CN101508529A - Method for producing bismuth vanadate compound film on glass substrate surface - Google Patents
Method for producing bismuth vanadate compound film on glass substrate surface Download PDFInfo
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- CN101508529A CN101508529A CNA2009100483824A CN200910048382A CN101508529A CN 101508529 A CN101508529 A CN 101508529A CN A2009100483824 A CNA2009100483824 A CN A2009100483824A CN 200910048382 A CN200910048382 A CN 200910048382A CN 101508529 A CN101508529 A CN 101508529A
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- glass substrate
- bismuth vanadate
- film
- pucherite
- deionized water
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Abstract
The invention discloses a method for preparing a bismuth vanadate composite film on the surface of a glass substrate, which comprises the following steps that: a sulfonic silane film is prepared on the surface of a hydroxylated glass substrate by a self-assembly method, then the glass substrate is placed into a N, N-dimethylformamide bismuth vanadate dispersion liquid, and bismuth vanadate is deposited on the surface of the glass substrate. Firstly, the glass substrate is dipped into a Pirahan solution, treated for 1 hour at the temperature of 90 DEG C, cleaned and dried, then dipped into a mercapto silane solution, kept stand for 6 to 8 hours, then taken out for washing, blow-dried by nitrogen, and then placed into a nitric acid solution to obtain the glass substrate of which the surface is attached with the sulfonic silane film; and then the glass substrate is placed into a bismuth vanadate suspension, is kept stand for 4 to 20 hours at a temperature of between 20 and 80 DEG C, is taken out to be washed by a large amount of deionized water, and is blow-dried by nitrogen after the washing, thus the glass substrate of which the surface is deposited with a modified bismuth vanadate composite film is obtained. The method can reduce the friction coefficient from 0.8 (no film exists) to 0.1, and has obvious antifriction effect.
Description
Technical field
The present invention relates to a kind of method for preparing bismuth vanadate compound film at glass substrate surface.Belong to the film preparing technology field.
Background technology
Electromechanical integration, ultrapreciseization and microminiaturized trend appear in the modern mechanical the reach of science, the friction pair gap of many new and high technology devices etc. often is in nanometer scale, owing to be subjected to the influence of dimensional effect in the micromachine, micro friction wear and nano-scale thin film lubrication have become key issue, can prepare the self-assembled nanometer film with self-assembling method at present and solve this problem.Compare with other preparation thin film technique, the self-assembled film technology has operability, adaptability is strong, is with a wide range of applications.
Pucherite is most typical monodimension nanometer material, has numerous excellent properties with its particular structure.Pucherite has superpower mechanical property, good adsorption property, thereby has caused very big attention in the material field.But pucherite radial nano-grade size and high surface energy cause its easy reunion, and be dispersed relatively poor, reduced the effective L D ratio of pucherite.In addition, pucherite is insoluble in most solvents, and wet performance is poor, is difficult to be formed with effective adhesive with substrate.
Find that by literature search publication number is the Chinese invention patent of CN1358804A, has introduced a kind of preparation method of solid film surface fatty acid self-composed monomolecular ultrathin lubrication membrane, this method is the unimolecular layer at solid surface self-assembly one deck lipid acid.Choose the lipid acid that easily is adsorbed in solid surface, be mixed with dilute solution, the ceramic membrane that makes is immersed the lipid acid dilute solution that configures rapidly under room temperature, reacted 24～48 minutes.This method needs 24～96 hours time to prepare precursor solution in the process of preparation self-assembled film, make that so whole film forming period is long, and in the process that substrate is handled, do not relate to concrete grammar, more do not relate to improvement and the research of pucherite to film performance.
Summary of the invention
The invention discloses a kind of method for preparing bismuth vanadate compound film at glass substrate surface, its purpose is to overcome the long drawback of existing preparation self-assembled film process film forming period, the present invention not only preparation cycle is short, preparation technology is simple, and the laminated film that is self-assembled into has good antifriction performance.
A kind ofly prepare the method for bismuth vanadate compound film, it is characterized in that comprising the steps: at glass substrate surface
A) glass substrate adopts hydroxylation to handle:
A) earlier glass substrate being dipped in volume ratio is H
2SO
4: H
2O
2In=70: 30 the solution, handled 1 hour down in 90 ℃;
B) with dry in the baking oven that is placed on after the deionized water ultrasonic cleaning in the dust keeper;
C) to immerse hydrosulphonyl silane concentration be in the benzole soln of 0.1～2.0mmol/L to the glass substrate after will handling, and leaves standstill taking-ups in 6～8 hours, and flushing then dries up with nitrogen;
D) glass substrate being placed mass concentration is 30%～60% nitric acid again, 50～80 ℃ of reactions 1 hour down, takes out and use deionized water rinsing, obtains the glass substrate that the surface has the sulfonic silane film;
B) preparation pucherite dispersion liquid:
E) pucherite is at room temperature put into N by 0.1～0.2mg/ml, the dinethylformamide dispersion agent, 40W ultrasonic dispersing 1～4 hour obtains stable pucherite suspension;
C) the preparation surface deposition has the glass substrate of bismuth vanadate compound film:
F) surface-assembled there is the glass substrate of sulfonic silane film immerse in the pucherite suspension for preparing, under 20～80 ℃, left standstill 4～20 hours;
G) take out the glass substrate deionized water rinsing, the flushing back dries up with nitrogen, so just obtains the glass substrate that surface deposition has the modification bismuth vanadate compound film.
Technology of the present invention is simple, and preparation cycle is short, does not have problem of environmental pollution; The bismuth vanadate compound film of glass substrate surface preparation can be with frictional coefficient 0.8 during from no film be reduced to about 0.1, have fairly obvious antifriction function.Bismuth vanadate compound film also has good wear resistance in addition, can become micromachine ideal boundary lubricant film.
Embodiment
Below by specific embodiment technical scheme of the present invention is further described.But present embodiment is not limited to the present invention, and all employings similarity method of the present invention and similar variation thereof all should be listed protection scope of the present invention in.
Embodiment 1:
At first, glass substrate adopts hydroxylation pre-treatment, treatment process: glass substrate is dipped in Pirahan solution (H
2SO
4: H
2O
2=70: 30, V/V) in, handled 1 hour down in 90 ℃, use a large amount of deionized water ultrasonic cleaning 20 minutes again, be placed in the baking oven in the dust keeper dry, to leave standstill 6 hours in the glass substrate immersion hydrosulphonyl silane solution after handling, the component volumetric molar concentration of hydrosulphonyl silane solution is: 3-sulfydryl propyl group methyl dimethoxysilane 0.2mmol/L, solvent is a benzole soln.Use chloroform, acetone, deionized water rinsing after the taking-up respectively, remove the organic molecule of surface physics absorption, dry up with nitrogen again that to place weight concentration be 30% nitric acid, 80 ℃ of reaction taking-ups after 1 hour down, use a large amount of deionized water rinsings, so just end sulfydryl in-situ oxidation is become sulfonic group, obtain the glass substrate of surface with the sulfonic silane film.
At room temperature pucherite is put into N by 0.15mg/ml, dinethylformamide (DMF) dispersion agent, ultrasonic dispersing (40W) 2 hours obtains steady suspension.
There is the glass substrate of sulfonic silane film to immerse in the pucherite suspension for preparing surface-assembled, under 20 ℃, left standstill 4 hours, take out and use a large amount of deionized water rinsings, the flushing back dries up with nitrogen, so just obtains the glass substrate that surface deposition has the modification bismuth vanadate compound film.
Adopt SPM-9500 atomic force microscope (AFM), JEM-2010 scanning electronic microscope (SEM) and PHI-5702 type X-photoelectron spectrograph (XPS) to characterize the surface topography and the chemical ingredients of the composite membrane that obtains.Adopt the little frictional behaviour survey meter of the pure slip of some contact to measure the composite membrane frictional coefficient.
The XPS collection of illustrative plates shows in the Silan-based Thin Films that glass substrate surface is self-assembled into mercapto groups; Behind the in-situ oxidation, high valence state element sulphur is arranged, illustrate that the in-situ oxidation of the mercapto groups success on the surperficial Silan-based Thin Films has become sulfonic group.The SEM picture sees clearly that then pucherite is deposited on the surface of glass substrate, has formed bismuth vanadate compound film.On a little frictional behaviour survey meter of the pure slip of contact, measure the frictional coefficient of clean glass substrate and glass substrate surface pucherite composite membrane respectively.The pucherite composite membrane of glass substrate surface preparation can be with frictional coefficient 0.8 during from no film be reduced to 0.12, have fairly obvious antifriction function.
Embodiment 2:
At first, the hydroxylation pre-treatment of glass substrate: glass substrate is dipped in the Pirahan solution, handled 1 hour down in 90 ℃, use a large amount of deionized water ultrasonic cleaning 20 minutes again, be placed on drying in the inherent baking oven of a dust keeper, the glass substrate after handling is immersed in the hydrosulphonyl silane solution for preparing, left standstill 7 hours, the component volumetric molar concentration of hydrosulphonyl silane solution is: 3-sulfydryl propyl group methyl dimethoxysilane 1.0mmol/L, and solvent is a benzole soln; After removing the surface physics adsorbed organic matter with chloroform, acetone, deionized water rinsing respectively after the taking-up, dry up with nitrogen that to place mass concentration be 50% nitric acid, reacted 1 hour down at 65 ℃, take out and use a large amount of deionized water rinsings, so just end sulfydryl in-situ oxidation is become sulfonic group, obtain the glass substrate of surface with the sulfonic silane film.
At room temperature pucherite is put into N by 0.1mg/ml, dinethylformamide (DMF) dispersion agent, ultrasonic dispersing (40W) 3 hours obtains steady suspension.
There is the glass substrate of sulfonic silane film to immerse in the pucherite suspension for preparing surface-assembled, under 60 ℃, left standstill 6 hours, take out and use a large amount of deionized water rinsings, the flushing back dries up with nitrogen, so just obtains the glass substrate that surface deposition has the modification bismuth vanadate compound film.
Adopt the characterization method among the embodiment 1 that film quality is estimated.
The XPS collection of illustrative plates shows and contains sulfonic group and Ce elements in the thin film layers different in the laminated film that glass substrate surface is self-assembled into, and do not observe the index of silicon-dioxide after the Silan-based Thin Films assembling.The SEM picture sees clearly that then pucherite is deposited on the surface of glass substrate, has formed bismuth vanadate compound film.The bismuth vanadate compound film of glass substrate surface preparation can be with frictional coefficient 0.8 during from no film be reduced to about 0.11, have fairly obvious antifriction function.
Embodiment 3:
At first, the hydroxylation pre-treatment of glass substrate: glass substrate is dipped in the Pirahan solution, handled 1 hour down in 90 ℃, use a large amount of deionized water ultrasonic cleaning 20 minutes again, be placed on drying in the inherent baking oven of a dust keeper, the glass substrate after handling is immersed in the hydrosulphonyl silane for preparing, left standstill 8 hours, the component volumetric molar concentration of hydrosulphonyl silane solution is: 3-sulfydryl propyl trimethoxy silicane 2.0mmol/L, solvent are benzole soln; After using chloroform, acetone, deionized water rinsing respectively after the taking-up, dry up that to place mass concentration be 60% nitric acid 50 ℃ of reactions 1 hour down with nitrogen, take out and use a large amount of deionized water rinsings, so just end sulfydryl in-situ oxidation is become sulfonic group, obtain the glass substrate of surface with the sulfonic silane film.
At room temperature pucherite is put into N by 0.2mg/ml, dinethylformamide (DMF) dispersion agent, ultrasonic dispersing (40W) 4 hours obtains steady suspension.
There is the glass substrate of sulfonic silane film to immerse in the pucherite suspension for preparing surface-assembled, under 80 ℃, left standstill 20 hours, take out and use a large amount of deionized water rinsings, the flushing back dries up with nitrogen, so just obtains the glass substrate that surface deposition has the modification bismuth vanadate compound film.
Adopt the characterization method among the embodiment 1 that film quality is estimated.The XPS collection of illustrative plates shows is successfully assembling the hydrosulphonyl silane film on the substrate surface, and mercapto groups is become sulfonic group by in-situ oxidation; The SEM picture sees clearly that then pucherite is deposited on the surface of glass substrate, has formed bismuth vanadate compound film.The bismuth vanadate compound film of glass substrate surface preparation can be with frictional coefficient 0.8 during from no film be reduced to about 0.1, have fairly obvious antifriction function.
Claims (1)
1, a kind ofly prepares the method for bismuth vanadate compound film, it is characterized in that comprising the steps: at glass substrate surface
A) glass substrate adopts hydroxylation to handle:
A) earlier glass substrate being dipped in volume ratio is H
2SO
4: H
2O
2In=70: 30 the solution, handled 1 hour down in 90 ℃;
B) with dry in the baking oven that is placed on after the deionized water ultrasonic cleaning in the dust keeper;
C) to immerse hydrosulphonyl silane concentration be in the benzole soln of 0.1～2.0mmol/L to the glass substrate after will handling, and leaves standstill taking-ups in 6～8 hours, and flushing then dries up with nitrogen;
D) glass substrate being placed mass concentration is 30%～60% nitric acid again, 50～80 ℃ of reactions 1 hour down, takes out and use deionized water rinsing, obtains the glass substrate that the surface has the sulfonic silane film;
B) preparation pucherite dispersion liquid:
E) pucherite is at room temperature put into N by 0.1～0.2mg/ml, the dinethylformamide dispersion agent, 40W ultrasonic dispersing 1～4 hour obtains stable pucherite suspension;
C) the preparation surface deposition has the glass substrate of bismuth vanadate compound film:
F) surface-assembled there is the glass substrate of sulfonic silane film immerse in the pucherite suspension for preparing, under 20～80 ℃, left standstill 4～20 hours;
G) take out the glass substrate deionized water rinsing, the flushing back dries up with nitrogen, so just obtains the glass substrate that surface deposition has the modification bismuth vanadate compound film.
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|---|---|---|---|
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| CNA2009100483824A CN101508529A (en) | 2009-03-27 | 2009-03-27 | Method for producing bismuth vanadate compound film on glass substrate surface |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786023B (en) * | 2010-02-12 | 2011-10-19 | 湖州师范学院 | Ultrasonic chemical in-situ preparation method for phthalocyanine-sensitized vanadate nano-powder |
| CN102247831A (en) * | 2011-05-17 | 2011-11-23 | 东华大学 | Method for preparing activated carbon self-assembled bismuth vanadate water treatment agent |
| CN109778304A (en) * | 2019-03-20 | 2019-05-21 | 广州大学 | A kind of vanadium doping bismuth sulfide nano line crystal film and its preparation method and application |
-
2009
- 2009-03-27 CN CNA2009100483824A patent/CN101508529A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101786023B (en) * | 2010-02-12 | 2011-10-19 | 湖州师范学院 | Ultrasonic chemical in-situ preparation method for phthalocyanine-sensitized vanadate nano-powder |
| CN102247831A (en) * | 2011-05-17 | 2011-11-23 | 东华大学 | Method for preparing activated carbon self-assembled bismuth vanadate water treatment agent |
| CN109778304A (en) * | 2019-03-20 | 2019-05-21 | 广州大学 | A kind of vanadium doping bismuth sulfide nano line crystal film and its preparation method and application |
| CN109778304B (en) * | 2019-03-20 | 2020-07-31 | 广州大学 | Vanadium-doped bismuth sulfide nanowire crystal film and preparation method and application thereof |
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Open date: 20090819 |