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Single-step rapid preparation method of porous silicon-gold dendritic crystal composite structure

A composite structure and porous silicon technology, applied in nanotechnology, nanotechnology, instruments, etc. for sensing, can solve problems such as high environmental requirements, complicated operation, and long preparation time, and achieve simple steps, more steps to solve, The effect of efficient preparation

Pending Publication Date: 2020-11-20
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, regardless of the soaking method or the thermal decomposition method, there are disadvantages such as long preparation time, many steps, high environmental requirements, and complicated operations when preparing porous silicon composite metal nanostructures.

Method used

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  • Single-step rapid preparation method of porous silicon-gold dendritic crystal composite structure
  • Single-step rapid preparation method of porous silicon-gold dendritic crystal composite structure
  • Single-step rapid preparation method of porous silicon-gold dendritic crystal composite structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A single-step rapid preparation method for a porous silicon-gold dendrite composite structure, comprising the following steps:

[0032] (1) Pretreatment: select a P-type silicon chip, preferably, the silicon chip is a [100] crystal orientation P-type single crystal silicon, the resistivity is 10-20Ω·cm, and the thickness is 525 μm, and the silicon chip is cut with a diamond tool Divide into square silicon wafers of 1.5cm×1.5cm; place the cut square silicon wafers in a beaker filled with deionized water, alcohol, and acetone in turn and perform ultrasonic cleaning for 10 minutes to remove oil and impurities on the square silicon wafers , and then blow dry with a nitrogen gun;

[0033] (2) Preparation of electrochemical corrosion solution: use suction pipe to take out 16mL of HF (48wt%), 9mL of DMF (analytical pure AR) and 8mL of tetrachloroauric acid solution respectively on the operating table with fume hood and put into plastic measuring cylinder An electrochemical co...

Embodiment 2

[0039] The preparation steps of the porous silicon-gold dendrite composite structure are the same as in Example 1, the difference is that the concentration of tetrachloroauric acid solution is adjusted to 0.2M;

[0040] SEM characterization and SERS performance analysis of porous silicon-gold dendrite composite structure:

[0041] image 3 It is the SEM image of the porous silicon-gold dendrite composite structure prepared in Example 2, showing the structure under this corrosion condition, and it can be seen that a large number of gold nanodendrites are attached to the porous silicon.

[0042] Figure 4 It is the Raman spectrogram of porous silicon-gold dendrite composite structure and pure porous silicon, and the concentration of R6G is 10 in embodiment 2 -6 M, at 614cm -1 , 764cm -1 , 1360cm -1 , 1502cm -1 and 1643cm -1 It can be clearly seen that the spectral characteristic peaks of R6G and their peaks have been greatly enhanced, and the SERS intensity has been great...

Embodiment 3

[0044]The preparation steps of the porous silicon-gold dendrite composite structure are the same as in Example 1, the difference being that the concentration of tetrachloroauric acid solution is adjusted to 0.5M;

[0045] Porous silicon-gold dendrite composite structure SEM characterization and SERS performance analysis:

[0046] Through the SEM morphology test of the experimental samples; Figure 5 It is the SEM picture of the porous silicon-gold dendrite composite structure prepared in Example 3, showing the structure under this corrosion condition. It can be seen that denser gold nanodendrites are attached to the porous silicon.

[0047] Figure 6 is the Raman spectrum of porous silicon-gold dendrite composite structure and pure porous silicon, the concentration of R6G in this experiment is 10 -6 M, at 614cm -1 , 764cm -1 , 1360cm -1 , 1502cm -1 and 1643cm -1 It can be clearly seen that the spectral characteristic peak of R6G and its peak intensity have decreased com...

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Abstract

The invention belongs to the technical field of electrochemical corrosion and silicon microstructure preparation, which relates to a rapid preparation method of a porous silicon-gold dendritic crystalcomposite structure. The method comprises the following specific steps of firstly, selecting a silicon wafer, and cutting and cleaning the silicon wafer to obtain a pretreated silicon wafer, then mixing hydrofluoric acid, dimethylformamide and a tetrachloroauric acid solution to obtain an electrochemical corrosive liquid, immersing the pretreated silicon wafer, applying a constant current, and performing electrochemical corrosion to obtain a porous silicon-gold dendritic crystal composite structure through one-step treatment, and finally, cleaning the prepared porous silicon-gold dendritic crystal composite structure to obtain a final composite structure. According to the preparation method disclosed by the invention, the single-step rapid preparation of the porous silicon-gold nano composite structure is realized by preparing the electrochemical corrosive liquid and immersing the silicon wafer, and the SERS performance of the composite structure is regulated and controlled by changing the concentration of the tetrachloroauric acid solution; the method is simple in step, convenient to operate and short in consumed time, and the porous silicon-gold dendritic crystal composite structure can be rapidly and efficiently prepared.

Description

technical field [0001] The invention belongs to the technical field of electrochemical corrosion and silicon microstructure preparation, and in particular relates to a rapid preparation method of a porous silicon-gold dendrite composite structure. Background technique [0002] Since 1974, Fleischmann observed the high-intensity Raman scattering signal of pyridine molecules on the rough silver electrode surface in the experiment, but it was not until 2003 that the metal nanoparticle structure attached to the porous silicon substrate appeared for the first time, proving that the porous silicon-metal as Possibility of surface-enhanced Raman scattering (SERS) substrates. In 2004, Haohao Lin et al. used the immersion method to synthesize silver nanodendrites on the surface of porous silicon, and used rhodamine R6G probe molecules to detect the SERS performance of the substrate. In recent years, with the continuous development of technology, the research on the nanostructure of p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/65C25F3/12B82Y40/00B82Y15/00
CPCG01N21/658C25F3/12B82Y15/00B82Y40/00
Inventor 葛道晗张远丁杰张立强
Owner JIANGSU UNIV
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