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Preparation method of self-assembled sulfonic acid group silane-titanium dioxide composite film on monocrystalline silicon substrate surface

A technology of sulfonic acid silane and titanium dioxide, which is applied in the field of thin film preparation, can solve the problems of long film forming cycle and achieve the effects of low cost, simple configuration and uniform distribution

Inactive Publication Date: 2009-10-14
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method requires 24-96 hours to prepare the precursor solution in the process of preparing the self-assembled film, which makes the entire film-forming cycle too long, and does not involve specific methods in the process of substrate processing, and this method is Prepared an organic self-assembled thin film, which did not involve the improvement and research of titanium dioxide element on the performance of the thin film

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Pre-treat the monocrystalline silicon wafer, soak the monocrystalline silicon wafer in aqua regia, heat the aqua regia with an electric furnace for 5 hours, and naturally cool it at room temperature for 8 hours, take out the monocrystalline silicon wafer, and use a deionized Rinse repeatedly with water and dry in a desiccator;

[0020] Immerse the treated monocrystalline silicon wafer in the prepared mercaptosilane solution, let it stand for 8 hours, take it out, wash it with acetone, chloroform and deionized water respectively, dry it with nitrogen, place it in nitric acid solution, and set it at 80 React at ℃ for 2 hours, take it out and wash it with a large amount of deionized water, and oxidize the terminal sulfhydryl group into a sulfonic acid group in situ.

[0021] The substrate with the sulfonic acid silane film on the surface is placed in the prepared titanium dioxide self-assembly solution, and assembled at 80°C for 12 hours to obtain the sulfonic acid silane-...

Embodiment 2

[0028] Embodiment 2: the preparation process of this embodiment is the same as embodiment 1.

[0029] The molar concentration of the components of the mercaptosilane assembly solution used in this embodiment is: 0.3 mmol / L of mercaptosilane, and the solvent is benzene solution.

[0030] The concentration of the nitric acid solution for in-situ oxidation of sulfhydryl groups to sulfonic acid groups is: 40%.

[0031] The component weight percent of titania self-assembly solution is:

[0032] Ethanol content: 83%, titanate: 3.5%, ethylenediaminetetraacetic acid: 1%, ammonium chloride: 2%, urea: 10%, concentrated hydrochloric acid: 0.5%.

[0033] The characterization means in Example 1 were used to evaluate the film quality.

[0034] The results show that the thickness of the organic film self-assembled on the single crystal silicon wafer is between 5-8nm, and the film thickness of the composite film is between 15-40nm. The XPS spectrum shows that the composite film self-assemb...

Embodiment 3

[0035] Embodiment 3: the preparation process of this embodiment is the same as embodiment 1.

[0036] The molar concentration of the components of the mercaptosilane assembly solution used in this embodiment is: 1 mmol / L of mercaptosilane, and the solvent is benzene solution.

[0037] The concentration of the nitric acid solution for in-situ oxidation of sulfhydryl groups to sulfonic acid groups is: 60%.

[0038] The component weight percent of titania self-assembly solution is:

[0039] Ethanol content: 70%, titanate: 5%, ethylenediaminetetraacetic acid: 4%, ammonium chloride: 5%, urea: 15%, concentrated hydrochloric acid: 1%.

[0040] Adopt the experimental instrument in embodiment 1 to evaluate thin film, the result of characterization shows: the result shows that the organic thin film film thickness that self-assembles on single crystal silicon chip is between 5~7nm, and the film thickness of composite film is between 15~50nm between. The XPS pattern shows that the merc...

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Abstract

The invention relates to a preparation method of self-assembled sulfonic acid group silane-titanium dioxide composite film on monocrystalline silicon substrate surface. The invention is characterized in that the monocrystalline silicon piece is treated in advance and is immersed in prepared hydrosulphonyl silane solution, after holding for 8 hours, the monocrystalline silicon piece is taken out and washed by acetone, chloroform and deionized water, and the nitrogen is used for drying the monocrystalline silicon piece, after being dried, the monocrystalline silicon piece is put into the nitric acid with finite concentration for 2 hours under 80 DEG C, and then the sulfonic acid group silane-titanium dioxide self-assembled nano film is obtained. The preparation method has the advantages of simple process, low cost and no environment pollution and the obtained titanium dioxide nano film is well-distributed and compactly with evident antifriction effect. Furthermore the titanium dioxide self-assembled nano film has the advantage of good abrasion resistance property.

Description

technical field [0001] The invention relates to a method for preparing an organic and inorganic nanocomposite film, in particular to a method for preparing a sulfonic acid silane-titanium dioxide self-assembled nanometer film on the surface of a single crystal silicon substrate. It belongs to the field of film preparation. Background technique [0002] With the advancement of high technology, the machinery manufacturing industry is developing in the direction of miniaturization, which involves the tribological problems of the surface of micro-machines. Due to the advantages of high hardness, low cost and small surface roughness of silicon material, the application in MEMS has been paid more and more attention. However, silicon materials without surface treatment are highly brittle, and surface cracks are prone to delamination wear and brittle fracture under low tensile stress, which is difficult to meet the requirements of use. Therefore, surface modification technology is ...

Claims

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Application Information

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IPC IPC(8): C30B33/00C30B29/06
Inventor 李健
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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