分析化学2024，Vol.52Issue(12)：1823-1833,11.DOI:10.19756/j.issn.0253-3820.241294
基于单颗粒碰撞电分析化学双模表征银包金核壳纳米材料的合成过程
Single Nanoparticle Collision Electrochemistry for Dual-mode Characterization of Synthesis Process of Silver-coated Gold Core-shell Nanomaterials
摘要
Abstract
The accurate characterization of the synthesis process of core-shell nanomaterials is crucial for studying their structural evolution and structure-activity relationships.In this work,a new method that combined the advantages of electrocatalytic and direct electrolytic single-nanoparticle collision for dual-mode characterization of the synthesis process of core-shell nanomaterials was developed.The method was used to accurately detect the Ag shell volume(VAg)of Au@AgNPs synthetized at different conditions on the basis of the proportional relationship between VAg and oxidation peak charge(Q).Moreover,Au@AgNPs,small-sized Au seeds and generated Ag nuclei were detected based on the amplification of electrocatalytic single-nanoparticle collision to explore the growth mechanism of Ag shells.The results showed that when 3.2×10-3 mol/L of silver nitrate and 5.3×10-4 mol/L of sodium citrate were added to the Au seed solution,and the reaction continued at 95℃for 60 min,the largest sized spherical Au@AgNPs were synthesized(d≈33 nm),with VAg of about 2.2×10-17 cm3,and both the concentration of silver nitrate solution and sodium citrate solution affected VAg.In addition,it was found that the growth of Ag shells involved nucleation and coalescence,rather than directly deposition on the surface of Au seeds after Ag+reduction.Moreover,the rates of nucleation and growth varied at different stages,reaching up to 1.0×10-17 cm3/min in the first 1 min,decreasing to 5.5×10-20 cm3/min within 30-60 min,and almost 0 cm3/min during 60-120 min,following the pattern of being fast initially,then slowing down,and finally reaching a stagnation point.This work provided a new approach to accurately characterize the synthesis process of core-shell nanomaterials,which was of great significance for precisely constructing efficient core-shell nanomaterials.关键词
核壳纳米材料/单颗粒检测/银包金/成核生长/双模Key words
Core-shell nanomaterials/Single-particle detection/Silver-coated gold/Nucleation growth/Dual-mode引用本文复制引用
白乙艳,王晨阳,谈颖,徐雅琪,杨海英..基于单颗粒碰撞电分析化学双模表征银包金核壳纳米材料的合成过程[J].分析化学,2024,52(12):1823-1833,11.基金项目
山西省应用基础研究项目(Nos.202203021212173,202203021212175)、来晋奖励项目(Nos.QZX-2022001,l2022005)、山西省高等学校科技创新项目(No.2022L471)、运城学院博士科研启动项目(Nos.YQ-2021032,2022001)和运城学院化学学科项目资助. Supported by the Applied Basic Research Program of Science and Technology Department of Shanxi Province(Nos.202203021212173,202203021212175),the Reward Program for Coming to Shanxi(Nos.QZX-2022001,2022005),the Scientific and Technological Innovation Program of Higher Education Institutions in Shanxi(No.2022L471),the Yuncheng University Doctoral Research Launch Project(Nos.YQ-2021032,2022001)and the Chemistry Department of Yuncheng University. （Nos.202203021212173,202203021212175）
