铜基硫族纳米材料的可控合成及其在生化分析中的应用

发布时间：2018-01-03 12:40

本文关键词：铜基硫族纳米材料的可控合成及其在生化分析中的应用　出处：《西南大学》2015年博士论文　论文类型：学位论文

【摘要】：铜基硫族纳米材料因其优越的光学、电学、热学及其它物理化学性质,在多个领域被广泛研究。随着纳米技术的飞速发展,二元铜基硫族纳米材料将来可能被广泛应用于催化、电化学、能源、医疗诊断等领域。因此,探索研究多功能铜基硫族纳米材料的高效合成方法及应用具有一定的实际意义和价值。目前,铜基硫族纳米材料的研究还处于初始阶段,主要集中在多功能纳米材料的合成和性质探索方面,整体属于基础研究范畴。但其中使用最多的合成方法及合成材料的性质仍存在一些缺陷,例如牺牲模板法存在模板难以完全去除、耗时、成本高、过程复杂及合成的材料催化活性低等缺陷。所以,本文以不同形状铜基硫族纳米材料的合成及应用研究为目的,针对目前已有的合成方法及性质的不足开展以下研究内容：1.建立一个新颖、简单、快速、高效、可控的低温常压溶剂法,用于合成凹面CuS材料。分别对影响材料结构、大小及形貌的因素进行分析,结果发现通过调节反应条件可以实现不同形貌和大小CuS材料的可控合成；在此基础上通过时间相关的扫描电镜图像分析,提出了一个凹面CuS材料的可能形成机理；然后通过对亚甲蓝的催化降解及动力学研究,证实了我们合成的CuS材料具有极强的催化活性。2.在经典模板协助高压法的基础上,建立一个新颖的模板协助常压低温一锅水热法。采用该方法,我们成功合成了空心多孔CuS纳米球,并且对影响纳米球大小、形貌及分散性的因素,如反应温度、时间、还原剂量等进行分析,发现空心多孔CuS纳米球可以实现多通道可控合成。还发现该方法具有简单、可控、安全、经济等优点,可以实现大批量合成。然后将合成的空心多孔CuS纳米球用于催化氧化TMB的酶活性研究,结果证实该材料具有优良的过氧化物酶活性。进一步将其用于葡萄糖的检测,结果表明该方法线性范围宽,适合于大浓度葡萄糖的分析。最后通过比较发现,我们合成的空心多孔CuS纳米材料的酶催化活性远远优于已报道的相关CuS材料。3.三元CuSySe1-y合金多孔材料的合成、表征及性质探索。研究包含三个方面内容：1)通过自己建立的模板水热法,首先成功合成了三元CuSySe1-y合金多孔材料,并对其进行详细的表征。2)分别对影响材料粒径大小、形貌、分散性及均匀性的因素进行分析,结果发现反应温度、NaOH和还原剂量分别为50℃、550μmo1和100 μmol时,合成的三元CuSySe1-y合金多孔材料具有较好的形貌、分散性及均匀性。3)合成的三元合金多孔材料具有较好的局域等离子共振性质,通过改变S／Se摩尔比例,实现近红外局域等离子共振吸收从1027到1400 nm宽度可调,同时带隙从1.42到1.91 eV也对应可调。该研究为三元CuSySe1-y合金材料在光热治疗和光电转换方面的应用提供理论基础。4.树突状Cu20模板和Cu1-xSySe1-y合金纳米材料的合成及其在双氧水分析中的应用。通过简单的常压低温模板水热法,我们首先成功合成了树突状Cu20模板和Cu2-xSySe1-y合金纳米材料,并对其进行详细的表征。然后对影响材料粒径大小和形貌的因素分别进行分析,发现NaOH的量和反应温度对树突状Cu2-xSySe1-y合金纳米材料形貌和大小影响较大,而葡萄糖和还原剂的量影响较小。进一步通过时间相关的扫描电镜观察方式,重点研究了树突状Cu20模板的形成机理。最后将合成的Cu2-xSySe1-y合金纳米材料应用于双氧水的分析检测。总之,本文以不同形状铜基硫族纳米材料的合成为起点,以扫描电镜图片和吸收光谱为主要研究手段,探索新颖简单的合成方法及应用。
[Abstract]:Copper based chalcogenide nano materials because of its excellent optical, electrical, thermal and other physical and chemical properties, has been widely studied in many fields. With the rapid development of nanotechnology, two yuan of copper based chalcogenide nanomaterials may have been widely used in catalysis, electrochemistry, energy field, medical diagnosis and so on. Therefore, exploration has certain practical significance and value of efficient synthesis method of multifunctional copper based chalcogenide nano materials and application. At present, the research of copper based chalcogenide nano materials is still in the initial stage, mainly concentrated in the exploration of synthesis and properties of multifunctional nano materials, the overall belongs to the basic research category. But the nature of the use of the most the synthesis and materials, there are still some shortcomings, such as sacrificial template method is difficult to completely remove the template, time-consuming, high cost, complex process and synthetic materials. So the catalytic activity of low defect In this paper, the aim is to study the synthesis and application of different shapes of copper based chalcogenide nano materials, carry out the following research contents in view of the current shortage of the existing synthesis methods and properties: 1. to establish a novel, simple, fast, efficient, low temperature and low pressure solvent control, for a concave CuS material. Influence of materials the structure, size and morphology of factor analysis, the results found by adjusting the reaction conditions can achieve the controllable synthesis of different morphology and size of CuS material; scanning electron microscopy image analysis by the time related on the basis of this, put forward a concave CuS material formation; then through the research on the photocatalytic degradation of methylene blue and kinetics we confirmed, the synthesis of CuS based material has a strong catalytic activity of.2. assisted high pressure method in the classical template, create a new template to assist a low temperature The pot hydrothermal method. Using this method, we successfully synthesized porous hollow CuS nanospheres, and the influence of nanoparticle size, morphology and dispersion of the factors, such as reaction temperature, time and dose reduction were analyzed, found that porous hollow CuS nanospheres can realize multichannel controllable synthesis. This method is also found simple, controllable, safe, economic and other advantages, can realize batch synthesis. Then porous hollow CuS nanospheres synthesized for the study of enzyme activity in the catalytic oxidation of TMB, results show that the material has excellent peroxidase activity. Further used for the detection of glucose, the results show that this method has wide linear range, analysis suitable for high concentration glucose. Finally, by comparison, enzyme catalytic activity we synthesized hollow porous CuS nano material is much better than that of CuS material.3. reported three yuan CuSySe1-y alloy porous material The synthesis, characterization and properties of exploration. Research includes three aspects: 1) through the build template hydrothermal method, the first successful synthesis of materials three yuan of porous CuSySe1-y alloy were characterized with.2, respectively) on its influence on the material particle size, morphology, dispersion and uniformity factor the analysis results showed that the reaction temperature, NaOH and reducing doses were 50 DEG C, 550 mo1 and 100 mol, three yuan CuSySe1-y alloy synthesized porous materials has good morphology, dispersibility and uniformity of.3) three alloys synthesized porous materials with good properties of local plasmon resonance, by changing the the S / Se molar ratio, the near infrared plasmon resonance absorption from 1027 to 1400 nm and the band gap width is adjustable from 1.42 to 1.91 eV is adjustable. The corresponding research is three yuan CuSySe1-y alloy in photothermal therapy and photoelectric conversion To provide theoretical basis of.4. synthesis of dendritic Cu20 template and Cu1-xSySe1-y alloy nano material and its application in the analysis of hydrogen peroxide in the application. Through a simple template under atmospheric pressure and low temperature hydrothermal method, we successfully synthesized dendritic Cu20 template and Cu2-xSySe1-y alloy nano materials, and a detailed characterization of the materials. Then influence factors on particle size and morphology were analyzed, found that the influence of the amount of NaOH and reaction temperature of Cu2-xSySe1-y alloy nano materials on dendritic morphology and size is larger, and the glucose and reducing agent was less affected. Scanning electron microscopy further through time related observation, focus on the formation mechanism of dendritic Cu20 template. The detection and analysis of synthesis Cu2-xSySe1-y alloy nano materials used in hydrogen peroxide. In short, according to the different shapes of copper based chalcogenide nanomaterials synthesis Starting from the scanning electron microscope picture and absorption spectrum as the main research means, a novel and simple synthesis method and application are explored.

【学位授予单位】：西南大学
【学位级别】：博士
【学位授予年份】：2015
【分类号】：TB383.1

【参考文献】