铜基纳米线的宏量制备及其对聚甲醛的改性研究

发布时间：2018-03-26 13:21

  本文选题：铜纳米线　切入点：聚甲醛　出处：《河南大学》2015年硕士论文

【摘要】：本论文研究优化了液相还原法制备铜纳米线的方法,并开发出宏量制备的工艺,主要工作包括碱液、铜源的浓度变化而引起铜纳米线在形貌上的尺寸变化,从能源环保可持续发展、减小制备成本的角度出发,将工作重点放在碱液的循环利用、铜源由文献惯用的的硝酸铜优化为无杂质污染碱液的氢氧化铜,开发出不同规格铜纳米线制备的工艺,为铜纳米线的广泛应用的提供了制备基础;然后将铜纳米线作为改性体与聚甲醛共混制备复合材料,评价了添加改性体后对POM的性能影响。本论文主要工作内容和结果如下几个方面:(1)以硝酸铜为原料的铜纳米线制备在Na OH碱液里,以硝酸铜与乙二胺的络合体为前躯体、水合肼为还原剂,利用液相还原法制备了的铜纳米线,并且对样品进行了扫描电镜、透射电镜、X射线衍射仪形貌、结构的表征。通过改变碱液浓度、铜源浓度等条件制得了不同规格的铜纳米线,而且实现了系列反应釜的规模制备;另外通过大量的重复实验、改变实验细节可以将碱液做到5次的循环利用,大大降低了制备成本,同时也减小了污染、能耗。(2)以氢氧化铜为原料的铜纳米线制备与硝酸铜相比,还原氢氧化铜后不产生杂质污染物,故以Cu(OH)2为原料制备了一种直径约200nm,长度大于40μm的铜纳米线,并且实现了50L以下的反应制备,该工艺还可以做到碱液的连续循环使用,这样大大提高了制备效率和降低成本。另外一种规格的铜纳米线为直径为100-300nm,长度大于30μm,该工艺也可以实现碱液的连续循环使用。(3)铜镍合金纳米线的制备在碱性体系下,改变铜镍比,得到复合纳米线,当铜镍比为20:1时,可以制得粒径均一、直径小于100nm、长度大于50μm的合金纳米线,并且可以放大至3L反应体系进行制备。(4)铜纳米线/聚甲醛复合材料的制备及性能测试采用熔融共混法制备了铜纳米线/聚甲醛的复合材料,并通过XRD衍射、拉伸与冲击、热分析仪、UMT-2微摩擦磨损试验机以及扫描电镜等手段对基体和复合材料进行了测试,分析了材料的结构、力学性能、热稳定性、摩擦学性能、断面和磨痕形貌等。结果表明铜纳米线在复合材料里有较好的分散性,添加后大大提高了POM的热稳定性和摩擦学性能,力学性能有轻微的改善。
[Abstract]:In this paper, the preparation method of copper nanowires by liquid reduction method was optimized, and the macroscopical preparation process was developed. The main work included the changes of the concentration of alkali solution and copper source, which resulted in the change of the size of copper nanowires in morphology. In view of the sustainable development of energy and environmental protection and the reduction of preparation cost, the emphasis of the work is on the recycling of lye. The copper source is optimized from copper nitrate, which is commonly used in literature, to copper hydroxide without impurity pollution. The preparation process of copper nanowires with different specifications has been developed, which provides a basis for the wide application of copper nanowires, and then copper nanowires are used as modifiers to prepare composite materials by blending with polyformaldehyde. The main contents and results of this paper are as follows: 1) Copper nanowires were prepared from copper nitrate as raw material in NaOH alkali solution, and the complex of copper nitrate and ethylenediamine was used as precursor, and the main results were as follows: (1) Copper nanowires with copper nitrate as raw material were prepared in NaOH alkali solution, and the complex of copper nitrate with ethylenediamine was used as precursor. Copper nanowires were prepared by liquid phase reduction with hydrazine hydrate as reductant. The morphology and structure of the samples were characterized by SEM, TEM and XRD. Copper nanowires of different specifications have been prepared under the conditions of copper source concentration, and the scale preparation of series of reactors has been realized. In addition, through a large number of repeated experiments, the lye can be recycled for 5 times by changing the experimental details. Compared with copper nitrate, copper nanowires prepared from copper hydroxide can not produce impurity pollutants after reduction of copper hydroxide. Therefore, a kind of copper nanowires with diameter of about 200nm and length of more than 40 渭 m were prepared from Cu(OH)2, and the reaction below 50L was realized. This greatly improves the preparation efficiency and reduces the cost. Another type of copper nanowires is 100-300 nm in diameter and more than 30 渭 m in length. The process can also realize the continuous recycling of lye. 3) the preparation of copper and nickel alloy nanowires in alkaline system. When the Cu / Ni ratio is 20:1, the alloy nanowires with diameter less than 100 nm and length greater than 50 渭 m can be obtained. The copper nanowires / POM composites were prepared by melt blending method. The composites were prepared by XRD diffraction, tensile and impact. The microstructure, mechanical properties, thermal stability, tribological properties and tribological properties of the matrix and composite materials were analyzed by means of thermal analyzer UMT-2 micro-friction and wear tester and scanning electron microscope (SEM), and the microstructure, mechanical properties, thermal stability and tribological properties of the composites were analyzed. The results show that copper nanowires have good dispersion in the composites, and the thermal stability and tribological properties of POM are greatly improved by adding copper nanowires, and the mechanical properties are slightly improved.
【学位授予单位】：河南大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.1;TQ326.51

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