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混合溶剂法制备微纳米尺度碳酸盐和硫化物颗粒的研究
Exploration of Mixed Solvent Method and Preparation Characterization of Carbonate Particles and Sulphide Nanoparticles
【作者】 张峰;
【导师】 刘鲁梅;
【作者基本信息】 青岛科技大学 , 材料工程(专业学位), 2014, 硕士
【摘要】 物质的结构、形貌和尺寸往往影响或决定着物质的性能和应用。开发有效的方法以实现对材料结构、形貌和尺寸等的控制己经成为材料科学研究的重要课题之一。乙醇和水混合溶剂法作为一种新型的制备微观粒子特定结构和形貌的方法而得到广泛的研究。本文以乙醇和水混合作为溶剂,改变乙醇和水的比例,研究探讨了混合溶剂对无机盐(或含结晶水)微纳米粒子的作用机理,通过XRD、SEM等测试表征方法探究了混合溶剂比例,反应物浓度等因素对无机盐微纳米粒子的粒径,形貌的影响。利用UV-Vis-NIR光谱仪、光热转换装置对典型硫化物半导体材料硫化铅样品进行了光学分析及光热性能的研究。通过实验得到结论如下:1.改变混合溶剂中醇水比例,制备了四种碳酸盐粒子(碳酸锌,碳酸镍,碳酸钡,碳酸钙)。得出结论:随着醇水比例增大,得到的纳米粒子逐渐减小。通过Ostwald熟化理论,Ostwald-Freundlish方程和过饱和度与溶度积常数的关系公式分析了出现此现象的原因。探究了改变醇水比例如何导致溶剂界面张力,过饱和度,溶解度等方面的变化,进而导致了无机盐纳米粒子的变化以及反应物浓度对四种碳酸盐粒子的影响。2.改变醇水混合溶剂中醇水比例,制备了四种硫化物纳米粒子。得到结论:随着醇水比例增大,得到的纳米粒子逐渐减小。验证了制备四种碳酸盐时得出的结论。3.利用UV-Vis-NIR光谱仪、光热转换装置对硫化铅样品进行了光学分析及光热性能的研究。通过改变样品的粒度和固含量进行了光热转换性能的研究。1)样品在紫外、可见和近红外波段有较好的光吸收性能,尤其在1000-1200nm处吸收较明显。2)样品的固含量对光热转换性能有影响。随着固含量的增加,样品对光的吸收越多,光热转换性能越好。3)样品的粒径对光热转换性能有影响。随着样品粒径在一定范围内的增加,温升差越大,表明在一定范围内随着粒径的增加,样品对光的吸收越多,光热转换率越高。
【Abstract】 The structure, morphology and size of material tend to influence or determine thematerial properties and applications. To develop effective methods for achieving thecontrolling of material structure, morphology and size has gradually become one of theimportant subject of materials science. As a novel method for preparing materials withspecific composition and microscopic particles specific structure and morphology,mixed solvent method has been widely studied.In this paper, water was used as inorganic solvents, ethanol, acetone were organicsolvents. The mixed solvent could be gotten by changing the proportion of inorganicsolvents and organic solvents. The impact of changes of the mixed solvent on its ownnature and impact on the structure and morphology of different matters were studiedwith Scanning electron microscopy (SEM) and X-ray diffraction (XRD) Furthermore,UV-Vis-NIR s pectrometer and photothermal evaluation system were applied toanalyze the optical property and photothermal performance of the PbS products. Theresults are as follows:1. Four carbonate nanoparticles were prepared by changing the proportion ofalcohol-water mixed solvent. It is worthy emphasizing that when the characterizationof carbonate particle size, we found that with increasing of organic components in themixed solvent, the particle size obtained became smaller and this variation wasconsistent with the law of the surface tension of the mixed solvent.We analysised of the reasons for this phenomenon by Ostwald ripening theory, Ostwald-Freundlishequation and the Formula of supersaturation with solubility product constant. Exploredthe changes in the ratio of ethanol and water how to lead to the changes of solventinterfacial tension, supersaturation and solubility.2. Four kinds of sulfide semiconductor nanoparticles were prepared by changingthe proportion of alcohol-water mixed solvent. It is worthy emphasizing that when thecharacterization of sulfide semiconductor nanoparticles size, we found that withincreasing of organic components in the mixed solvent, the particle size obtainedbecame smaller and this variation was consistent with the law of the surface tension ofthe mixed solvent3. UV-Vis-NIR s pectrometer and photothermal evaluation system were applied toanalyze the optical property and photothermal performance of the PbS products.1) The as-prepared product exhibits fairly well property of light absorption inultraviolet, visible, near infrared bands, especially at1000-1200nm.2)The solid content of the samples has an effect on the photothermal conversionperformance. The absorption of light and photothermal properties is proportional to thesolid content.3) The sample size can affect the photothermal conversion performance. As thesample size increases in a certain range, the temperature difference became greater.Showed that with the increase of partical size in a certain range, the light-heatconversion rate becomes higher.
【Key words】 Mixed solvent; Micro/Nano particles; Optical absorption; photothermal conversion;