|Place of Conferral||北京|
|Keyword||化学溶液沉积法 薄膜 负温度系数热敏电阻 稳定性 复合结构|
尖晶石结构的Mn-Co-Ni-O基材料具备丰富的物理性质，是一类市场占有率较高的负温度系数(NTC)热敏电阻材料。在实际应用中，超薄超轻、快响应的元件成为需求之一，因此研究人员对 Mn-Co-Ni-O基薄膜材料在制备方法及结构、光学和电学性质等方面进行了系统的研究。但Mn-Co-Ni-O基薄膜材料在高温范围的性质和应用的研究，还需要进一步的探索。本文以尖晶石结构的Mn1.56Co0.96Ni0.48O4为基础材料，制备出Mn-Co-Ni-(Al、Mg)-O系列薄膜以及与钙钛矿结构SrMnO3复合的薄膜的前驱体化学溶液，然后将前驱体溶液沉积在硅衬底上形成薄膜，并将所得薄膜于750 ℃空气气氛的管式炉中退火1 h。通过对不同体系薄膜进行相结构、表面微观形貌、光学与电学性质的表征，详细分析了离子掺杂、结构优化对其光学和电学性能的影响。主要研究结果如下：1、采用化学溶液沉积法制备Mn-Co-Al/Mg-Ni-O四元薄膜。Mn-Co-Al-Ni-O系薄膜中，Al含量的增加使样品的平均粒径减小；薄膜经过150 ℃恒温老化处理300 h后表面的孔洞数目减少，且Al含量越多影响越大。表面颗粒致密均匀的Mn1.56(Co0.9Al0.1)0.96Ni0.48O4薄膜样品在老化处理前后表面阳离子分布几乎不变，且室温电阻漂移率最小，即表现得最稳定。在可见光范围(380-780 nm)内，Mn-Co-Al-Ni-O系薄膜经过老化处理后折射率和光吸收强度都有所增大。Mn-Co-Mg-Ni-O系薄膜在300-850 nm的光谱范围内的折射率随波长的增大呈增大趋势，在700-800 nm间出现较强的光吸收。其中，Mn1.56(Co0.8Mg0.2)0.96Ni0.48O4薄膜表面最光滑，粒子大小均匀；而Mn1.56(Co0.6Mg0.4)0.96Ni0.48O4薄膜将材料的热敏常数B25/50值提升至4577 K。2、采用化学溶液沉积法制备Mn-Co-Al-Mg-Ni-O五元系薄膜，通过对比四元系薄膜的微观形貌图，五元系薄膜表面颗粒细小均匀且排列较紧密。其中，Mn1.56(Co0.5Al0.1Mg0.4)0.96Ni0.48O4薄膜具有最高B25/50值5794 K。3、采用化学溶液沉积法制备[Mn1.56Co0.96Ni0.48O4]1-x[SrMnO3]x (x=0、0.1、0.3、0.5)系列的尖晶石-钙钛矿复合结构薄膜。随着钙钛矿相含量的增加，薄膜表面的链条-沟壑结构逐渐被填充，变为小孔洞均匀分布，椭圆偏振光谱显示薄膜的光吸收增强。 [Mn1.56Co0.96Ni0.48O4]0.5[SrMnO3]0.5在复合结构薄膜样品中具有最大的热敏常数B25/50值5390 K。
The Mn-Co-Ni-O materials of spinel structure have rich physical properties, which are the negative temperature coefficient (NTC) thermistor material with high market share. The devices with ultra-thin, ultra-light and fast response become one of the trends in practice, so that the Mn-Co-Ni-O thin film materials in preparation methods and structural, optical and electrical properties and so on have been researched deeply. However, it is necessary to be further explored that the properties and applications of Mn-Co-Ni-O thin films in the high-temperature field.In this paper, we prepared the precursor chemical solutions of Mn-Co-M-Ni-O serials, based on the spinel structure Mn1.56Co0.96Ni0.48O4 material, which include that the Mn-Co-Ni-(Al、Mg)-O series and the SrMnO3 spinel-perovskite structural series. These precursor solutions were deposited on silicon substrates to formed thin films, and these thin films were annealed in a tubular furnace among the air at 750 ℃ for 1 h. These films with different constituents were researched in their phase structure, surface micro-morphology, optical and electrical properties. It is aimed at to analyzed that the effects of these films in optical and electrical properties by doping ions or heating. The main results are as follows:1. Series thin films, which signed as Mn-Co-Al/Mg-Ni-O, were prepared by a chemical solution deposition method. The average grain sizes of the films samples decreased with increasing Al ratios in the Mn-Co-Al-Ni-O series films. The pores on the surfaces of the films decrease after aging treatment at 150 °C for 300 h, as well the effect is more obvious and more Al. The grains of Mn1.56(Co0.9Al0.1)0.96Ni0.48O4 thin film are uniform and density, as its cations distribution on surface is almost constant after aging treatment. The electical testing results show that the room temperature resistance drift rate of Mn1.56(Co0.9Al0.1)0.96Ni0.48O4 thin film is the lowest among this series, which is the most stable one. The refractive indexs n of the aging films are larger than those annealed across the visible light range (380-780 nm). For the Mn-Co-Mg-Ni-O series films, the refractive indexs n increases with the increases of wavelength across the range at 300-850 nm; the extinction coefficient k for each Mn-Co-Mg-Ni-O film shows a strong absorption peak between 700-800 nm. Among the Mn-Co-Mg-Ni-O series films, the surface of Mn1.56(Co0.8Mg0.2)0.96Ni0.48O4 film is the smoothest and its particle size is uniform. The Mn1.56(Co0.6Mg0.4)0.96Ni0.48O4 film obtained the maximum B25/50 value of 4577 K in this series of samples.2. The Mn-Co-Al-Mg-Ni-O series thin films were prepared by a chemical solution deposition method. The particles of the Mn-Co-Al-Mg-Ni-O series thin films are fine, uniform, dense and smooth through comparing the microtopographys of quaternary films. The Mn1.56(Co0.5Al0.1Mg0.4)0.96Ni0.48O4 film has the maximum B25/50 value, which is 5794 K in this series.3. The spinel-perovskite composite structure films of [Mn1.56Co0.96Ni0.48O4]1-x[SrMnO3]x (x=0, 0.1, 0.3, 0.5) were prepared by a chemical solution deposition method. The grain chain-gully structure on the film surface is filled gradually with increasing the perovskite phase contents, resulting the light absorption were enhanced. The film, (Mn1.56Co0.96Ni0.48O4)0.5(SrMnO3)0.5, has the largest material constant B25/50 value of 5390 K among the composite films.
|张珺. Mn-Co-M(Al、Mg、Sr)-Ni-O系薄膜的制备及性能研究[D]. 北京. 中国科学院大学,2018.|
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