电化学法制备纳米锑粉的研究

发布时间：2019-04-09 10:38

【摘要】： 本论文主要采用电化学法制备了纳米锑粉末,运用X射线衍射(XRD)、透射电子显微镜(TEM)及傅立叶变换红外光谱(FT-IR)等分析测试手段对所制备的纳米锑粉进行了分析和表征。研究对于对电化学方法制备纳米锑粉的工艺进行了大量的试验。通过XRD、TEM和FT-IR红外光谱等检测手段,分析了制备粉体的相结构,粒径大小与团聚情况。结果表明：不同实验条件下,所制备的纳米锑粉相结构都是一致的,只是粉体的粒径大小,形貌,团聚情况,以及氧化情况随实验条件发生变化。研究发现,表面分散剂在纳米粉体制备过程中具有重要作用,即纳米晶核在电沉积后会被表面分散剂包覆,从而抑制了晶粒的生长,同时使纳米颗粒具有了常温抗氧化的能力。对表面分散剂的选择进行了较深入的分析,通过实验分析发现,使用乳化剂OP-10作为表面分散剂进行纳米锑粉的制备,能够获得尺寸较小、分散性较好、颗粒分布较窄、抗氧化性能较强的纳米锑粉颗粒。为考察电流密度和电解时间对电化学制备纳米锑粉粒径的影响,进行了单因素试验的研究。电流密度的大小,影响着形核速率；电解时间,影响着表面分散剂的浓度问题。结果表明：电流密度与电解时间都可以影响到粉体的粒径、团聚和氧化情况。其中,电流密度小于10mA/cm2时,纳米颗粒较大；电流密度约为25mA/cm2时,可获得较为理想的纳米球形颗粒。通过设计电解时间,可以制备得到粒径在12nm到100nm以上的纳米粉体；电解时间为30min时,可获得较为理想的纳米球形颗粒。
[Abstract]:In this paper, nano-antimony powder was prepared by electrochemical method. X-ray diffraction (XRD), was used to prepare nanometer antimony powder. The nano-antimony powders were characterized by transmission electron microscopy (TEM) and Fourier transform infrared spectroscopy (FT-IR). A large number of experiments have been carried out on the preparation of nano-antimony powder by electrochemical method. The phase structure, particle size and agglomeration of the prepared powder were analyzed by means of XRD,TEM and FT-IR infrared spectroscopy. The results show that the phase structure of the nano-antimony powder prepared under different experimental conditions is the same, except that the particle size, morphology, agglomeration and oxidation of the nano-antimony powder change with the experimental conditions. It is found that the surface dispersant plays an important role in the preparation of nano-powder, that is, the nanocrystalline core will be coated by surface dispersant after electrodeposition, which can inhibit the growth of grain and make the nano-particles have the ability of anti-oxidation at room temperature. The selection of surface dispersant was analyzed deeply. It was found that the preparation of nanometer antimony powder with emulsifier OP-10 as surface dispersant could obtain smaller size, better dispersion and narrower distribution of particles. Antimony nanoparticles with strong antimony resistance. In order to investigate the effect of current density and electrolysis time on the particle size of nano-antimony powder prepared by electrochemistry, a single-factor experiment was carried out. The size of current density affects nucleation rate and electrolysis time affects the concentration of surface dispersant. The results show that both the current density and electrolysis time can affect the particle size, agglomeration and oxidation of the powders. When the current density is less than 10mA/cm2, the nano-particles are larger, and when the current density is about 25mA/cm2, the ideal nano-spherical particles can be obtained. By designing the electrolysis time, the nano-powders with particle size from 12nm to 100nm can be prepared, and when the electrolysis time is 30min, the ideal nano-spherical particles can be obtained.
【学位授予单位】：兰州理工大学
【学位级别】：硕士
【学位授予年份】：2010
【分类号】：TB383.1

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