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目的:开发出切实可行的石英毛细管内壁镀金工艺,应用于激光拉曼的气体分析检测中。方法先用石英玻璃片进行镀金工艺研究,经过对羟基化、硅烷化、纳米金颗粒修饰、湿法镀金各步条件参数的确定,获得最佳的镀金工艺方案,再对相关参数进行调整,应用于石英毛细管。将镀金石英毛细管应用于激光拉曼的气体分析测试中,分析其对散射信号的增强效果。结果 NaOH的浓度和毛细管内溶液的流速及时间显著影响纳米金颗粒的吸附沉积。最佳的石英毛细管内壁镀金工艺为:5 mol/L NaOH处理1 minˇAPTMS/IPA烷基化修饰ˇ金溶胶在流速0.8 mL/min下处理4 hˇ含盐酸羟胺的镀金液在流速0.8 mL/min下处理4 h。该工艺制得的内壁镀金毛细管用于气体拉曼测试后,可将空气中N2相对峰值从148 counts(未镀金毛细管)提高至480 counts。结论制备出的镀金石英毛细管可增强激光拉曼检测气体的信号,为进一步实现气体在线拉曼监测奠定基础。

ABSTRACT:Objective To develop feasible gold deposition technology on the inner wall of the quartz capillary, which is used for gas detection and analysis by laser Raman. Methods Gold plating was studied with quartz glass first and an optimal technology was achieved after the determination of condition parameters for hydroxylation, silanization, gold nanoparticles modification and wet plating. Then this process was applied to the quartz capillary after adjustment of relevant parameters. The gilded quartz capillary was used for gas analysis through laser Raman measurements, and the enhancement effect of scattering signals was analyzed. Re-sults The concentration of sodium hydroxide, the flow rate and flow time of solution in the capillary obviously affected the adsorption of gold nanoparticles. The optimal technology for gold plating inside the quartz capillary was as following:5 mol/L NaOH treatment for 1 minˇAPTMS/IPA alkylated modificationˇgold sol process at the flow rate of 0. 8 mL/min for 4 h ˇtreatment with plating liquid containing hydroxylamine hydrochloride for 4 h at the flow rate of 0. 8 mL/min. The gilded capillary was used for gas Raman tests and the relative peak strength of N2 in the air was increased from 148 counts ( without gold plating) to 480 counts. Conclu-sion By the use of gold-deposited quartz capillary, corresponding signals of gas could be effectively enhanced under laser Raman detection, which lays a foundation for the further in-situ Raman analysis of gas.

参考文献

[1] 李颖,段玉然,李维华.纳米锐钛矿的拉曼光谱特征[J].光谱学与光谱分析,2000(05):699-701.
[2] 卢灿忠,杨文斌,汪盛,吴传德,林祥,庄鸿辉.纳米无机巨簇分子的红外、拉曼光谱研究[J].光谱学与光谱分析,2000(06):838-839.
[3] WANGSY;HANSTYUCE;WASTONPA et al.Analysis of Metabolites in Aqueous Solutions by Using Laser Raman Spectroscopy[J].Applied Optics,1993,32(06):925-929.
[4] Bell Steven E. J. .Rapid analysis of ecstasy and related phenethylamines in seized tablets by Raman spectroscopy[J].The Analyst: The Analytical Journal of the Royal Society of Chemistry: A Monthly International Publication Dealing with All Branches of Analytical Chemistry,2000(3):541-544.
[5] 吴维中;柯惟中 .激光拉曼光谱法验证中草药有效成分的结构特征[J].光谱学与光谱分析,1995,15(06):51-54.
[6] FLEISCHMANNM;HENDRAPJ;MCQUILLAA .Raman Spectra of Pyridine Adsorbed at a Silver Electrode[J].CHEMICAL PHYSICS LETTERS,1974,26(02):163-166.
[7] JEANMAIREDL;VANDUYNERP .Surface Raman Spec-tro Electrochemistry:Part 1. Heterocyclic,Aromatic,and Ali-phatic Amines Adsorbed on the Anodized Silver Electrode[J].Journal of Electroanalytical Chemistry,1977,84(01):1-20.
[8] GERSTENJI;BIRKERL;LOMBARDIJR .Theory of En-hance i Light Scattering from Molecules Adsorbed at the Metal-solution Interface[J].Physical Review Letters,1979,43(02):147-150.
[9] 郑军伟,李晓伟,周跃国,顾仁敖.银纳米粒子阵列的自组装及其表面增强拉曼光谱应用[J].光谱学与光谱分析,2000(06):814-816.
[10] JOYDEEP C D;MANASH G;MISRA T N .Surface-enhanced Raman Scattering of 2,2忆-biquinoline Adsorbed on Colloidal Silver Particles[J].Spectrochimica Acta Part A:Molecular and Biomolecular Spectroscopy,2000,51:2107-2115.
[11] 刘玲.激光拉曼光谱及其应用进展[J].山西大学学报(自然科学版),2001(03):279-282.
[12] Hu, X.;Meng, G.;Huang, Q.;Xu, W.;Han, F.;Sun, K.;Xu, Q.;Wang, Z. .Large-scale homogeneously distributed Ag-NPs with sub-10nm gaps assembled on a two-layered honeycomb-like TiO _2 film as sensitive and reproducible SERS substrates[J].Nanotechnology,2012(38):385705-1-385705-6.
[13] Huang, Z.;Meng, G.;Huang, Q.;Chen, B.;Zhu, C.;Zhang, Z. .Large-area Ag nanorod array substrates for SERS: AAO template-assisted fabrication, functionalization, and application in detection PCBs[J].Journal of Raman Spectroscopy: An International Journal for Original Work in All Aspects of Raman Spectroscopy, Including Higher Order Processes, and Also Brillouin- and Rayleigh Scattering,2013(2):240-246.
[14] ZHOU Q;ZHANG X;HUANG Y et al.Rapid Detection of Polychlorinated Biphenyls at Trace Levels in Real Environ-mental Samples by Surface-enhanced Raman Scattering[J].SENSORS,2011(11):10851-10858.
[15] Bianhua Liu;Guangmei Han;Zhongping Zhang;Renyong Liu;Changlong Jiang;Suhua Wang;Ming-Yong Han .Shell Thickness-Dependent Raman Enhancement for Rapid Identification and Detection of Pesticide Residues at Fruit Peels[J].Analytical chemistry,2012(1):255-261.
[16] Godhuli Sinha;Laura E. Depero;Ivano Alessandri .Recyclable SERS Substrates Based on Au-Coated ZnO Nanorods[J].ACS applied materials & interfaces,2011(7):2557-2563.
[17] 周宥辰,王艳艳,马志方,姜艳霞,邱瑾,孙世刚.湿化学镀SPR金基底及其性能表征[J].电化学,2011(01):31-36.
[18] GRABAR K C;FREEMAN R G;HOMMER M B et al.Preparation and Characterization of Au Colloid Monolayers[J].Analytical Chemistry,1995,67:735-743.
[19] Grabar KC;Smith PC;Musick MD;Davis JA;Walter DG;Jackson MA .KINETIC CONTROL OF INTERPARTICLE SPACING IN AU COLLOID-BASED SURFACES - RATIONAL NANOMETER-SCALE ARCHITECTURE[J].Journal of the American Chemical Society,1996(5):1148-1153.
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