分步液相还原法制备六方片状纳米银粉工艺研究  

Research on Processing of Ag Hexagonal Nanoplates by Stepwise Liquid-phase Reduction Method

作　　者：刘庆滨 朱一民[1,2] 韩跃新 董再蒸[1,2] LIU Qingbin;ZHU Yimin;HAN Yuexin;DONG Zaizheng(Institute of Mineral Engineering and Powder Technology,School of Resources and Civil Engineering,Northeastern University,Shenyang 110819,China;Liaoning Mineral Materials Technology Innovation Center,Shenyang 110819,China)

机构地区：[1]东北大学资源与土木工程学院矿物工程与粉体技术研究所,沈阳110819 [2]辽宁省矿物材料专业技术创新中心,沈阳110819

出　　处：《有色金属（选矿部分）》2024年第5期190-198,共9页Nonferrous Metals（Mineral Processing Section）

基　　金：辽宁省科技创新平台建设项目。

摘　　要：为探究分步液相还原法制备六方片状纳米银粉工艺条件对纳米银粉形貌及粒径的影响,以硝酸银为银源,过氧化氢为氧化刻蚀剂,硼氢化钠、抗坏血酸为还原剂,柠檬酸钠为形貌诱导剂,通过分步液相还原法制备出了六方片状纳米银粉。考察了制备工艺中晶种阶段过氧化氢用量、硼氢化钠用量、生长阶段柠檬酸钠用量、反应溶液pH值等工艺条件对纳米银粉形貌及粒径的影响规律,并分析了其影响机理。结果表明,当晶种阶段过氧化氢与硝酸银摩尔比为50∶1、硼氢化钠与硝酸银摩尔比为2∶1、生长阶段柠檬酸钠与硝酸银摩尔比为2∶1,反应溶液pH=8时,可制备出粒度分布均匀的六方片状纳米银粉,其六边形平均边长为40~60nm。晶种阶段过氧化氢用量是影响纳米银粉形貌的关键因素,随过氧化氢用量增大,纳米银粉形貌发生由类球状到片状的转化,过氧化氢过量可使片状纳米银粉边缘发生刻蚀作用;生长阶段反应溶液酸碱度是影响纳米银粉粒径的关键因素,随反应溶液pH值增大,纳米银粉平均粒径逐渐减小;柠檬酸钠可在纳米银粉表面发生选择性吸附,诱导纳米银粉发生各向异性生长,生成片状结构。In order to investigate the effect of the process conditions on the morphology and particle size of Ag hexagonal nanoplates prepared by liquid-phase reduction method,the Ag hexagonal nanoplates were prepared by stepwise liquid phase reduction method using AgNO3as raw material,H2O2as oxidizing etchant,NaBH4and AA as reducing agents,TSC as morphology inducer.We investigated the influence law of process conditions such as H2O2and NaBH4dosage at the stage of crystal seeding,TSC dosage at the stage of growth,and solution pH on the morphology and particle size of nanosilver,and analyzed the influence mechanism.The results showed that the production of Ag hexagonal nanoplates was more favorable when the molar ratio of H2O2/AgNO3in the growth phase was 50∶1,the molar ratio of NaBH4/AgNO3 was 2∶1,the molar ratio of TSC/AgNO3in the growth phase was 2∶1,and the pH of the reaction solution was 8,the average edge length of Ag hexagonal nanoplates was between 40and 60nm.The amount of H2O2in the crystal seeding stage was the key factor affecting the morphology of the nanosilver,with the increase of H2O2,the morphology of the nano-silver experiences a transformation from sphere to flaky,and the excess of H2O2can make the edge of silver nanoplate experiences an etching effect.The pH of the reaction solution during the growth phase was a key factor affecting the particle size of the nano-silver,with the increase of the pH of the reaction solution,the average particle size of the nanosilver decreases.Sodium citrate can undergo selective adsorption on the surface of nano-silver,which induced anisotropic growth of nano-silver and generates a lamellar structure.

关 键 词：片状纳米银 液相还原法 形貌调控 制备工艺 

分 类 号：TD989[矿业工程—选矿]