Ag/TiN复合薄膜制备及其表面增强拉曼光谱研究  

Preparation and Surface Enhanced Raman Spectroscopy of Ag/TiN Composite Films

作　　者：赵静 冯林杰 裴媛 魏恒勇 李波 吴振刚 李景武[5] ZHAO Jing;FENG Linjie;PEI Yuan;WEI Hengyong;LI Bo;WU Zhengang;LI Jingwu(School of Pharmacy,North China University of Science and Technology,Tangshan 063210,China;The 982 Hospital of the Joint Support Force of the Chinese People's Liberation Army,Tangshan 063099,China;College of Material Science and Engineering,North China University of Science and Technology,Tangshan 063210,China;College of Environmental Engineering,University of Emergency Management,Langfang 065201,China;The Cancer Institute,Tangshan People's Hospital,Tangshan 063001,China)

机构地区：[1]华北理工大学药学院,唐山063210 [2]中国人民解放军联勤保障部队第九八二医院,唐山063099 [3]华北理工大学材料科学与工程学院,唐山063210 [4]华北科技学院环境工程学院,廊坊065201 [5]唐山市人民医院肿瘤研究所,唐山063001

出　　处：《光散射学报》2022年第4期296-305,共10页The Journal of Light Scattering

基　　金：河北省自然基金(H2022209066);河北省引智项目:拉曼光谱应用于内镜和肿瘤诊断技术的研发;河北省危险化学品安全与控制技术重点实验室开放课题(20211204-5);河北省省属高校基本科研业务费项目(JQN2022015)。

摘　　要：高灵敏基底材料是表面增强拉曼光谱(SERS)技术应用的关键。本研究采用电化学沉积法将氮化钛(TiN)薄膜与贵金属银复合,利用两者协同效应提高SERS灵敏度。借助XRD、SEM、UV-VIS和Raman等测试手段系统探究了电化学沉积参数对复合基底SERS性能的影响。研究发现,当沉积液浓度为5 mmol/L、沉积电压为5 V及沉积时间为5 min时,复合基底单质Ag和TiN两种物相共存,Ag纳米颗粒沿优势晶面生长,银颗粒在TiN薄膜上生长为棒状结构,分布均匀。与其他沉积参数下制备的基底相比,上述条件下合成的复合薄膜展现出较明显的等离子体共振吸收双峰,表明体系中Ag和TiN两相间产生等离子体共振叠加效应,电磁场耦合作用增强,局部表面等离子体共振耦合作用增加,薄膜表面形成更多的SERS“热点”,并有助于促进电荷转移,进而赋予基底较为优异的SERS性能。这证实了优化电化学沉积参数来调控复合薄膜形貌从而改善SERS基底性能的可行性,可为采用电化学沉积技术制备Ag/TiN复合薄膜作为SERS基底材料提供技术支持。The highly sensitive substrate material is the key to the application of surface-enhanced Raman spectroscopy(SERS)technique.In this study,TiN thin film was compounded with noble metal silver by electrochemical deposition method to improve its SERS sensitivity by using their synergistic effect.The effects of electrochemical deposition parameters on the SERS properties of composite substrates were systematically investigated by means of XRD,SEM,UV-VIS and Raman.The results showed that when the concentration of deposition solution was 5 mmol/L,the deposition voltage was 5 V and the deposition time was 5 min,the two phases of monomeric Ag and TiN coexisted in the composite substrate,the Ag nanoparticles growth along the dominant crystal plane,and the silver particles on the TiN film grew into rod structure with uniform.Comparing with the substrates prepared under other deposition parameters,the composite film synthesized under the above conditions showed more obvious double peaks of plasma resonance absorption,which indicated that the superposition effect of plasma resonance was generated between the monomeric Ag and TiN phases in the system,the electromagnetic field coupling effect was enhanced,so that the local surface plasmon resonance coupling between them was increased,and more SERS"hot spots"were formed on the surface of the film,which was helpful to promote charge transfer,thus the substrate was endowed with more excellent SERS performance.The results confirmed the feasibility of optimizing the electrochemical deposition parameters to modulate the morphology of the composite film and thus improve the performance of SERS substrates,which provide technical support for the preparation of Ag/TiN and other noble metal-semiconductor composite films as SERS substrate materials by electrochemical deposition technology.

关 键 词：氮化钛薄膜 纳米银 电化学沉积 表面增强拉曼光谱 

分 类 号：O657[理学—分析化学]