Mn-Co-Ni-O系热敏薄膜的磁控溅射方法制备及其光电性能研究

发布时间：2018-01-05 13:01

本文关键词：Mn-Co-Ni-O系热敏薄膜的磁控溅射方法制备及其光电性能研究　出处：《新疆大学》2015年硕士论文　论文类型：学位论文

【摘要】：以Mn,Co,Ni为主的尖晶石过渡族金属氧化物(AB2O4)是一种具有负温度系数的热敏材料,它具有较高的温度电阻(TCR),耐老化性能好,工作温度范围和光谱的反应范围广,能够长期稳定工作等优点,被广泛应用于温度测量计,辐射热测量计和非致冷型红外探测仪等精确测量仪器上。在Mn-Co-Ni-O系材料的制备方面,主要有物理方法和化学方法两种方法,其中高温固相法等物理方法已经具备了较为成熟的工艺体系。本文以高温固相合成法作为基础,以射频磁控溅射为主要手段,对Mn-Co-Ni-O系薄膜的制备工艺进行了摸索,并对所制备的Mn-Co-Ni-O系薄膜的物相结构,电学,光学性能以及它们之间的联系进行了研究。本文的研究工作主要从以下几个方面展开:(1)磁控溅射制备Mn-Co-Ni-O系薄膜使用磁控溅射方法在Si O2/Si衬底上生长Mn-Co-Ni-O系薄膜,通过对一系列工艺参数的摸索和比较,找出最佳的生长条件,并希望改变生长条件,对所制备的薄膜厚度进行控制。希望能对Mn-Co-Ni-O系陶瓷材料的微型化提供参考。(2)Mn-Co-Ni-O系薄膜的物相和形貌表征采用磁控溅射方法制备了一系列不同厚度的Mn-Co-Ni-O系薄膜,通过EDS,XRD,XPS等手段对不同厚度薄膜进行物相的定量和定性分析,发现不同厚度薄膜的Mn,Co,Ni元素比例没有太大区别,但样品中Mn3+和Mn4+的比例却发生了规律性的变化。采用FESEM,AFM对不同厚度薄膜进行形貌表征。(3)Mn-Co-Ni-O系薄膜的电学性能分析对厚度组Mn-Co-Ni-O系薄膜电学性能进行了研究。根据以往的研究表明,在薄膜材料中,随着薄厚的增加,薄膜材料的室温电阻(R0)和特征温度(T0,有些研究中称为B值)都会减小。但是按照这个趋势,块体材料的特征温度(T0)应该小于薄膜材料。实际上同种工艺参数制备块体材料的特征温度(B值)却相差不大,通过对一系列200nm-900nm左右薄膜研究,发现存在着这样一个线性关系:201/()cTμd-d或20ln()()cTμd-d,其中d为薄膜的厚度,dc为薄膜材料特征温度转折点(或B值转折点)的膜厚。并且,当材料由二维材料变为三维的块体材料时依然适用。为了验证该曲线拟合的正确性,这里结合以往其他研究者的一些数据,发现大致符合这一规律。并结合霍尔效应测试对薄膜材料的载流子浓度,半导体类型分析,同时结合小极化子跃迁模型对这一现象进行解释。(4)Mn-Co-Ni-O系薄膜的光学性能分析采用红外椭圆偏振光谱仪器对不同厚度的Mn-Co-Ni-O系薄膜进行测量,得到一系列不同厚度样品的红外椭偏谱。通过仪器拟合得到近红外和可见光区域范围内薄膜光学系数的变化,并对不同厚度薄膜进行对比分析。
[Abstract]:Spinel transition metal oxide (AB _ 2O _ 4) is a kind of thermal sensitive material with negative temperature coefficient. It has high temperature resistance and good aging resistance. Because of its wide range of reaction temperature and spectrum and the ability to work stably for a long time, it has been widely used in temperature measurement. In the accurate measuring instruments such as radiation calorimeter and uncooled infrared detector, there are two main methods in the preparation of Mn-Co-Ni-O system materials: physical method and chemical method. The physical methods such as high temperature solid phase method have already had a more mature process system. This paper takes the high temperature solid state synthesis method as the foundation and the radio frequency magnetron sputtering as the main means. The preparation process of Mn-Co-Ni-O system thin films was explored, and the phase structure and electricity of the prepared Mn-Co-Ni-O system films were also studied. The optical properties and the relationship between them are studied in this paper. Mn-Co-Ni-O films were prepared by magnetron sputtering. Mn-Co-Ni-O films were grown on Sio _ 2 / Si substrates by magnetron sputtering. Through the exploration and comparison of a series of technological parameters, the best growth conditions are found, and the growth conditions are desired to be changed. The thickness of the prepared films is controlled. It is hoped that it can provide a reference for the miniaturization of Mn-Co-Ni-O system ceramics. Phase and morphology characterization of Mn-Co-Ni-O films A series of Mn-Co-Ni-O films with different thickness were prepared by magnetron sputtering. The quantitative and qualitative analysis of the phases of thin films with different thickness by means of EDS- XRDX XPS shows that there is no significant difference in the proportion of Ni elements in mn _ (Co) O _ (2) O _ (2) films with different thickness. However, the proportion of Mn3 and Mn4 in the sample changed regularly. FESEM was used. Morphology characterization of thin films with different thickness by AFM. The electrical properties of Mn-Co-Ni-O films were analyzed. The electrical properties of Mn-Co-Ni-O films with thickness group were studied. In thin film materials, the room temperature resistance (R0) and the characteristic temperature (T _ 0) of the thin film materials decrease with the increase of the thickness, which is called "B value" in some studies, but according to this trend. The characteristic temperature of bulk material (T0) should be smaller than that of thin film material. In fact, the characteristic temperature (B value) of the same process parameters for the preparation of bulk material is not much different. A series of thin films about 200nm-900nm have been studied. It is found that there is a linear relationship between the 10 ~ (-1) C ~ (-1) C ~ (d-d) or the ~ (20) lnn ~ (2 +) C ~ (-T) 渭 d ~ (d-d). Where d is the thickness of the film and DC is the thickness of the film at the temperature turning point (or B value turning point) of the film material. In order to verify the correctness of the curve fitting, some data from other researchers are used in this paper. It is found that this rule is approximately in accord with this rule. The carrier concentration and semiconductor type of the thin film materials are analyzed with Hall effect test. At the same time, the phenomenon is explained by the small polaron transition model. The optical properties of Mn-Co-Ni-O thin films were analyzed. The Mn-Co-Ni-O films with different thickness were measured by infrared elliptical polarization spectrometer. Infrared ellipsometry spectra of a series of samples with different thickness were obtained. The optical coefficients of thin films in the range of near infrared and visible light were obtained by means of instrument fitting, and the films of different thickness were compared and analyzed.
【学位授予单位】：新疆大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.2

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