表面增强拉曼光谱活性基底的制备与性质研究  

Preparation and Properties of Active Substrates for Surface Enhanced Raman Spectroscopic Analysis

作　　者：赵博儒 沈劲松 孙志 陈峰 陈智栋 赵健伟[1] ZHAO Bo-Ru;SHEN Jing-Song;SUN Zhi;CHEN Feng;CHEN Zhi-Dong;ZHAO Jian-Wei(College of Materials and Textile Engineering,Jiaxing University,Jiaxing 314001 China;Jiangsu Donghua Testing Technology Co.Ltd,Taizhou 214500,China;College of Materials Science and Engineering,Changzhou University,Changzhou 213100,China)

机构地区：[1]嘉兴学院材料与纺织工程学院,嘉兴314001 [2]江苏东华测试技术股份有限公司,泰州214500 [3]常州大学材料科学与工程学院,常州213100

出　　处：《分析化学》2020年第2期282-288,共7页Chinese Journal of Analytical Chemistry

基　　金：浙江省自然科学基金项目(Nos.LY19B030006,LY19E090005);国家自然科学基金项目(Nos.51861145202,51802121)资助~~

摘　　要：建立了无氰电沉积粒径约20 nm的银颗粒制备表面增强拉曼光谱活性银基底的方法,考察了基底的相关性质。利用电化学循环伏安法在不同的扫描速度下研究此沉积体系的电化学行为,结果表明,银的电沉积过程受扩散控制,当扫描速度增大时,氧化峰位略正移,但还原峰明显负移。扫描电镜表征结果表明,沉积银层的结晶形状规则,分布均匀,粒径为(20±10)nm。以甲基橙为探针,考察了沉积银基底对拉曼光谱信号的增强作用,其增强因子为5.2×105。沉积银基底对罗丹明6G(R6G)分子检测的线性范围为1×100^-12~1×100^-6 mol/L,相关系数为0.98,检出限低于1×10^-12 mol/L。拉曼光谱Mapping图表明,沉积银活性基底在大范围内的增强效果均匀。The silver active substrates with average particle size of about 20 nm for surface-enhanced Raman spectroscopic analysis were prepared using cyanide-free electrochemical deposition method.The electrochemical deposition behavior of the system was studied by cyclic voltammetry at different scanning rates.The results showed that the electrodeposition process of silver was controlled by diffusion.With the increase of scanning rate,the oxidation peak slightly shifted positively,whereas the reduction peak had a significant negative shift.The result of scanning electron microscopy showed that the silver particles were fine,uniform,and regular in shape,and their size was(20±10)nm.Using methyl orange as a probe,the enhancement of Raman spectral signal with the silver-deposited substrate was investigated,and an enhancement factor of 5.2×10^5 was obtained.The linear range for detection of rhodamine 6G was 1×10^-12-1×10^-6 mol/L,the correlation coefficient was 0.98,and the limit of the detection was lower than 1×10^-12 mol/L.Raman spectroscopy mapping also showed that the silver-deposited substrate had a uniform distribution.

关 键 词：沉积银 活性基底 表面增强拉曼散射 检出限 

分 类 号：O657.37[理学—分析化学]