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Method for preparing sulfonic silane-rare earth nanometer composite film on glass substrate surface

The technology of sulfonic silane and glass substrate is applied in the field of thin film preparation, which can solve the problems of long heat treatment time and complicated process conditions for self-assembling thin films, and achieve the effects of uniform distribution, dense film formation and simple preparation.

Inactive Publication Date: 2006-02-22
SHANGHAI JIAO TONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process conditions of the self-assembled film prepared by this method are relatively cumbersome, and the heat treatment time is also long, and the film prepared by this method is an organic film, not a rare earth composite film

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] First, the glass substrate is pretreated by hydroxylation. The treatment method: the glass substrate is immersed in Pirahan solution (H 2 SO 4 :H 2 o 2 =70:30, V / V), treated at 90°C for 1 hour, then ultrasonically cleaned with a large amount of deionized water for 20 minutes, placed in a dust-proof device and dried in an oven, the treated glass substrate was immersed in mercapto After standing in the silane solution for 6 hours, the molar concentration of the components of the mercaptosilane solution is: 0.2 mmol / L of 3-mercaptopropylmethyldimethoxysilane, and the solvent is benzene solution. After taking it out, wash it with chloroform, acetone, and deionized water respectively to remove the organic molecules physically adsorbed on the surface, then dry it with nitrogen, place it in nitric acid with a weight concentration of 30%, and take it out after reacting at 80°C for 1 hour. Rinse with ion water, so that the terminal mercapto groups are oxidized into sulfonic a...

Embodiment 2

[0023] First, the hydroxylation pretreatment of the glass substrate: immerse the glass substrate in Pirahan solution, treat it at 90°C for 1 hour, then ultrasonically clean it with a large amount of deionized water for 20 minutes, put it in a dust-proof device and dry it in an oven , immerse the treated glass substrate in the prepared mercaptosilane solution and let it stand for 7 hours. The molar concentration of the components of the mercaptosilane solution is: 3-mercaptopropylmethyldimethoxysilane 1.0mmol / L, solvent It is a benzene solution; after taking it out, wash it with chloroform, acetone, and deionized water to remove the organic matter physically adsorbed on the surface, blow it dry with nitrogen, place it in nitric acid with a mass concentration of 50%, and react at 65°C for 1 hour. Take it out with a large amount of Rinse with deionized water, so that the terminal mercapto groups are oxidized into sulfonic acid groups in situ, and a glass substrate with a sulfonic ...

Embodiment 3

[0030] First, the hydroxylation pretreatment of the glass substrate: immerse the glass substrate in Pirahan solution, treat it at 90°C for 1 hour, then ultrasonically clean it with a large amount of deionized water for 20 minutes, put it in a dust-proof device and dry it in an oven , immerse the treated glass substrate in the prepared mercaptosilane, let it stand for 8 hours, the molar concentration of the components of the mercaptosilane solution is: 2.0mmol / L of 3-mercaptopropyltrimethoxysilane, and the solvent is benzene solution; After taking it out, wash it with chloroform, acetone, and deionized water respectively, blow it dry with nitrogen, place it in nitric acid with a mass concentration of 60%, and react at 50°C for 1 hour, take it out and wash it with a large amount of deionized water, so that the terminal mercapto The sulfonic acid group is oxidized to obtain a glass substrate with a sulfonic acid silane film on the surface.

[0031] The molar ratio of each compone...

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Abstract

The method to prepare sulfo radical silicane-rare earth nano composite thin membrane on glass substrate surface comprises, preparing sulfo radical silicane thin membrane with self-assemblt method and then rare-earth-element thin membrane with sol-gel method on hydroxylated substrate surface; dipping the substrate into Pirahan solution for one hour at 90Deg temperature; after clearing and drying, dipping it into mercaptoalkyl solution for 6-8h; clearing, blowing with nitrogen and putting into hitric acid to obtain the substrate with surface adsorbed sulfo radical silicane thin membrane; following, dipping the substrate into peptization solution composed of rare earth compounds, titanate, alcohol, diethyl ethanolamine and dimethyl formamide, drawing, drying, or repeating said operation to prepare multilayer thin membrane; putting sample in muffle furnace, heating slowly to 500Deg; then, cooling naturally to room temperature and obtain the product.

Description

technical field [0001] The invention relates to a preparation method of a rare earth nanocomposite film, in particular to a method for preparing a sulfonic acid silane-rare earth nanocomposite film by self-assembly on the surface of a glass substrate. It belongs to the field of film preparation. Background technique [0002] The development of modern mechanical science shows the trend of mechatronics, ultra-precision and miniaturization. The gap between friction pairs of many high-tech devices is often at the nanometer level. Due to the influence of size effects in micro-machines, micro-friction and wear and nano-film Lubrication has become a key issue, which can be solved by preparing self-assembled nano-films by self-assembly method. However, the film thickness adjustment range of the self-assembled monolayer film is limited, and the requirements for the substrate and film-forming materials are strict. The sol-gel method has the advantages of simple equipment, low cost, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C17/34C03C17/30
Inventor 程先华白涛蒋喆
Owner SHANGHAI JIAO TONG UNIV
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