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Preparation method of recyclable surface-enhanced Raman-spectrum active substrate

A surface-enhanced Raman and active substrate technology, applied in the field of laser Raman spectroscopy detection appliances, can solve the problems of reduced practical availability and increased cost, and achieve the effect of high Raman enhancement effect

Inactive Publication Date: 2013-04-17
JIANGSU UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, the surface-enhanced Raman scattering effect occurs under special experimental conditions, and has special requirements on the type of substrate and surface morphology. At this stage, there are only three noble metals, gold, silver, and copper, and a few rare alkalis. Metals (such as lithium and sodium) have a strong surface-enhanced Raman scattering effect, and the use of these noble metals directly increases the cost of surface-enhanced Raman scattering detection, and these expensive surface-enhanced Raman scattering active substrates still exist once Therefore, it is imperative to develop recyclable or reusable surface-enhanced Raman scattering substrate materials, Mathias Brust (P. Aldeanueva-Potel, et al. Anal. Chem., 2009, 81, 9233.) prepared Ag-loaded agarose gel, because the surface of Ag nanoparticles is coated with polymer gel, which isolates the direct contact between Ag and adsorbed molecules, and the molecules adsorbed on the gel surface can pass through Solvent washing to realize the recycling of the substrate; some scholars such as Yao Jianlin (Guo Qinghua, et al. Acta Chemica Sinica, 2011, 69, 1060. B. Lv, et al. J. Solid State Chem., 2010, 183, 2968. J . Du, et al. J. Colloid Interf. Sci., 2011, 358, 54.) Construct Ag or Au nanoparticles and magnetic substances into a composite substrate, and recycle and recycle the composite nanostructure by enriching it with an external magnetic field use; or Au nanoparticles coated with a layer of dense SiO 2 shell, which isolates the direct contact between Au and adsorbed molecules, and obtains a kind of AuSiO 2 Recyclable surface-enhanced Raman scattering substrates with core-shell structures (D. Li, et al. J. Mater. Chem., 2010, 20, 3688.); however, in the preparation of these substrates, cladding thickness control is critical (Too thick will reduce the surface-enhanced Raman scattering effect of Au or Ag, and too thin will cause direct contact with adsorbed molecules). In addition, these substrates may also have problems such as unclean ultrasonic cleaning and pinholes in the cladding layer.

Method used

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  • Preparation method of recyclable surface-enhanced Raman-spectrum active substrate
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  • Preparation method of recyclable surface-enhanced Raman-spectrum active substrate

Examples

Experimental program
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Effect test

Embodiment 1

[0022] Add 17.08mL of tetrabutyl titanate, 69mL of absolute ethanol, and 2.9mL of glacial acetic acid into a three-necked flask in sequence, and add 0.5mL of acetylacetone, stir magnetically at room temperature for 1 hour, and slowly drop in 11mL of 90.9 % ethanol solution (volume ratio of ethanol / water is 10:1), to obtain light yellow transparent TiO with 0.5mol / L titanium concentration 2 sol, and then 2.01 g of polyethylene glycol 2000 was added to the above sol, stirred and refluxed at 80° C. for 1 hour to obtain a polyethylene glycol-modified TiO2 sol, which was set aside.

[0023] The carrier substrate selected in this example is a quartz glass sheet. The quartz sheet is cleaned with hydrogen peroxide / sulfuric acid mixture (volume ratio 1:4), ethanol, and deionized water, and dried in vacuum at 100°C for 2 hours. figure 1 Schematic diagram of the preparation, immerse the cleaned quartz glass substrate in TiO 2 Sol for 10 minutes, use the pulling method to slowly pull out...

Embodiment 2

[0027] In this example, the surface-enhanced Raman scattering substrate prepared in Example 1 was selected and placed in a 1×10 -5 mol / L of methylene blue aqueous solution soaked for 1 hour, dried naturally, and measured its surface-enhanced Raman spectrum, and the test results were as follows: Figure 4 shown; Figure 4 Show 10 in -5 The Raman signal of mol / L methylene blue on the prepared surface-enhanced Raman scattering substrate is very obvious, and the Raman signal of methylene blue disappears after being irradiated with 12W, 254nm ultraviolet light for 30 minutes. Then soak the substrate in 10 -5 mol / L of methylene blue solution, the surface enhanced Raman signal reproduced, so repeated 5 times, Figure 4 It shows that the surface-enhanced Raman signal has no obvious attenuation. Experimental results show that the number of effective cycles can reach 20 + .

Embodiment 3

[0029]In this example, the surface-enhanced Raman scattering substrate prepared in Example 1 is selected, and first placed in a 1×10 -5 mol / L methylene blue aqueous solution for several times, and its surface-enhanced Raman spectrum was measured. After irradiating with 12 W, 254nm UV lamp for 30 minutes, soak in 1×10 -5 mol / L rose bengal aqueous solution, and then measure its surface-enhanced Raman spectrum. Finally, after irradiating with 12W, 254nm ultraviolet lamp for 30 minutes, soak in 1×10 -5 mol / L crystal violet aqueous solution, measure its surface-enhanced Raman spectrum, the test results are as follows Figure 5 shown; Figure 5 It shows that the Raman signal of methylene blue disappears after being irradiated by a 12W, 254nm UV lamp for 30 minutes, and the substrate is soaked in 10 -5 mol / L rose bengal solution, measured rose bengal high quality surface enhanced Raman signal. The rose red Raman signal disappeared after being irradiated by ultraviolet light ...

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Abstract

The invention belongs to the technical field of laser-Raman spectrum detection appliances and Raman spectrum analysis and detection, and in particular relates to a recyclable surface-enhanced Raman-spectrum active substrate with low cost and good reproducibility, and a preparation method thereof. The substrate is characterized in that a porous titanium dioxide film is loaded on the surface of a carrier base sheet through a dipping and lifting method, and then gold nanoparticles grow on the surface of the titanium dioxide film. The composite substrate has an outstanding surface enhanced effect; and chemical compound molecules absorbed on the surface of gold in a previous Raman experiment can be effectively removed through ultraviolet irradiation, and thus the substrate can be recycled.

Description

technical field [0001] The invention belongs to the technical field of laser Raman spectrum detection equipment and Raman spectrum analysis and detection, and particularly relates to a recyclable, low-cost, and good-reproducibility surface-enhanced Raman spectrum active substrate and a preparation method thereof. Background technique [0002] Surface-enhanced Raman scattering (SERS) is an abnormal surface optical phenomenon, which means that when a compound is adsorbed or close to the surface of some special noble metals, its Raman scattering cross-section is enhanced by about 4 to 10 orders of magnitude, making laser Raman spectroscopy analysis The signal-to-noise ratio has been greatly improved, and the detection accuracy has taken a leap. In some specific systems, the detection sensitivity at the single-molecule level can even be achieved. Due to its extremely high detection sensitivity, surface-enhanced Raman scattering technology has been used in surface chemistry, a...

Claims

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Application Information

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IPC IPC(8): G01N21/65
Inventor 傅小奇王双殷恒波姜廷顺
Owner JIANGSU UNIV
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