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Mn-Co-Ni-O系NTC薄膜热敏电阻材料的制备工艺及性能研究
陈雪颖
学位类型硕士
导师徐金宝
2013-05-27
学位授予单位中国科学院大学
学位授予地点北京
学位专业微电子学与固体电子学
关键词薄膜 Ntc热敏电阻 电学性能 导电机理
其他摘要

负温度系数(Negative Temperature Coefficient, NTC)热敏电阻材料是电阻率随着温度的升高呈指数规律降低的热敏材料,作为温度传感器的感温元器件,可广泛应用于温度检测与控制、温度补偿和抑制浪涌电流等领域。具有AB2O4尖晶石型结构的Mn-Co-Ni-O材料体系是NTC热敏电阻材料的主要研究体系之一,所制备的NTC热敏电阻器具有热稳定性能良好、灵敏度高、精度高、响应速度快等优势。当前,作为NTC热敏电阻材料的研究热点之一,膜状NTC热敏电阻材料在航天、工业、电子、家用电器等领域均有广阔的市场前景,因此是一个很有价值的研究方向。

本文以Mn-Co-Ni-O系尖晶石结构NTC薄膜热敏电阻材料作为主要研究对象,详细讨论了采用不同工艺制备NTC薄膜热敏电阻的方法,并对不同工艺制备的NTC薄膜热敏电阻的性能参数、微观结构等展开了研究与探讨。本文主要研究内容分为以下四点:

(1)采用溶胶-凝胶制备工艺,以乙酸盐为原材料,乙酸溶液为溶剂,化学体系为Mn-Co-Ni-O,在Si衬底上制备单一组分薄膜NTC热敏电阻材料,退火温度分别为650℃,700℃,750℃,800℃。详细论述不同退火热处理温度对MCN薄膜NTC热敏电阻材料电学性能、微观形貌、物相结构的影响。结果表明,退火温度为650℃时,薄膜已形成尖晶石结构,退火温度为750℃时,材料的电学性能、相纯度、薄膜表面致密度等性能均优于其他退火条件下的热敏电阻。

(2)采用溶胶-凝胶法制备薄膜热敏材料,高温退火处理过程对热敏材料进行结晶化使形成尖晶石结构,制备工艺单一,因此我们采用醇热方法晶化具有尖晶石结构的NTC薄膜热敏电阻。结果表明:在醇热法合成温度150℃、反应时间12h的条件下,可以实现薄膜热敏材料的结晶化。使用醇热法合成NTC薄膜热敏电阻的方法具有可行性,操作简单,成本低廉,但薄膜成膜质量较差,与衬底的粘附力降低,实验成功率低,因此需要进一步改进实验工艺条件以制备出性能优异的热敏电阻。

(3)在大量薄膜NTC热敏电阻材料的实验数据基础上,以多种组分交替沉积制备纳米复合薄膜材料为研究内容,采用溶胶-凝胶法制备多层膜热敏电阻,对薄膜的物相结构、微观形貌、导电机理等进行了研究。

(4)最后开展的实验工作是采用溶胶-凝胶法制备Mn1.5Co1.5-xNixO4(x=0, 0.25, 0.5, 1.5)NTC热敏电阻,详细讨论了前驱体粉体的物相结构、红外吸收光谱,以及热敏电阻材料的导电机理和电学性能。采用溶胶-凝胶法制备Mn1.5Co1.5-xNixO4(x=0, 0.25, 0.5, 1.5)NTC热敏电阻,烧结温度750℃,成瓷烧结温度1050℃,材料的各项参数可通过阻温关系等得出。

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The resistivity of negative temperature coefficient (NTC) thermistor material decreases exponentially with temperature. The NTC thermistor can be widely used for detection and control temperature devices, temperature compensation devices and surge current protection devices. There are some advantages about the Mn-Co-Ni-O NTC thermistor, such as thermal stability, high sensitivity, high accuracy, fast response. Current, as one of the focus of the NTC thermistor material, the thin film NTC thermistor material is an important functional material and widely used in the field of aerospace, electron industry, household appliances. In this paper, Mn-Co-Ni-O NTC film thermistor material with spinel structure is the main research object, it was prepared by different preparation process on Si substrates, such as sol-gel method. Our work is to prepare NTC thin film materials and make them crystallize at different annealing temperature. The main contents of our work are four points: (1)At first, the starting material were manganese acetate, nickel acetate and cobalt acetate, acetic acid solution was used as solvent, Mn-Co-Ni-O(MCN) thin films NTC thermistor with single-component structure were prepared on Si substrates by sol-gel preparation process, the annealing temperature was 650℃, 700℃, 750℃ and 800℃, respectively. The effects of different annealing temperature of the MCN thin films thermistor on the electrical properties, microstructure morphology and phase component were studied and discussed in this paper. The results showed that, when the annealing temperature is 650°C, spinel structure of the thin films was already formed. When the annealing temperature is 750°C, for the electrical properties, the phase purity, the surface density and other properties, the MCN thin film had superior properties than the other thermistor. (2)In the early experimental work, the NTC thin film material was prepared by sol-gel method; it was a single preparation process. In this article, alcohol thermal reaction was used for synthesis of Mn-Co-Ni-O thin film NTC thermistor. The results showed that: when the synthesis temperature is 150°C, then the reaction time is 12h, the Mn-Co-Ni-O thin film would be crystallized by alcohol-thermal reaction. Therefore, this was a feasible method that low temperature synthesis of manganese cobalt nickel thin film by alcohol-thermal reaction. However, obviously, there were some disadvantages such as the poor quality of the thin film and the adhesion reduced with the substrate. Therefore, we need to further improve the experimental process conditions to achieve the thin film thermistor with well performance. (3)The thin film NTC thermistors were deposited by single chemical component; there were a large number of experimental data and on the thin-film NTC thermistor material. We were alternating deposited by variety of chemical components Mn-Co-Ni-O nanoparticle composite films on Si substrate. The effects of the thin film on the phase composition, microscopic morphology were investigated. (4)The last, Mn1.5Co1.5-xNixO4(x=0,0.25,0.5,1.5) NTC thermistors were prepared by sol-gel method. The phase composition and the infrared absorption spectrum of the precursor powder were investigated. We systematically studied the effects of technological parameters of NTC thermistor material on their conductive mechanism and electrical properties. The results showed that Mn1.5Co1.5-xNixO4 NTC thermistor was prepared by the sol-gel process, sintering temperature at 750°C, sintering porcelain temperature of 1050°C, with good electrical performance and high sensitivity, controllable chemical composition.
文献类型学位论文
条目标识符http://ir.xjipc.cas.cn/handle/365002/2519
专题材料物理与化学研究室
作者单位中国科学院新疆理化技术研究所
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陈雪颖. Mn-Co-Ni-O系NTC薄膜热敏电阻材料的制备工艺及性能研究[D]. 北京. 中国科学院大学,2013.
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