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高分子稳定钌纳米金属簇的制备及形貌研究

Synthesis and Morphology Study of Ruthenium Nanoclusters

【作者】 牛海军

【导师】 高俊刚; 刘汉范;

【作者基本信息】 河北大学 , 高分子化学与物理, 2003, 硕士

【摘要】 本论文研究了聚乙烯基吡咯烷酮稳定的钌纳米金属簇的制备与形貌控制问题。主要工作分为以下三个部分: 1.对纳米金属簇的特性、纳米金属簇的制备及其在催化中的应用作了较系统的评述,介绍了近年来纳米金属簇的形貌研究。 2.采用回流RuCl3低沸点醇溶液的方法制备了一系列具有不同尺寸大小的高分子稳定钌纳米金属颗粒。得到平均颗粒直径从1.2nm到1.6nm且相对标准偏差均小于0.33的不同尺寸大小的窄分布的钌金属颗粒。通过改变高分子保护剂聚乙烯基吡咯烷酮的用量,溶剂纯化及惰性气体保护等实验条件因素,讨论了不同制备条件对高分子稳定的钌纳米金属簇的粒径及分布的影响。在回流的情况下,金属颗粒的尺寸随—聚乙烯基吡咯烷酮的用量减少而依次增大。说明保护剂的用量是钌纳米金属簇尺寸大小的重要影响因素。研究表明,反应体系中溶剂纯化与否和惰性气体保护对钌纳米金属簇的颗粒尺寸变化影响不大,说明溶剂中的水与空气中的氧对钌金属簇的形成过程没有大的影响。 3.提出了一种合成尺寸可控的梭状Ru金属颗粒的方法。通过增加溶液中Ru3+的浓度,可以得到具有两种微观结构的透明紫色Ru胶体溶液:一种是尺寸可在149nm到659nm范围内变化的梭状Ru金属颗粒结构;另一种是平均粒径为1.9nm的Ru纳米金属小颗粒。用透射电镜(TEM)、X-射线衍射(XRD)和紫外可见光谱表征了钌纳米金属颗粒梭状结构的形貌控制,证明梭状的Ru颗粒是由分散于胶体溶液中的平均粒径为1.9nm的Ru纳米金属小颗粒聚集而成的。

【Abstract】 This thesis is focused on the preparation and morphology control of polymer-stabilized Ru nanoparticles. It is mainly composed of the following three parts:1 A review was given on the special properties and preparation of metal nanoclusters as well as their application in catalysis. In addition, a detailed introduction was made to the morphology study of metal nanoparticles.2 A new route to the preparation of poly (N-vinyl-2-pyrrolidone) (PVP)-stabilized ruthenium colloids by refluxing ruthenium(III) chloride in low boiling point alcohols was developed. A series of Ru nanoparticles were obtained with the average diameters varying in the range of 1.2-1.6 nm with relative standard deviations of less than 0.33. The effect of different preparation conditions on the diameters and distribution of polymer-stabilized Ru colloids was investigated by altering the molar ratio of PVP : Ru, taking solvent purification, accepting inertia gas protection, and so on. Under the preparation of refluxing, the diameters of the ruthenium colloids increased with the decrease of the molar ratio of protective polymer-PVP, indicting that the amount of protective polymer used is an important factor controlling the diameter of metal nanoparticles.3 In this report, we describe a method for the synthesis of ruthenium particles with controllable shuttle-like shapes. By increasing the concentration of Ru3+ in the reaction solution, we can obtain a transparent deep purple colloidal solution of ruthenium particles which consists of two microstructues, one is large shuttle-like ruthenium particles with the lengths ranged from 149 nm to 659 nm, and the other is tiny Ru Colloids with the average diameter of 1.9 nm. TEM, XRD and UV-visible absorption spectrophotometry were introduced to study the morphology of the colloids.

  • 【网络出版投稿人】 河北大学
  • 【网络出版年期】2004年 02期
  • 【分类号】O614
  • 【下载频次】201
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