新穎多孔復合SERS基底的制備及性能的研究
發(fā)布時間：2018-11-06 07:50
【摘要】：具有廣闊應用前景的表面增強拉曼散射(SERS)以其較高的靈敏度和較好的分辨率在光譜材料等領域引起了熱切的關注。眾所周知,SERS技術的持續(xù)發(fā)展主要依賴于新型SERS活性基底的研究和制備。只有新穎多功能的SERS基底發(fā)展起來,才能完美地解決活性SERS基底匱乏的難題,達到增加拉曼光譜應用性的目的。構建均一、有效的SERS基底仍然具有挑戰(zhàn)性,因為這一般都需要高成本的消耗和復雜的合成過程。為了解決上述問題,本文首先采用溶劑熱法制備了多孔花狀的羥基磷灰石/Ag復合物作為基底,討論了SERS增強性能和催化還原對硝基苯酚的能力。另外我們還通過溶膠凝膠法制備了多孔有序的Ni摻雜的TiO2反蛋白石光子晶體和Co離子摻雜的GO-TiO2反蛋白石光子晶體,主要討論了其SERS性能及光電轉化、光催化性能。論文主要研究結果如下：1.通過溶劑熱一鍋法制備了多孔的HA/Ag納米復合物,并利用XRD、SEM、 BET、Raman等技術對產(chǎn)物進行表征。結果表明,大小相對均勻的Ag納米顆粒附著在多孔花狀的HA表面上,多孔HA/Ag納米復合物可以用作表面增強拉曼光譜(SERS)基底,對羅丹明6G(Rh6G)的拉曼光譜有很好的增強作用,檢測Rh6G極限達到10-10。另外,上述產(chǎn)物能夠8 min內催化還原對硝基苯酚(4-NP)。本實驗簡單、方便的合成方法也為制備其他多功能的復合材料提供了借鑒。2.以我們以均勻大小的PS球為模板,制備出了有序多孔的反蛋白石結構的Ni摻雜的TiO2光子晶體,并將其有效的運用于活性SERS基底。結果表明,摻雜的Ni離子能進入TiO2的晶格,在納米TiO2的帶隙中形成豐富的摻雜能級,顯著提高了反蛋白石結構TiO2的SERS性能。所以該基底的拉曼光譜對4-巰基苯甲酸(4-MBA)具有有很好的檢測效果,檢測極限達到10-11。另外,在模擬太陽光照射下,90min對亞甲基藍(MB)的光催化降解率可達95%。因此,該反蛋白石薄膜有望在污水的檢測、環(huán)境清潔等方面得到應用。3.在前期研究的基礎上,通過多步法合成多孔有序的反蛋白石結構的Co離子摻雜的GO-TiO2光子晶體,并將其作為表面增強拉曼散射(SERS)的活性基底。研究了Co的摻雜和GO的存在對于所制備的光子晶體SERS基底性能的改進。結果表明,適量的Co摻雜能夠在反蛋白石TiO2的能隙中靠近導帶的位置形成摻雜能級,促進電荷轉移的過程；適量GO的加入也能起到增強Raman的作用,進而顯著地提高了GO復合Co-TiO2基底對4-巰基苯甲酸(4-MBA)拉曼光譜的增強能力,進而提高了SERS性能,檢測4-MBA極限達到10-12。另外,該反蛋白石薄膜在模擬太陽光的照射下光催化MB降解的效率和光電流密度是普通的反蛋白石TiO2薄膜1.5倍和6倍。
[Abstract]:Surface enhanced Raman scattering (SERS), which has wide application prospects, has attracted much attention in the field of spectral materials due to its high sensitivity and good resolution. As we all know, the sustainable development of SERS technology mainly depends on the research and preparation of new active substrates of SERS. Only when novel multifunctional SERS substrates are developed can the problem of lacking active SERS substrates be solved perfectly and the application of Raman spectra be increased. Building a uniform and effective SERS substrate remains challenging because it typically requires high cost and complex composition processes. In order to solve the above problems, the porous flower-like hydroxyapatite / Ag composites were prepared by solvothermal method. The enhancement of SERS and the ability of catalytic reduction of p-nitrophenol were discussed. In addition, porous ordered TiO2 opal photonic crystals doped with Ni and GO-TiO2 opal photonic crystals doped with Co ion were prepared by sol-gel method. The properties of SERS, photoconversion and photocatalysis were discussed. The main research results are as follows: 1. Porous HA/Ag nanocomposites were prepared by solvothermal one-pot method and characterized by XRD,SEM, BET,Raman. The results showed that the Ag nanoparticles with relatively uniform size were attached to the porous HA surface, and the porous HA/Ag nanocomposites could be used as (SERS) substrates for enhanced Raman spectra. The Raman spectra of Rhodamine 6G (Rh6G) were enhanced and the detection limit of Rh6G was 10-10. In addition, the above products can catalyze the reduction of p-nitrophenol (4-NP) in 8 min. This experiment is simple and convenient for the preparation of other multifunctional composite materials. 2. An ordered porous Ni doped TiO2 photonic crystal was prepared by using a uniform size PS sphere as a template and was effectively applied to the active SERS substrate. The results show that the doped Ni ions can enter the lattice of TiO2 and form rich doped energy levels in the band gap of TiO2 nanocrystalline, which improves the SERS performance of TiO2 with inverse opal structure. Therefore, the Raman spectrum of the substrate has a good effect on the detection of 4-mercaptobenzoic acid (4-MBA), and the detection limit is up to 10-11. In addition, under simulated solar irradiation, the photocatalytic degradation rate of methylene blue (MB) by 90min was up to 95. Therefore, the reverse opal film is expected to be used in the detection of sewage, environmental cleanliness and other aspects. On the basis of previous studies, GO-TiO2 photonic crystals doped with Co ions with porous and ordered antiopal structure were synthesized by multistep method and used as active substrates for surface-enhanced Raman scattering (SERS). The improvement of the properties of the photonic crystal SERS substrate prepared by doping Co and the existence of GO has been studied. The results show that the doping level can be formed near the conduction band in the energy gap of opal TiO2 by proper amount of Co doping, which can promote the process of charge transfer. The addition of appropriate amount of GO can also enhance the Raman, thus significantly improving the enhancement of the Raman spectra of 4-mercaptobenzoic acid (4-MBA) on the GO composite Co-TiO2 substrate, and further improving the SERS performance. The detection limit of 4-MBA is 10-12. In addition, the photocatalytic MB degradation efficiency and photocurrent density of this opal film are 1.5 and 6 times higher than those of conventional opal TiO2 films under simulated solar irradiation.
【學位授予單位】：安徽大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：O657.37;TB33
本文編號：2313623
[Abstract]:Surface enhanced Raman scattering (SERS), which has wide application prospects, has attracted much attention in the field of spectral materials due to its high sensitivity and good resolution. As we all know, the sustainable development of SERS technology mainly depends on the research and preparation of new active substrates of SERS. Only when novel multifunctional SERS substrates are developed can the problem of lacking active SERS substrates be solved perfectly and the application of Raman spectra be increased. Building a uniform and effective SERS substrate remains challenging because it typically requires high cost and complex composition processes. In order to solve the above problems, the porous flower-like hydroxyapatite / Ag composites were prepared by solvothermal method. The enhancement of SERS and the ability of catalytic reduction of p-nitrophenol were discussed. In addition, porous ordered TiO2 opal photonic crystals doped with Ni and GO-TiO2 opal photonic crystals doped with Co ion were prepared by sol-gel method. The properties of SERS, photoconversion and photocatalysis were discussed. The main research results are as follows: 1. Porous HA/Ag nanocomposites were prepared by solvothermal one-pot method and characterized by XRD,SEM, BET,Raman. The results showed that the Ag nanoparticles with relatively uniform size were attached to the porous HA surface, and the porous HA/Ag nanocomposites could be used as (SERS) substrates for enhanced Raman spectra. The Raman spectra of Rhodamine 6G (Rh6G) were enhanced and the detection limit of Rh6G was 10-10. In addition, the above products can catalyze the reduction of p-nitrophenol (4-NP) in 8 min. This experiment is simple and convenient for the preparation of other multifunctional composite materials. 2. An ordered porous Ni doped TiO2 photonic crystal was prepared by using a uniform size PS sphere as a template and was effectively applied to the active SERS substrate. The results show that the doped Ni ions can enter the lattice of TiO2 and form rich doped energy levels in the band gap of TiO2 nanocrystalline, which improves the SERS performance of TiO2 with inverse opal structure. Therefore, the Raman spectrum of the substrate has a good effect on the detection of 4-mercaptobenzoic acid (4-MBA), and the detection limit is up to 10-11. In addition, under simulated solar irradiation, the photocatalytic degradation rate of methylene blue (MB) by 90min was up to 95. Therefore, the reverse opal film is expected to be used in the detection of sewage, environmental cleanliness and other aspects. On the basis of previous studies, GO-TiO2 photonic crystals doped with Co ions with porous and ordered antiopal structure were synthesized by multistep method and used as active substrates for surface-enhanced Raman scattering (SERS). The improvement of the properties of the photonic crystal SERS substrate prepared by doping Co and the existence of GO has been studied. The results show that the doping level can be formed near the conduction band in the energy gap of opal TiO2 by proper amount of Co doping, which can promote the process of charge transfer. The addition of appropriate amount of GO can also enhance the Raman, thus significantly improving the enhancement of the Raman spectra of 4-mercaptobenzoic acid (4-MBA) on the GO composite Co-TiO2 substrate, and further improving the SERS performance. The detection limit of 4-MBA is 10-12. In addition, the photocatalytic MB degradation efficiency and photocurrent density of this opal film are 1.5 and 6 times higher than those of conventional opal TiO2 films under simulated solar irradiation.
【學位授予單位】：安徽大學
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：O657.37;TB33
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