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Preparation method of SERS (Surface Enhanced Raman Scattering) substrate with wettability multistage nano array structure

A nano-array and nano-structure technology, which is applied in the field of preparation of wettable multi-level nano-array structure SERS substrate, can solve the problems of poor repeatability measurement of SERS substrate signal and insufficient structure uniformity, so as to improve detection sensitivity and Enhancement Factors, High Sensitivity and Uniformity, Effect of Enhanced Degree of Control

Pending Publication Date: 2022-08-05
GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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Problems solved by technology

Patent CN 109358032 A sputters Au films on nanoscale flat insulators, semiconductors, and conductors as electrodes, and prepares leaf-shaped and needle-shaped Au nanostructures by electrodeposition. Although this structure has a large number of active hot spots, the structure The uniformity is not good enough, which may eventually lead to poor repeatability measurement of the SERS substrate signal, and the repeatability of the SERS signal is also the main problem to be solved urgently

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  • Preparation method of SERS (Surface Enhanced Raman Scattering) substrate with wettability multistage nano array structure
  • Preparation method of SERS (Surface Enhanced Raman Scattering) substrate with wettability multistage nano array structure
  • Preparation method of SERS (Surface Enhanced Raman Scattering) substrate with wettability multistage nano array structure

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preparation example Construction

[0047] A preparation method of a wettable multi-level nano-array structure SERS substrate, such as figure 1 As shown, the method includes the following steps:

[0048] 1) Polish the silicon wafer containing the silicon oxide layer, clean it, and then use the gas-liquid interface self-assembly method to deposit a single-layer polystyrene (PS) ball in a hexagonal close arrangement on the surface of the silicon oxide as a subsequent etching mask ; Using low-temperature inductively coupled plasma-enhanced reactive ion etching (ICP-RIE) or plasma degumming technology to etch the obtained hexagonal close-arranged monolayer PS film, and each sphere is uniformly reduced to a specific size, to obtain a PS nanosphere mask layer with equal spacing and non-close arrangement;

[0049] 2) Reactive ion etching (RIE) technology is used to etch silicon oxide with polystyrene nanospheres as a mask to form a large-area ordered polystyrene-silicon oxide column array structure;

[0050] 3) conti...

Embodiment 1

[0054] 1) Use a 4-inch single-sided polished silicon wafer with a 300nm silicon oxide layer as the substrate, and configure concentrated H 2 SO 4 :H 2 O 2 Mix the cleaning solution, immerse the silicon wafer substrate in it, boil it at 120°C for 2 hours, remove oil stains and other contaminants on the surface of the silicon wafer, rinse with ultrapure water and rinse with N 2 Blow dry spare;

[0055] The cleaned wafers were placed in the apparatus mentioned in the work already reported by our group (doi: 10.1109 / NEMS51815.2021.9451289), deionized water was added to completely submerge the wafer, and 6 mL of 20 mM The SDS solution was allowed to stand for 10 min, and then 550 μL of PS suspension with a diameter of 300 nm (volume ratio, alcohol: PS=3:2) was added to the above solution very slowly along the slide with a micro-syringe, and allowed to stand for 1 h. The PS monolayer film on the gas-liquid interface was transferred to the silicon oxide wafer, and the spherical d...

Embodiment 2

[0064] The preparation method of the wettable multi-level nano-array structure SERS substrate of Example 2 is the same as that of Example 1, except that the thickness of silicon oxide selected in step 1) of Example 1 is 100 nm, and the silicon oxide in step 2) is etched The reactive gas used in the etching is CF 4 , the gas flow rate is 40sccm, the reaction pressure is 1Pa, the etching power is 300W, the etching time is 180s, and the silicon oxide etching depth is 100nm; the reaction gas used in the silicon etching in step 3) is SF 6 and O 2 , the gas flow is 60sccm and 10sccm, the reaction pressure is 5Pa, the etching power is 300W, the etching time is 420s, and the silicon etching depth is 600nm; in step 4), a chemical coupling method is used to load a Layers of gold nanoparticles.

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Abstract

The invention discloses a preparation method of an SERS (Surface Enhanced Raman Scattering) substrate with a wettability multistage nano array structure, belonging to the cross technical field of micro-nano processing, surface interface regulation and control and electrochemical synthesis. The preparation method comprises the following steps: firstly, obtaining a regular and non-close-packed PS (Polystyrene) pellet mask on a silicon oxide wafer by adopting a gas-liquid interface self-assembly method in combination with a reactive ion etching process; etching the silicon oxide and the silicon in sequence to obtain a large-area silicon column structure; the surface of the obtained silicon column structure is coated with a metal film, and the substrate is soaked in a sulfydryl-containing molecular solution for hydrophobicity regulation and control; and finally, preparing a pine-branch-shaped Au nano array structure on the hydrophobic silicon substrate by adopting an electrochemical deposition technology, so as to obtain the SERS substrate which is flexible and adjustable in nano array structure gap, large in area, low in cost, high in repeatability, rich in active heat and high in sensitivity.

Description

technical field [0001] The invention belongs to the interdisciplinary technical fields of micro-nano processing, surface-interface regulation and electrochemical synthesis, and in particular relates to a preparation method of a wettable multilevel nano-array structure SERS substrate. Background technique [0002] The surface-enhanced Raman scattering effect (SERS) was discovered in the mid-1970s. This effect makes the Raman signal of molecules adsorbed on the metal surface with SERS activity be as high as that of the Raman signal of the same number of molecules in solution. 10 6 The huge enhancement of multiple times leads to the extremely high detection sensitivity and selectivity of SERS technology for surface species, which can realize the capture of "fingerprint" information of various substances on the interface at the molecular level. SERS has been widely used in labeling and wireless Research fields such as label detection, materials science, biochemistry, biomedicin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B81C1/00C23C14/16C23C14/24C23C14/35
CPCC23C14/16C23C14/165C23C14/24C23C14/35B81C1/00111B81C1/00523B81C2201/013
Inventor 明安杰陈凡红赵永敏赵玉鹏毛昌辉
Owner GENERAL RESEARCH INSTITUTE FOR NONFERROUS METALS BEIJNG
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