K±1.65%,ρ1500℃=1.06‑2.63×103Ω·cm±1.4%,在温度区间500℃‑1500℃内具有明显的负温度系数特性,材料电性能稳定,一致性好,老化性能稳定,对氧分压不敏感,是适合制造用于高温测量以及不同氧气氛下温度监控的热敏电阻材料。
Description
技术领域
本发明涉及一种锆酸盐体系高温负温度系数热敏电阻材料,该热敏电阻材料在500℃-1500℃范围内具有明显的负温度系数特性和氧分压不敏感特性,属于半导体传感器领域。
背景技术
随着深海探索、军事和航空航天、汽车电子工业的蓬勃发展,对具有高精度并能承受恶劣环境的传感、监控和控制系统的敏感元器件需求不断增长,材料在极端环境下应用也越来越多。作为热敏元器件之一,NTC(negative temperature coefficient)热敏电阻有着随着温度的升高,电阻呈指数下降的特性。在制造温度传感器、温度补偿、稳压、超高频率检测设备,金属热电偶,抑制浪涌电流等方面,具有很大的发展潜力。然而传统的尖晶石型NTC适用温度范围为-60-300℃,在高温下相结构及其不稳定,温度300℃以上长期使用会出现显著老化现象,不能实现精准测量。钙钛矿结构的热敏电阻材料在温度800℃及以上高温环境下长期应用相结构会发生变化,电阻率漂移严重,高温相稳定性仍有待提高。因此,开发出更高应用温度的新型高温NTC材料成为热敏材料研究的热点。
开发高温NTC热敏电阻材料的关键的挑战是,此类材料必须具在高温、高压和严重氧化/腐蚀的恶劣环境下仍然保持稳定的物理、化学和热性能。然而传统的尖晶石型NTC适用温度范围为-60-300℃,在高温下相结构及其不稳定,温度300℃以上长期使用会出现显著老化现象,不能实现精准测量。钙钛矿结构的热敏电阻材料在温度800℃及以上高温环境下长期应用由于元素挥发,晶界副反应等导致相结构会发生变化,电阻率漂移严重,高温相稳定性仍有待提高。另外,已知大多数报道的材料的最高温度上限只有温度800℃,少数材料能达到1000℃。同时,当温度上升到温度上限时电阻仅有数十欧姆,限制了它们在高温环境中的实际应用,此外,这些材料还存在老化特性差以及电学性能易受富氧环境影响,提高热敏电阻材料在更高温度下的老化寿命以及氧气氛下的稳定性是迫切需要解决的问题。
发明内容
本发明的目的在于,提供一种锆酸盐体系高温负温度系数热敏电阻材料,该热敏电阻材料是将二氧化锆分别与三氧化二钬或三氧化二镧按照化学计量比混合,经过湿法球磨、冷等静压成型、高温烧结,即可得到锆酸盐体系高温负温度系数热敏电阻材料,该材料电性能参数为B500℃/1500℃=11281-16706K±1.65%,ρ1500℃=1.06-2.63×103Ω·cm±1.4%,在温度区间500℃-1500℃内具有明显的负温度系数特性,材料电性能稳定、一致性好、老化性能稳定、对氧分压不敏感,是适合制造用于高温测量以及不同氧气氛下温度监控的热敏电阻材料。
本发明所述的一种锆酸盐体系高温负温度系数热敏电阻材料,该热敏电阻材料的化学通式为:A2Zr2O7,其中A=La或Ho,由原料二氧化锆与三氧化二钬或三氧化二镧混合烧制而成,具体操作按下列步骤进行:
a、按A2Zr2O7的组成,称取二氧化锆分别与三氧化二钬或三氧化二镧进行混合,置于玛瑙球磨罐中,以分析纯无水乙醇为分散介质,湿磨12h,将湿磨后的浆料在温度150℃下烘干,取出研磨1-2h,得到粉体;
b、将步骤a中得到的粉体在温度1400℃下煅烧6-7小时,得到烧绿石结构A2Zr207(A=La、Ho)粉体;
c、将步骤a中得到的粉体以15-25kg/cm2的压力进行压块成型,时间为1-2min,将成型的块体进行冷等静压,在压强为250-300MPa保压3min,然后将块体在温度1600℃下烧结10h,即得热敏电阻材料;
d、将步骤c得到的热敏电阻材料正反两面涂覆铂浆电极,然后在温度900℃下退火1-2h,即得到电性能参数为:B500℃/1500℃=11281-16706K±1.65%,ρ1500℃=1.06-2.63×103Ω·cm±1.4%的锆酸盐体系高温负温度系数热敏电阻材料。
一种锆酸盐高温负温度系数热敏电阻材料的制备方法,按下列步骤进行:
a、按A2Zr2O7的组成,称取二氧化锆分别与三氧化二钬或三氧化二镧进行混合,置于玛瑙球磨罐中,以分析纯无水乙醇为分散介质,湿磨12h,将湿磨后的浆料在温度150℃下烘干,取出研磨1-2h,得到粉体;
b、将步骤a中得到的粉体在温度1400℃下煅烧6-7小时,得到烧绿石结构A2Zr207(A=La、Ho)粉体;
c、将步骤a中得到的粉体以15-25kg/cm2的压力进行压块成型,时间为1-2min,将成型的块体进行冷等静压,在压强为250-300MPa保压3min,然后将块体在温度1600℃下烧结10h,即得热敏电阻材料;
d、将步骤c得到的热敏电阻材料正反两面涂覆铂浆电极,然后在温度900℃下退火1-2h,即得到电性能参数为:B500℃/1500℃=11281-16706K±1.65%,ρ1500℃=1.06-2.63×103Ω·cm±1.4%的锆酸盐体系高温负温度系数热敏电阻材料。
本发明所述的锆酸盐体系高温负温度系数热敏电阻材料,该热敏电阻材料是将二氧化锆分别与三氧化二钬或三氧化二镧按照A2Zr207(A=La、Ho)化学计量比混合,经过湿法球磨、冷等静压成型、高温烧结,即可得到锆酸盐体系材料,该体系材料电性能参数为B500℃/1500℃=11281-16706K±1.65%,ρ1500℃=1.06-2.63×103Ω·cm±1.4%。可通过改变A位阳离子,从而得到一系列的A2Zr2O7型高温负温度系数热敏电阻材料。
本发明所述的锆酸盐体系高温负温度系数热敏电阻材料,该热敏电阻材料其创新点主要有:
(1)本发明所获得的锆酸盐体系A2Zr207(A=La、Ho)高温负温度系数热敏电阻材料在较高的温度范围500℃-1500℃内具有典型的NTC特性,在高温环境中性能稳定。
(2)该材料电阻率几乎与氧分压的变化无关,且在高温环境下也能保持较高的电阻率,依然达到千欧级别,有利于其在高温环境的实际应用。
该材料电性能稳定、一致性好、老化性能稳定、对氧分压不敏感,是适合制造用于高温测量以及不同氧气氛下温度监控的热敏电阻材料。
附图说明
图1为本发明A2Zr207(A=La、Ho)材料的电阻率与温度的关系图。
图2为本发明A2Zr207(A=La、Ho)材料的电阻率与氧分压的关系图。
具体实施方式
实施例1
a、按La2Zr2O7的组成,称取二氧化锆与三氧化二镧进行混合,置于玛瑙球磨罐中,以分析纯无水乙醇为分散介质,湿磨12h,将湿磨后的浆料在温度150℃下烘干,取出研磨1h,得到粉体;
b、将步骤a中得到的粉体在温度1400℃下煅烧6小时,得烧绿石结构La2Zr207粉体;
c、将步骤b中得到的粉体以15kg/cm2的压力进行压块成型,时间为1min,将成型的块体进行冷等静压,在压强为250MPa保压3min,然后将块体在温度1600℃下烧结10h,即得到La2Zr207高温负温度系数热敏电阻材料;
d、将步骤c得到的La2Zr207高温负温度系数热敏电阻材料正反两面涂覆铂浆电极,然后在温度900℃下退火2h,即得到电性能参数为:B500℃/1500℃=16982K,ρ1500℃=1.045×103Ω·cm的La2Zr207高温负温度系数热敏电阻材料。
实施例2
a、按La2Zr2O7的组成,称取二氧化锆与三氧化二镧进行混合,置于玛瑙球磨罐中,以分析纯无水乙醇为分散介质,湿磨12h,将湿磨后的浆料在温度150℃下烘干,取出研磨2h,得到粉体;
b、将步骤a中得到的粉体在温度1400℃下煅烧7小时,得烧绿石结构La2Zr207粉体;
c、将步骤b中得到的粉体以20kg/cm2的压力进行压块成型,时间为2min,将成型的块体进行冷等静压,在压强为300MPa保压3min,然后将块体在温度1600℃下烧结10h,即得到La2Zr207高温负温度系数热敏电阻材料;
d、将步骤c得到的La2Zr207高温负温度系数热敏电阻材料正反两面涂覆铂浆电极,然后在温度900℃下退火1h,即得到电性能参数为:B500℃/1500℃=16430K,ρ1500℃=1.075×103Ω·cm的La2Zr207高温负温度系数热敏电阻材料。
实施例3
a、按Ho2Zr2O7的组成,称取二氧化锆与三氧化二钬进行混合,置于玛瑙球磨罐中,以分析纯无水乙醇为分散介质,湿磨12h,将湿磨后的浆料在温度150℃下烘干,取出研磨1h,得到粉体;
b、将步骤a中得到的粉体在1400℃下煅烧7小时,得烧绿石结构的Ho2Zr2O7粉体;
c、将步骤b中得到的粉体以18kg/cm2的压力进行压块成型,时间为1min,将成型的块体进行冷等静压,在压强为280MPa保压3min,然后将块体在温度1600℃下烧结10h,即得到Ho2Zr2O7高温负温度系数热敏电阻材料;
d、将步骤c得到的Ho2Zr2O7高温负温度系数热敏电阻材料正反两面涂覆铂浆电极,然后在温度900℃下退火1h,即得到电性能参数为:B500℃/1500℃=11094K,ρ1500℃=2.67×103Ω·cm的Ho2Zr2O7高温负温度系数热敏电阻材料。
实施例4
a、按Ho2Zr2O7的组成,称取二氧化锆与三氧化二钬进行混合,置于玛瑙球磨罐中,以分析纯无水乙醇为分散介质,湿磨12h,将湿磨后的浆料在温度150℃下烘干,取出研磨2h,得到粉体;
b、将步骤a中得到的粉体在1400℃下煅烧6小时,得烧绿石结构的Ho2Zr2O7粉体;
c、将步骤b中得到的粉体以22kg/cm2的压力进行压块成型,时间为2min,将成型的块体进行冷等静压,在压强为300MPa保压3min,然后将块体在温度1600℃下烧结10h,即得到Ho2Zr2O7高温负温度系数热敏电阻材料;
d、将步骤c得到的Ho2Zr2O7高温负温度系数热敏电阻材料正反两面涂覆铂浆电极,然后在温度900℃下退火2h,即得到电性能参数为:B500℃/1500℃=11467K,ρ1500℃=2.59×103Ω·cm的Ho2Zr2O7高温负温度系数热敏电阻材料。
实施例5
将实施例1-4获得的任意一种锆酸盐系负温度系数热敏电阻材料,通过改变A位阳离子,从而得到锆酸盐型高温负温度系数热敏电阻材料。材料制备方法简单、体积小、电性能稳定、一致性好、老化性能稳定、对氧分压不敏感,是两种适合制造用于高温测量以及不同氧气氛下温度监控的热敏电阻材料。
Claims (2)
1.一种锆酸盐体系高温负温度系数热敏电阻材料,其特征在于,该热敏电阻材料的化学通式为:A2Zr2O7,其中A=La或Ho,由原料二氧化锆与三氧化二钬或三氧化二镧混合烧制而成,具体操作按下列步骤进行:
a、按A2Zr2O7的组成,称取二氧化锆分别与三氧化二钬或三氧化二镧进行混合,置于玛瑙球磨罐中,以分析纯无水乙醇为分散介质,湿磨12h,将湿磨后的浆料在温度150℃下烘干,取出研磨1-2h,得到粉体;
b、将步骤a中得到的粉体在温度1400℃下煅烧6-7小时,得到烧绿石结构A2Zr207(A=La、Ho)粉体;
c、将步骤a中得到的粉体以15-25kg/cm2的压力进行压块成型,时间为1-2min,将成型的块体进行冷等静压,在压强为250-300MPa保压3min,然后将块体在温度1600℃下烧结10h,即得热敏电阻材料;
d、将步骤c得到的热敏电阻材料正反两面涂覆铂浆电极,然后在温度900℃下退火1-2h,即得到电性能参数为:B500℃/1500℃=11281-16706K±1.65%,ρ1500℃=1.06-2.63×103Ω·cm±1.4%的锆酸盐体系高温负温度系数热敏电阻材料。
2.一种锆酸盐高温负温度系数热敏电阻材料的制备方法,其特征在于按下列步骤进行:
a、按A2Zr2O7的组成,称取二氧化锆分别与三氧化二钬或三氧化二镧进行混合,置于玛瑙球磨罐中,以分析纯无水乙醇为分散介质,湿磨12h,将湿磨后的浆料在温度150℃下烘干,取出研磨1-2h,得到粉体;
b、将步骤a中得到的粉体在温度1400℃下煅烧6-7小时,得到烧绿石结构A2Zr207(A=La、Ho)粉体;
c、将步骤a中得到的粉体以15-25kg/cm2的压力进行压块成型,时间为1-2min,将成型的块体进行冷等静压,在压强为250-300MPa保压3min,然后将块体在温度1600℃下烧结10h,即得热敏电阻材料;
d、将步骤c得到的热敏电阻材料正反两面涂覆铂浆电极,然后在温度900℃下退火1-2h,即得到电性能参数为:B500℃/1500℃=11281-16706K±1.65%,ρ1500℃=1.06-2.63×103Ω·cm±1.4%的锆酸盐体系高温负温度系数热敏电阻材料。
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