以氯金酸为金源,四氯化钛为钛源,采用溶胶-凝胶得到镀膜前驱体溶液,再结合氨气还原氮化法制备Au-TiN复合薄膜,利用XRD、FE-SEM、UV-VIS-NIR、RAMAN测试表征薄膜结构、光学性能及SERS效应。结果表明,在Au-TiN复合薄膜中的TiN为面心立方晶型,Au为面心立方晶型。随Au含量的增加,Au颗粒平均粒径由50nm增加到100nm,且在复合薄膜中分布均匀。UV-VIS-NIR分析显示,随Au含量的增加,薄膜在可见光区的吸收峰出现了蓝移,并且峰形变宽。利用R6G作为探针分子研究了Au-TiN复合薄膜的SERS效应,结果表明,Au-TiN复合薄膜具有显著的拉曼增强效应,当Au含量为6mol%时,复合薄膜的拉曼增强效应最佳,检测极限可达10-5M,增强因子为0.55×103,且放置2个月后SERS能力仅降低28%。
Chlorauric acid and titanium tetrachloride were used as raw materials,the precursor solution was prepared by sol-gel method and the Au-TiN composite films were prepared by ammonia reduction nitriding process.The structure,optical properties and SERS effect were characterized by XRD,FE-SEM,UV-VIS-NIR and RAMAN tests.The results showed that TiN was the face centered cubic crystal and Au was the face centered cubic crystal in the Au-TiN composite films.With the increase of Au content,the size of Au particles increased from the average 50nm to the average 100nm.Meanwhile,the optical absorption peaks of the films in the visible region showed blue shift and the peak became broad.The SERS of TiN film was studied using R6G as a probe molecule.The results showed that the Au-TiN films had significant SERS effect.When the Au content was 6mol%,the raman enhancement effect of the films was the best,the detection limit was up to 10-5M,the enhancement factor was 0.55×103,and the raman enhancement effect decreased only 28% after 2 months.
[1] Rodríguez-Fernández D,Langer J,Henriksen-Lacey M,et al.Hybrid Au-SiO2 core-satellite colloids as switchable SERS tags[J].Chem Materials,2015,27 (7):2540-2545.
[2] Liu N,Gong M Z,Zhang P,et al.Silver-embedded zeolite crystals as substrates for surface-enhanced Raman scattering[J].Journal of Materials Science,2011,46:3162-3168.
[3] 汤俊琪,田超,曾崇毅,等.碱性银胶的表面增强拉曼效应及对牛奶中三聚氰胺的检测[J].光谱学与光谱分析,2013,33 (3):709-713.
[4] 李晓坤,张友林,孔祥贵.Ag纳米粒子聚集体的SiO包覆及其SERS效应[J].发光学报,2014,35 (7):853-857.
[5] 丁倩倩.Au基复合纳米催化剂的性能及其SERS原位监测催化过程的研究[D].合肥:中国科学技术大学,2016.
[6] Zhao J H,Lin J,Wei H Y,et al.Surface enhanced Raman scattering substrates based on titanium nitride nanorods[J].Optical Materials,2015,47:219-224.
[7] Lorite I,Serrano A,Schwartzberg A,et al.Surface enhanced Raman spectros-copy by titanium nitride non-continuous thin films[J].Thin Solid Films,2013,531:144-146.
[8] Chang C,Shih S G,Chen P H,et al.Effect of duty cycles on the deposition and characteristics of high power impulse magnetron sputtering deposited TiN thin films[J].Surface & Coatings Technology,2014,259:232-237.
[9] 陈颖,魏恒勇,董占亮,等.氨气还原氮化法制备TiN薄膜及其SERS效应研究[J].功能材料,2016,47 (2):2197-2200.
[10] 薛向欣,张晶,赵翠梅,等.贵金属/半导体复合SERS基底的研究进展[J].吉林师范大学学报 (自然科学版),2017,38 (2):97-100.
[11] Scherger J D,Evans E A,Dura J A,et al.Extending nanoscale spectroscopy with titanium nitride probes[J].Journal of Raman Spectroscopy,2016,47 (11):1332-1336.
[12] Ban R,Yu Y,Zhang M,et al.Synergetic SERS enhancement in metal-like/metal double shell structure for sensitive and stable application[J].ACS Appl Mater Interfaces,2017,9 (15):13564.
[13] 蒋思文,李霞,张月皎,等.不同粒径、超均匀球形金纳米粒子合成及其表面增强拉曼散射效应研究[J].光谱学与光谱分析,2016,36 (1):99-103.
[14] 陈雷,薛向欣,刘洋,等.二氧化硅—金核壳材料的制备与SERS研究[J].吉林师范大学学报 (自然科学版),2015,36 (4):29-33.
[15] Cheng C W,Yan B,Wong S M,et al.Fabrication and SERS performance of silver-nanoparticle-decorated Si/ZnO nanotrees in ordered arrays[J].ACS Applied Materials & Interfaces,2010,2:1824-1828.
[16] 季兴宏,浦绍瑞,付双钦,等.Ag/双晶TiO2作为表面增强拉曼散射基底的性能研究[J].涂料工业,2014,44 (3):14-18.
[17] 李君,程秀兰,吕朋雨,等.基于负载金纳米颗粒的TiO2纳米线的SERS基底[J].功能材料与器件学报,2014,20 (1):1-6.
基金资助
国家自然科学基金(51272066)
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