无机类富勒烯结构镍基纳米材料的表面增强拉曼散射效应  

Surface-Enhanced Raman Scattering of Inorganic Fullerene-like Nickel-Based Materials

作　　者：舒敏 李俊芳[2] 梁俊辉 陈达[1] 席广成[2] SHU Min;LI Junfang;LIANG Junhui;CHEN Da;XI Guangcheng(College of Materials and Chemistry,China Jiliang University,Hangzhou 310018,China;Chinese Academy of Inspection and Quarantine,Beijing 100020,China)

机构地区：[1]中国计量大学材料与化学学院,杭州310018 [2]中国检验检疫科学研究院,北京100020

出　　处：《光散射学报》2023年第4期399-406,共8页The Journal of Light Scattering

基　　金：国家自然科学基金(22374139)。

摘　　要：本研究采用溶剂热法成功制备了具有类富勒烯结构的羟基氯化镍纳米球,并将其作为表面增强拉曼散射(SERS)基底,以结晶紫(CV)作为探针分子,通过532 nm激发对其SERS性能进行研究。结果显示,该基底的最低检测限为10^(-8) mol/L。通过引入硫元素并调节反应物浓度比例,成功制备了硫-羟基氯化镍,并保持了类富勒烯结构。研究发现,掺杂硫后的基底能够更有效地增强拉曼散射效应,提高了检测灵敏度,并实现了对结晶紫(CV)的痕量检测,检测浓度可达到10^(-11) mol/L,提升了3个数量级。此外,通过对5000个测量点的SERS信号强度统计,得到了硫-羟基氯化镍基底的信号相对标准偏差(RSD)值为4.4%,表明其具有良好的重现性和均匀性。使用扫描电子显微镜(SEM)、透射电子显微镜(TEM)和X射线衍射仪(XRD)对羟基氯化镍和硫羟基氯化镍进行了形貌结构表征。In the present study,a solvent-thermal method was used to successfully synthesise hydroxylated nickel chloride with a fullerene-like structure.This synthesized material was implemented as a substrate for surface-enhanced Raman scattering(SERS),and crystal violet(CV)served as a probe molecule to evaluate the SERS performance under an excitation wavelength of 532 nm.The results obtained demonstrate the remarkable sensitivity of the substrate in detecting crystal violet,even at the significantly low concentration of 10^(-8) mol/L.Furthermore,by introducing sulphur and carefully adjusting the concentration ratios of the reactants,a sulphur-hydroxylated nickel chloride compound was synthesised while retaining its characteristic fullerene-like structure.This incorporation of sulfur into the substrate effectively enhanced the Raman scattering effect,thereby significantly improving its sensitivity for the detection of trace amounts of crystal violet(CV)at an unprecedented concentration as low as 10^(-11) mol/L,resulting in an improvement of three orders of magnitude.In addition,an examination of the SERS signal from 5000 data points revealed a standard deviation(RSD)of 4.4% for the sulphur-hydroxylated nickel chloride substrate,indicating exceptional reproducibility and uniformity.The morphological and structural characterisation of both hydroxylated and sulphur-hydroxylated nickel chloride was carried out using various analytical techniques such as scanning electron microscopy(SEM),transmission electron microscopy(TEM)and X-ray diffraction(XRD).

关 键 词：表面增强拉曼光谱 无机类富勒烯 硫掺杂 纳米材料 结晶紫 

分 类 号：O652.1[理学—分析化学]