CN114426431B - 一种有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法 - Google Patents

一种有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法 Download PDF

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CN114426431B
CN114426431B CN202210171239.XA CN202210171239A CN114426431B CN 114426431 B CN114426431 B CN 114426431B CN 202210171239 A CN202210171239 A CN 202210171239A CN 114426431 B CN114426431 B CN 114426431B
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张惠敏
秦晴
常爱民
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Xinjiang Technical Institute of Physics and Chemistry of CAS
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Abstract

本发明涉及一种有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法，该材料是采用三氧化二钇，三氧化二钐，碳酸钡，四氧化三钴经混合球磨、预烧、研磨、等静压成型、高温烧结，即得到有序缺氧型钙钛矿层状Y‑Sm‑Ba‑Co‑O材料体系，并进行了电阻测试，结果表明：其电阻率ρ60K=3×105‑8×105Ω·cm，其材料常数B40/180=688‑826K。该材料体系可用于40‑180K的深低温温区。

Description

一种有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法
技术领域
本发明涉及一种用于深低温的有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法。
背景技术
负温度系数(NTC)热敏电阻是利用材料的电阻率随温度变化的敏感程度所具有的特性而制成的器件，其电阻随着温度的升高而降低，NTC热敏电阻也广泛的应用于电路和电子元件的保护以及流速，射线测量仪器与应用领域。深低温用NTC热敏电阻也常常被用于深空探测方面，在红外遥感器方面，可以通过低温制冷对电子的能级跃迁产生抑制，可以失实现高灵敏度的探测；在大型科学仪器、量子通讯方、超导电子学、低温半导体电子学等等领域广泛应用。
近年来，为了制得低温高性能NTC热敏电阻，科技工作者也开发一些新的材料，如有序缺氧型钙钛矿Ln-Ba-Co-O,该结构由平行于(010)的单层角共CoO6八面体组成，它们主要通过沿a→的角共CoO5金字塔的双带进行相互连接，Co原子位于八面体位置和位于金字塔位置的氧原子以及阴离子空位排列有序。
以尖晶石结构为主的NTC热敏陶瓷材料，相对来说室温电阻率会偏大并且电阻值不容易调控，因为这些过渡金属氧化物的挥发温度比较低，所以在制备和烧结的过程中比较容易产生原材料的成分的挥发，重复性较低。除此之外，降低尖晶石结构的电阻率，导致温度系数降低。从尖晶石的结构角度分析，尖晶石结构的八面体和四面体的阳离子都会随时间的变化从而缓慢变化，重新排布也会引起结构弛豫现象的产生，致使热敏陶瓷的不稳定性，从而导致材料的老化，影响材料的性能和使用寿命。
常用的NTC热敏电阻中，热敏电阻主要是利用锰，钴，镍，镁和铜等两种或者两种以上的过渡金属的氧化物所组成，通过制备和烧结等工艺从而制成半导体陶瓷电阻，如在中国发明专利CN006667B公布的Co-Fe-O陶瓷系列体系，这些热敏陶瓷体系的组成都是至少含有两种或者两种以上的过渡金属的氧化物，并且以尖晶石的立方结构为主相。
发明内容
本发明的目的是，提供一种有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法，该材料是采用三氧化二钇，三氧化二钐，碳酸钡，四氧化三钴经混合球磨、预烧、研磨、等静压成型、高温烧结，即得到层状Y-Sm-Ba-Co-O材料体系，并进行了电阻测试，结果表明：其电阻率ρ60K＝3×105-8×105Ω·cm，其材料常数B40/180＝688-826K。该材料体系可用于40-180K的深低温温区。
本发明所述的一种有序缺氧型钙钛矿层状结构热敏陶瓷材料，该材料的组成为Y-Sm-Ba-Co-O，采用高温固相法制成，具体操作按下列步骤进行：
a、按重量百分比将Y2O3:Sm2O3:BaCO3:Co3O4＝5％-20％:5％-20％:15％-25％:60％-50％进行准确称量，采用球磨法研磨12-24h，于温度700-1100℃下预烧1-6h，得到粉体；
b、将步骤a预烧后的粉体研磨6-12h，并在300-350Mpa等静压1-5min，得到坯体；
c、将步骤b获得的坯体在温度1100-1300℃烧结1-6h，即得到有序缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
一种有序缺氧型钙钛矿层状结构热敏陶瓷材料的制备方法，按下列步骤进行：
a、按重量百分比Y2O3:Sm2O3:BaCO3:Co3O4＝5％-20％:5％-20％:15％-25％:60％-50％进行准确称量，采用球磨法研磨12-24h，于温度700-1100℃下预烧1-6h，得到粉体；
b、将步骤a预烧后的粉体研磨6-12h，并在300-350Mpa等静压1-5min，得到坯体；
c、将步骤b获得的坯体在温度1100-1300℃烧结1-6h，即得到有序缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
本发明所述的一种有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法，所涉及的NTC热敏材料组成为Y-Sm-Ba-Co-O，是由于Y3+和Ba2+阳离子呈一定比列排列，沿c排列成交替层，氧空位位于Y3+层的水平面，形成六边隧道，这种结构非常灵活，因此它可以接受可变数量的氧气，它导致了长程和短程超结构的形成。
本发明所述的一种有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法，是由[CoO2]-[BaO]-[CoO2]-[YOδ]层状结构组成，其中的Co离子Co3+在低温(T<150K)时，会出现铁磁磁耦合现象，Co3+离子也会驱动铁磁的有序性产生，在40K下反铁磁基质中，超顺铁磁的形成和钴离子的种类有关，Co3+在低温下处于低自旋状态(LS)，O-2P轨道和Co-3d轨道之间存在较强的极化费米能级，费米能级附近电荷的转移隙较窄，温度降低也会导致近LS中的部分Co离子发生持续的跃迁，以Y-Ba-Co-O为基底，因为Co本身的满足深低温热敏电阻的一些性能可以调节材料的室温电阻率和温度常数，并且不同半径的离子的引入也会影响材料的烧结性。
本发明所述的一种有序缺氧型钙钛矿层状结构热敏陶瓷材料及制备方法，其优点和特色主要表现在：是一种很有特色的缺氧型双层状类钙钛矿结构，结构层之间可以接受可变数量的氧气，灵活度很高，可以调控氧气对周围离子的影响，容易实现低温目标。缺氧型钙钛矿层状材料，材料常数和低温下的电阻率可以通过改变掺杂离子而获得。
附图说明
图1为Y-Sm-Ba-Co-O材料的SEM图。
具体实施方式
实施例1
a、将Y2O3、Sm2O3、BaCO3和Co3O4按重量百分比Y2O3 5％，Sm2O3 20％，BaCO3 25％，Co3O4 50％,进行准确称量，采用球磨法研磨12h于温度1100℃下预烧1h，得到粉体；
b、将步骤a预烧后的粉体研磨12h，并在300Mpa等静压5min，得到坯体；
c、将步骤b获得的坯体在温度1100℃烧结6h，即得到缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
将烧结缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料进行涂覆电极进行电阻测试，其电阻率ρ60K＝8×105Ω·cm，材料常数B40/180＝826K。
实施例2
a、将Y2O3、Sm2O3、BaCO3和Co3O4按重量百分比Y2O3 8％，Sm2O3 17％，BaCO3 17％，Co3O4 58％,进行准确称量，采用球磨法研磨14.4h，于温度1020℃下预烧2h，得到粉体；
b、将步骤a预烧后的粉体研磨10.8h，并在310Mpa等静压4.2min，得到坯体；
c、将步骤b获得的坯体在温度1140℃烧结5h，即得到缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
将烧结缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料进行涂覆电极并进行电阻测试，其电阻率ρ60K＝6×105Ω·cm，其材料常数B40/180＝823K。
实施例3
a、将Y2O3、Sm2O3、BaCO3和Co3O4按重量百分比Y2O3 11％，Sm2O3 14％，BaCO3 19％，Co3O4 56％，进行准确称量，采用球磨法研磨16.8h，于温度940℃下预烧3h，得到粉体；
b、将步骤a预烧后的粉体研磨9.6h，并在320Mpa等静压3.4min，得到坯体；
c、将步骤b获得的坯体在温度1180℃烧结4h，即得到缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
将烧结缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料进行涂覆电极，并进行电阻测试，其电阻率ρ60K＝4.7×105Ω·cm，其材料常数B40/180＝790K。
实施例4
a、将Y2O3、Sm2O3、BaCO3和Co3O4按重量百分比Y2O3 14％，Sm2O3 11％，BaCO3 21％，Co3O4 54％,进行准确称量，采用球磨法研磨19.2h，于温度860℃下预烧4h，得到粉体；
b、将步骤a预烧后的粉体研磨8.4h，并在330Mpa等静压2.6min，得到坯体；
c、将步骤b获得的坯体在温度1220℃烧结3h，即得到缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
将烧结缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料进行涂覆电极进行电阻测试，其电阻率ρ60K＝3.4×105Ω·cm，其材料常数B40/180＝760K。
实施例5
a、将Y2O3、Sm2O3、BaCO3和Co3O4按重量百分比Y2O3 17％，Sm2O3 8％，BaCO3 23％，Co3O4 52％,进行准确称量，采用球磨法研磨21.6h，于温度780℃下预烧5h，得到粉体；
b、将步骤a预烧后的粉体研磨7.2h，并在340Mpa等静压1.8min，得到坯体；
c、将步骤b获得的坯体在温度1260℃烧结2h，即得到缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
将烧结缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料进行涂覆电极进行电阻测试，其电阻率ρ60K＝3.2×105Ω·cm，材料常数B40/180＝724K。
实施例6
a、将Y2O3、Sm2O3、BaCO3和Co3O4按重量百分比Y2O3 20％，Sm2O3 5％，BaCO3 15％，Co3O4 60％,进行准确称量，采用球磨法研磨小24h，于温度700℃下预烧6h，得到粉体；
b、将步骤a预烧后的粉体研磨6h，并在350Mpa等静压1min，得到坯体；
c、将步骤b获得的坯体在温度1300℃烧结1h，即得到缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
将烧结缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料进行涂覆电极，并进行电阻测试，其电阻率ρ60K＝3×105Ω·cm，材料常数B40/180＝688K。

Claims (2)

1.一种有序缺氧型钙钛矿层状结构热敏陶瓷材料，其特征在于该材料的组成为Y-Sm-Ba-Co-O，采用高温固相法制成，具体操作按下列步骤进行：
a、按重量百分比将Y2O3:Sm2O3: BaCO3:Co3O4 =5%-20%:5%-20%:15%-25%:60%-50%进行准确称量，采用球磨法研磨12-24h，于温度700-1100℃下预烧1-6h，得到粉体；
b、将步骤a预烧后的粉体研磨6-12h，并在300-350Mpa等静压1-5min，得到坯体；
c、将步骤b获得的坯体在温度1100-1300℃烧结1-6h，即得到有序缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
2.一种有序缺氧型钙钛矿层状结构热敏陶瓷材料的制备方法，其特征在于按下列步骤进行：
a、按重量百分比Y2O3:Sm2O3: BaCO3:Co3O4 =5%-20%:5%-20%:15%-25%:60%-50%进行准确称量，采用球磨法研磨12-24h，于温度700-1100℃下预烧1-6h，得到粉体；
b、将步骤a预烧后的粉体研磨6-12h，并在300-350Mpa等静压1-5min，得到坯体；
c、将步骤b获得的坯体在温度1100-1300℃烧结1-6h，即得到有序缺氧型钙钛矿Y-Sm-Ba-Co-O层状结构热敏陶瓷材料。
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