物理化学学报 >> 2004, Vol. 20 >> Issue (02): 211-215.doi: 10.3866/PKU.WHXB20040222

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晶种法合成金溶胶过程中非球形粒子的抑制

曹林有;朱涛;刘忠范   

  1. 北京大学化学与分子工程学院,纳米科技中心,北京　100871
  • 收稿日期:2003-07-31 修回日期:2003-09-19 发布日期:2004-02-15
  • 通讯作者: 朱涛 E-mail:tzhu@chem.pku.edu.cn

Synthesis of Gold Colloid with Exclusion of Nonspherical Nanoparticles by Seeding Growth

Gao Lin-You;Zhu Tao;Liu Zhong-Fan   

  1. Center for Nanoscale Science and Technology, College of Chemistry and Molecular Engineering, Peking University, Beijing　100871
  • Received:2003-07-31 Revised:2003-09-19 Published:2004-02-15
  • Contact: Zhu Tao E-mail:tzhu@chem.pku.edu.cn

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摘要： 羟胺晶种法制备金纳米粒子时会观察到少量的非球形粒子副产物.研究发现,反应试剂的比例以及试剂的加样顺序对非球形粒子的产生具有明显的影响.羟胺与金氯酸的摩尔比例([NH2OH]:[HAuCl4])较高时能够抑制非球形粒子的生成,较低时则生成较多的非球形粒子.不同的加样顺序使得加样过程中[NH2OH]:[HAuCl4]不同,也可以导致产物中非球形粒子含量的差异.基于以上发现,采用较大的NH2OH用量以维持反应过程中的[NH2OH]:[HAuCl4]比例在10～30左右,并采用适当的加样顺序(先将晶种同NH2OH混合,再加HAuCl4),从14 nm的晶种出发以逐步(step-by-step)的方式依次合成了平均粒径为26、57、81和130 nm的金纳米粒子,产物中基本不含非球形粒子,粒径可控，并具有良好的单分散性(RSD为～10％).

关键词: 晶种法, 金纳米粒子, 非球形粒子

Abstract: This paper reports a method for the preparation of monodispersed gold colloid by seeding growth, with elimination of the nonspherical by-products, which were often observed and difficult to separate in previous works. The formation of nonspherical particles was found to be closely associated with the experimental conditions, such as, molar ratios and addition sequence of the reagents. The larger the [NH2OH]:[HAuCl4] ratio, the less and smaller the nonspherical particles. In addition, the effect of addition sequence can be ascribed to that of [NH2OH]:[HAuCl4] ratio, since different addition sequences make different instantaneous [NH2OH]:[HAuCl4] ratios during the addition and thus lead to different shape distribution of particles. Based on these findings, a method is adopted to rule out the nonspherical particles, by using high ratios of [NH2OH] to [HAuCl4] (the [NH2OH]:[HAuCl4] ratio being kept in the range of 10～30) and favorable addition sequence (NH2OH being added to seeds prior to HAuCl4). No nonspherical nanoparticles can be observed, and the resulted gold colloid shows good monodispersity and excellent size-controllability.

Key words: Seeding growth method, Gold nanoparticles, Nonspherical particles