Ultra-stable silver-tantalum composite material surface-enhanced Raman scattering substrate and preparation method

A surface-enhanced Raman, composite material technology, applied in metal material coating process, sputtering coating, vacuum evaporation coating and other directions, can solve the limitation of adsorption, separation, catalysis, sensing, inconvenient mass preparation, preparation process complex problems, to achieve the effects of good chemical stability, good surface plasma performance, and simple operation

Active Publication Date: 2019-10-11
XI AN JIAOTONG UNIV
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Problems solved by technology

(Gao C, HuY, Wang M, et al.Fully alloyed Ag / Au nanospheres:combining the plasmonic property of Ag with the stability of Au.[J].Journal of the American Chemical Society,2014,136(20):7474-9 .) (Song Z L, Chen Z, Bian X, et al.Alkyne-Functionalized Superstable Graphic Silver Nanoparticles for Raman Imaging[J].Journal of the American Chemical Society,2014,136(39):13558.) Most of these methods prepare The process is complicated, it is not convenient to prepare in large quantities, and the cost is high. In addition, the surface of the silver material prepared by these methods is covered with a large number of organic compounds, which seriously limits the application of adsorption, separation, catalysis, sensing, etc.

Method used

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  • Ultra-stable silver-tantalum composite material surface-enhanced Raman scattering substrate and preparation method
  • Ultra-stable silver-tantalum composite material surface-enhanced Raman scattering substrate and preparation method
  • Ultra-stable silver-tantalum composite material surface-enhanced Raman scattering substrate and preparation method

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preparation example Construction

[0039] The invention provides a method for preparing a silver-tantalum composite SERS substrate material, comprising the following steps:

[0040] 1) Single crystal silicon wafer is selected as the substrate, and the single crystal silicon wafer substrate is selected from Si(100), Si(111), SiO 2 sheet or quartz glass. And perform pretreatment before coating; specifically, use deionized water, absolute ethanol, and acetone to ultrasonically clean the surface of the single crystal silicon wafer for 10-20 minutes.

[0041] 2) Put the cleaned single crystal silicon substrate into the magnetron sputtering coating equipment to prepare the chromium primer layer, specifically using Ar gas or nitrogen as the sputtering atmosphere, under the condition of applying a voltage of 60V to the substrate, using Magnetron sputtering is performed on the chromium target by radio frequency, and the radio frequency frequency is controlled at 250kHz; a layer of chromium film with a thickness of 100-...

Embodiment 1

[0047] 1) Cleaning: immerse the Si(100) substrate in ethanol and acetone solution for 10 minutes, take it out and soak it in deionized water for 10 minutes, then take it out, dry it with high-purity nitrogen, and then quickly put it into the magnetron sputtering coating equipment .

[0048] 2) Chromium primer preparation: prepare a chromium primer on the surface of the cleaned Si(100) substrate, use Ar gas as the sputtering atmosphere, apply a voltage of 60V, and use radio frequency to perform magnetron sputtering on the chromium target with a radio frequency of 250kHz; The thickness of the chromium film is 100nm.

[0049] 3) Silver and tantalum deposition: After the preparation of the chromium base layer, co-sputtering of silver and tantalum elements is carried out, in which the applied voltage is 60V, the current of the silver target is 5A, the current of the tantalum target is 2A, and the deposition time is 30min. The thickness of silver and tantalum composite film deposit...

Embodiment 2

[0061] 1) Cleaning: immerse the Si(111) substrate in ethanol and acetone solution for 10 minutes, take it out and soak it in deionized water for 15 minutes, then take it out, dry it with high-purity nitrogen, and then quickly put it into the magnetron sputtering coating equipment .

[0062] 2) Chromium primer preparation: prepare chromium primer on the clean single crystal silicon surface, use nitrogen as the sputtering atmosphere, apply 60V voltage, and use radio frequency to perform magnetron sputtering on the chromium target with a radio frequency frequency of 250kHz; the thickness of the chromium film 500nm.

[0063] 3) Silver and tantalum deposition: After the preparation of the chromium base layer, co-sputtering of silver and tantalum elements is carried out, in which the applied voltage is 60V, the current of the silver target is 5A, the current of the tantalum target is 5A, and the deposition time is 15min. The thickness of silver and tantalum composite film deposited...

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Abstract

The invention provides a superstable silver-tantalum composite surface-reinforced Raman scattering substrate and a preparation method thereof. According to the invention, a silver-tantalum composite film is deposited through magnetron sputtering; a cleaned single-crystal silicon wafer is vacuumized and deposited with a chromium film; the intensity of current is controlled; the deposition rates ofsilver and tantalum elements are respectively and accurately adjusted and controlled; the reaction pressure of a chamber is maintained; the silver and tantalum elements are deposited through continuous sputtering to form a bimetallic composite material; thus, corrosion resistance and stability of silver are effectively improved; and superstable surface-reinforced Raman scattering detection is realized. The silver-tantalum composite substrate provided by the invention is prepared through magnetron sputtering under a vacuum condition and has pollution-free and high-cleanliness surface, so sensitivity and accuracy of surface-reinforced Raman scattering detection are effectively improved. The superstable silver-tantalum composite surface-reinforced Raman scattering substrate provided by the invention has the advantages of simple preparation process, large specific surface area, low cost, convenient industrial production, and capability of being extensively applied to the fields of surface-reinforced Raman scattering sensing, metal catalysis, nanometer probes, photoelectric devices, solar cells, adsorption materials, etc.

Description

technical field [0001] The invention relates to the technical field of advanced nano-composite materials, in particular to an ultra-stable silver-tantalum composite surface-enhanced Raman scattering substrate and a preparation method. Background technique [0002] Noble metal nanomaterials, especially silver nanomaterials, have large optical cross-sections, excellent surface plasmon resonance properties, and lower cost, so they are very excellent SERS substrate materials and have been widely used in the field of SERS detection. . However, the stability of silver nanomaterials is poor, and they are easily corroded, oxidized or sulfurized, which reduces the plasma signal and limits the application of silver nanomaterials in SERS detection. At present, researchers use methods such as chemical liquid phase synthesis to prepare gold-silver alloy materials or coat graphene and oxide shells on the surface of nano-silver to improve the corrosion resistance of silver. (Gao C, HuY, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C23C14/35C23C14/16C22C5/06C22C27/06C22C27/02
Inventor 宋忠孝陈东圳赵永席黄剑井津域李莎
Owner XI AN JIAOTONG UNIV
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