CN110357609A - 一种钕铌为半导化的ntc热敏电阻材料及其制备方法 - Google Patents

一种钕铌为半导化的ntc热敏电阻材料及其制备方法 Download PDF

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CN110357609A
CN110357609A CN201910518376.4A CN201910518376A CN110357609A CN 110357609 A CN110357609 A CN 110357609A CN 201910518376 A CN201910518376 A CN 201910518376A CN 110357609 A CN110357609 A CN 110357609A
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王明东
戴文金
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Shandong Greentec Electric Technology Co Ltd
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Abstract

本发明公开了一种钕铌为半导化的NTC热敏电阻材料及其制备方法，属于电子信息功能材料与器件技术领域。本发明以锰镍铁钴的氧化物为主要成分组成、钕铌为半导化掺杂元素，采用固相反应法制备，通过球磨、烘干、预烧、二次球磨、烘干、粉碎过筛等工序来制备。本发明的热敏电阻材料具有稳定性好，具有电阻值、材料常数、电阻温度系数等电气特性可控的特点，适用于温度测量、温度控制和线路补偿，以及电路和电子元件的保护以及流量、流速、射线测量的仪器与应用领域。

Description

一种钕铌为半导化的NTC热敏电阻材料及其制备方法
技术领域
本发明属于电子信息功能材料与器件技术领域，具体涉及的是一种具有高成瓷致密性，具有尖晶石结构，电阻率、B值稳定的NTC热敏电阻材料及其制备方法。
背景技术
NTC(Negative Temperature Coefficient)是指随温度上升电阻呈指数关系减小、具有负温度系数的热敏电阻现象和材料。该材料是利用锰、铜、硅、钴、铁、镍、锌等两种或两种以上的金属氧化物进行充分混合、成型、烧结等工艺而成的半导体陶瓷，可制成具有负温度系数(NTC)的热敏电阻。其电阻率和材料常数随材料成分比例、烧结气氛、烧结温度和结构状态不同而变化。现在还出现了以碳化硅、硒化锡、氮化钽等为代表的非氧化物系NTC热敏电阻材料。
NTC热敏电阻器的发展经历了漫长的阶段。1834年，科学家首次发现了硫化银有负温度系数的特性。1930年，科学家发现氧化亚铜-氧化铜也具有负温度系数的性能，并将之成功地运用在航空仪器的温度补偿电路中。随后，由于晶体管技术的不断发展，热敏电阻器的研究取得重大进展。1960年研制出了NTC热敏电阻器。NTC热敏电阻器广泛用于测温、控温、温度补偿等方面。
功率型NTC热敏电阻多用于电源抑制浪涌。抑制浪涌用NTC热敏电阻器，是一种大功率的圆片式热敏电阻器，常用于有电容器、加热器和马达启动的电子电路中。
在电路电源接通瞬间，电路中会产生比正常工作时高出许多倍的浪涌电流，而NTC热敏电阻器的初始阻值较大，可以抑制电路中过大的电流，从而保护其电源电路及负载。当电路进入正常工作状态时，热敏电阻器由于通过电流而引起阻体温度上升，电阻值下降至很小，不会影响电路的正常工作。
目前的热敏电阻材料在稳定性，电阻值、材料常数、电阻温度系数等电气特性方面还存在许多不可控的因素，因此，申请人提出了一种钕铌为半导化的NTC热敏电阻材料及其制备方法。
发明内容
本发明的目的是提供一种性好可实现稳定批量生产的钕铌为半导化的NTC热敏电阻材料及其制备方法。
本发明解决所述技术问题采用的技术方案如下：
一种钕铌为半导化的NTC热敏电阻材料由主晶相材料和掺杂相材料经球磨混合、预烧、掺杂球磨、压滤烘干制成。其中：所述主晶相材料为Mn3O4质量百分比为40～60％，NiO质量百分比为15～25％，Fe2O3质量百分比为10～20％，Co2O3质量百分比为5～15％；所述掺杂相材料Nd2O3，质量百分比为0.1～2％，Nb2O5质量百分比为0.1～2％。
所述主晶相材料中Mn、Ni、Fe、Co之间的摩尔比为1-x-y-z：x：y：z，x为0.2～0.4，y为0.1～0.3，z为0.1～0.3。
所述掺杂相材料为稀土氧化物，Nd2O3质量百分比为0.1～2％，Nb2O5质量百分比为0.1～2％。
一种钕铌为半导化的NTC热敏电阻材料的制备方法，包括如下步骤：主晶相材料制备，按摩尔比称量Mn3O4、NiO、Fe2O3、Co2O3，按照料：球：水的比例1：2：0.8进行球磨，压滤烘干后，在900/6H条件下预烧；预烧后的主晶相材料，粉碎后按1：0.1～2％的比例添加掺杂相材料Nd2O3及Nb2O5，按步骤一的条件进行二次球磨，压滤烘干，然后粉碎过筛。
本发明以钕铌为半导化的NTC热敏电阻材料的成分组成为：Mn1-x-y-zNixFeyCoz，其中x为0.2～0.4，y为0.1～0.3，z为0.1～0.3。
本发明组成NTC材料的关键组成为Mn1-x-y-zNixFeyCoz，配方成分中含有锰、镍、铁、钴和钕、铌元素，制备这种热敏电阻的原材料Mn、Ni、Fe、Co、Nd、Nb是含这些元素的氧化物。其中，半导化元素钕、铌是为了调整热敏电阻元件的室温电阻率，元素铁、钴是用于调节热敏电阻元件的室温电阻率和体现热敏特性的材料常数与温度系数，同时钴的引入也可以增强热敏电阻的烧结性。
本发明的主要重点在于热敏电阻材料的成分配方，实际应用过程中可以根据需要对合成方法和生产工艺进行相应调整，灵活性大。合成方法可采用固相反应法、溶胶-凝胶法、共沉淀法、气相沉积法或其它陶瓷材料的合成方法来实现。本发明选用适于工业大生产的固相反应法，利于生产成本降低。
本发明的热敏电阻材料特性的检测是采用涂覆银浆，高温烧渗为电极，测量元件的室温电阻及电阻-温度特性。
本发明涉及的NTC热敏电阻材料的特色和优势表现在：①材料成分简单，原材料比较丰富，环境友好；②制备过程中烧结温度较低，适合陶瓷元件、薄膜、片式等NTC热敏电阻元件的生产；③材料以稀土元素钕、铌作为半导化掺杂元素；④通过调整半导化掺杂元素钕、铌的含量可大范围调整热敏电阻元件的室温电阻值；⑤通过调节成分组成中铁、钴的含量，可以较大范围地调节热敏元件的材料常数与温度系数。
本发明NTC热敏电阻材料的电性能可实现以下参数要求：室温电阻率ρ25＝18±4%Ω·mm-1，B值＝3380±1%。
本发明的内容结合以下实施例作进一步的说明。以下实施例只是符合本发明技术内容的几个实例，并不说明本发明仅限于下述实例所述的内容。本发明的重点在于成分配方，所述原材料、工艺方法和步骤可以根据实际生产条件进行相应的调整，灵活性大。
具体实施方式
本发明采用分析纯度的MnCO3、NiO、Fe2O3、Co2O3为原料制备主晶相，以纯度为4N的Nd2O3、Nb2O5进行掺杂，具体实施方式如下：
按表1称量配料，将混合料放入搅拌式球磨罐中，按料球水质量比1:2:0.8，球磨2～6小时，转速为260转/分钟。粒度控制在D50=1.2μm以内，将球磨混好的料压滤，放于100℃烘箱烘干，粉碎后过40 目筛，在箱式电阻炉中按900℃/6H条件预烧，粉碎后过40目筛备用；按表1中的比例添加掺杂相材料Nd2O3、Nb2O5进行二次球磨、压滤、烘干，粉碎后过80目筛，加PVA(聚乙烯醇) 造粒，用手动压机20MPa 成型Φ12.2mm×2mm圆片。将生坯样置于烧结炉中，1250℃/4H条件下，烧结成热敏陶瓷样品，涂银后在850℃/10M条件下烧渗，通过恒温油槽、精密电阻仪、千分尺等对样品进行性能测试。
本发明具体实施例成瓷密度、电阻率、B值结果详细见表2。
表1各实例中原料的百分比。
表2 各实例的样品性能。

Claims (6)

1.一种钕铌为半导化的NTC热敏电阻材料及其制备方法，其特征在于由主晶相材料和掺杂相材料经球磨混合、预烧、掺杂球磨、压滤烘干制成；其中所述主晶相材料为Mn3O4质量百分比为40～60％，NiO质量百分比为15～25％，Fe2O3质量百分比为10～20％，Co2O3质量百分比为5～15％；所述掺杂相材料Nd2O3，质量百分比为0.1～2％，Nb2O5质量百分比为0.1～2％。
2.根据权利要求1 所述的一种钕铌为半导化的NTC热敏电阻材料及其制备方法，其特征在于所述主晶相材料中Mn、Ni、Fe、Co之间的摩尔比为1-x-y-z：x：y：z，x为0.2～0.4，y为0.1～0.3，z为0.1～0.3。
3.根据权利要求1 所述的一种钕铌为半导化的NTC热敏电阻材料及其制备方法，其特征在于，所述掺杂相材料为稀土氧化物，Nd2O3质量百分比为0.1～2％，Nb2O5质量百分比为0.1～2％。
4.根据权利要求1 所述的一种钕铌为半导化的NTC热敏电阻材料及其制备方法，其特征在于所述电阻材料的制备方法包括如下步骤：主晶相材料制备，按摩尔比称量Mn3O4、NiO、Fe2O3、Co2O3，按料：球：水的比例1：2：0.8进行球磨，压滤烘干后，在900/6H条件下预烧；预烧后的主晶相材料，粉碎后按1：0.1～2％的比例添加掺杂相材料Nd2O3及Nb2O5，按步骤一的条件进行二次球磨，压滤烘干，然后粉碎过筛。
5.根据权利要求1 所述的一种钕铌为半导化的NTC热敏电阻材料及其制备方法，其特征在于本发明电阻材料的成分组成为：Mn1-x-y-zNixFeyCoz，其中x为0.2～0.4，y为0.1～0.3，z为0.1～0.3。
6.根据权利要求1 所述的一种钕铌为半导化的NTC热敏电阻材料及其制备方法，其特征在于本发明电阻材料的关键组成为Mn1-x-y-zNixFeyCoz，配方成分中含有锰、镍、铁、钴和钕、铌元素，制备这种热敏电阻的原材料Mn、Ni、Fe、Co、Nd、Nb是含这些元素的氧化物；其中，半导化元素钕、铌是为了调整热敏电阻元件的室温电阻率，元素铁、钴是用于调节热敏电阻元件的室温电阻率和体现热敏特性的材料常数与温度系数，同时钴的引入也可以增强热敏电阻的烧结性。
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