CN107244814A - A kind of preparation method of hydrophobic rub resistance translucent alumina film - Google Patents
A kind of preparation method of hydrophobic rub resistance translucent alumina film Download PDFInfo
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- CN107244814A CN107244814A CN201710552749.0A CN201710552749A CN107244814A CN 107244814 A CN107244814 A CN 107244814A CN 201710552749 A CN201710552749 A CN 201710552749A CN 107244814 A CN107244814 A CN 107244814A
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/3411—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions with at least two coatings of inorganic materials
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/34—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts
- C01F7/36—Preparation of aluminium hydroxide by precipitation from solutions containing aluminium salts from organic aluminium salts
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/20—Materials for coating a single layer on glass
- C03C2217/21—Oxides
- C03C2217/214—Al2O3
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/70—Properties of coatings
- C03C2217/78—Coatings specially designed to be durable, e.g. scratch-resistant
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/112—Deposition methods from solutions or suspensions by spraying
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/30—Aspects of methods for coating glass not covered above
- C03C2218/32—After-treatment
Abstract
The invention discloses a kind of preparation method of hydrophobic rub resistance translucent alumina film, it is related to a kind of aluminum oxide film, includes each raw material of following parts by weight：8~12 parts of aluminium secondary butylate, 800~1200 parts of distilled water, 2~4 parts of nitric acid, 80~120 parts of ethyl acetate, mass percent concentration is 95% 80~120 parts of ethanol, 80~120 parts of deionized water, 80~120 parts of sour corrosion solution, 0.5~1.5 part of caustic corrosion solution, 1~3 part of hexadecyl trimethoxy silane.The preparation method for the hydrophobic rub resistance translucent alumina film that the invention is provided, the reaction time is short, and easy to operate, cost is low；Multiple sintering process increases the surface microporous structure of film；Realize that point type corrodes, it is to avoid the corrosion of film large area, can effective control corrosion rate degree by changing spraying distance or regulation liquid outlet quantity；The service life of film can effectively be extended.
Description
Technical field
The present invention relates to a kind of aluminum oxide film, and in particular to a kind of preparation of hydrophobic rub resistance translucent alumina film
Method.
Background technology
The organic film of a layered low-surface energy mainly is plated in film surface in the prior art, hydrophobic effect is reached.Generally
Colloidal sol is made using aluminium isopropoxide, the reaction time needs 6~12h, and the reaction time is long, and aluminium isopropoxide is on the high side；Mainly adopt
With spin-coating method or czochralski method, do not applied to for surface area especially big and material in irregular shape, and czochralski method colloidal sol consumption
It is especially big, usually it is difficult to realize coating single side；Mainly monofilm；It is using hydro-thermal method or acid and alkali corrosion method, i.e., film is whole
Individual to invade heating manufacture surface roughness in water or corrosive solution, film is corroded in large area；In aluminum oxide film table
Face applies one layer of organic film, and organic film crocking resistance is poor.
The content of the invention
Instant invention overcomes above-mentioned shortcoming, first purpose of the invention is to provide a kind of translucent oxygen of hydrophobic rub resistance
Change aluminium film, include each raw material of following parts by weight：8~12 parts of aluminium secondary butylate, 800~1200 parts of distilled water, 2~4 parts of nitric acid,
80~120 parts of ethyl acetate, mass percent concentration is 95% 80~120 parts of ethanol, 80~120 parts of deionized water, sour
80~120 parts of corrosion solution, 0.5~1.5 part of caustic corrosion solution, 1~3 part of hexadecyl trimethoxy silane.
It is preferred that, the hydrophobic rub resistance translucent alumina film includes each raw material of following parts by weight：Aluminium secondary butylate 10
Part, 1000 parts of distilled water, 3 parts of nitric acid, 100 parts of ethyl acetate, mass percent concentration is 95% 100 parts of ethanol, deionization
100 parts of water, 100 parts of sour corrosion solution, 1 part of caustic corrosion solution, 2 parts of hexadecyl trimethoxy silane.
Second object of the present invention is to provide a kind of preparation method of hydrophobic rub resistance translucent alumina film, specifically
Comprise the following steps：
1) preparation of alumina sol：In the distilled water that aluminium secondary butylate is added to 85 DEG C, magnetic agitation 30min is used, then
Using nitre acid for adjusting pH as 2, magnetic agitation 30min, obtains alumina sol at 85 DEG C, by the colloidal sol be aged 5 days it is stand-by；
2) preparation of glass carrier：The preparation of glass carrier：Load fragment is taken respectively with ethyl acetate 100ml, 95% ethanol
100ml, deionized water 100ml clean 30min, dried for standby in ultrasonoscope successively；
3) plated film is repeated：With spray-on process on glass carrier plated film, drying at room temperature 1 day, it is sintered with Muffle furnace,
Initial temperature is set to 50 DEG C, and heating rate is 1 DEG C/min, 200 DEG C of insulations 30min, 350 DEG C of insulation 30min, 550 DEG C of insulations
3h, repeats plated film 2~30 times, sinters 2~30 times, obtains film；
4) spray-on process chemical attack：By step 3) in obtained film be placed directly in the panel heater of temperature-adjustable
On, any one in film surface sprays sour corrosion solution or caustic corrosion solution obtains film body；
5) organic-alumina composite film is plated：By hexadecyl trimethoxy silane using mass percent concentration as 100%
Ethanol dissolved as solvent, be configured to mass percent concentration be 10% hexadecyl trimethoxy silane solution, take this
Hexadecyl trimethoxy silane solution 2.5g, while taking step 1) in obtained alumina sol 2.5g, in step 4) in
The film body surface alternating spray-on process plated film arrived, the heat drying in plated film, then with 160 DEG C of heat treatments in Muffle furnace
30min, is made hydrophobic rub resistance translucent alumina film.
It is preferred that, step 4) described in sour corrosion solution be hydrochloric acid solution, sulfuric acid solution, salpeter solution or acetum
In any one.
It is preferred that, step 4) described in caustic corrosion solution be any one in sodium hydroxide solution or potassium hydroxide solution
Kind.
It is preferred that, step 4) in film surface sprinkling sour corrosion solution or the instrument that uses of caustic corrosion solution be spray
Day with fog.
It is preferred that, step 5) in muffle furnace be set to 160 DEG C.
It is preferred that, step 2) in ethanol mass percent concentration be 95%.
The beneficial effects of the invention are as follows：
1) aluminum hydroxide sol is made using aluminium secondary butylate in the present invention, course of reaction only needs 1h, substantially reduces colloidal sol
Production Time, and aluminium secondary butylate price is cheap compared with aluminium isopropoxide；
2) using spraying coating method, any shape, the material of any size can light plated film, easy to operate, practicality,
Cost is low；
3) multiple plated film is used, multiple sintering process increases the surface microporous structure of film；
4) by film put on the heaters, with sprayer by corrosive liquid atomized spray on film, realize point type corrode,
The corrosion of film large area is avoided, can effective control corrosion rate degree by changing spraying distance or regulation liquid outlet quantity；
5) by the way that low-surface energy substance hexadecyl trimethoxy silane is added directly into colloidal sol, plated film, sintering makes
Hexadecyl trimethoxy silane is directly entrained in film layer, is sintered at 220 DEG C, makes organic matter effectively and aluminum oxide is combined, have
The protection of aluminum oxide, it is possible to reduce the frictional dissipation of outer bound pair hexadecyl trimethoxy silane, effectively extension film make
Use the life-span.
6) the roll angle contact angle of film and water produced by the present invention is 137.4 °, after 4.76N ball mills friction 300S,
Contact angle stills remain in 110 °, and other hydrophobic film contact angles that rubbed under equal conditions drop to less than 85 °.
Embodiment
Embodiment 1
The method that aluminium secondary butylate makes aluminum hydroxide sol comprises the following steps：
1) preparation of alumina sol：Aluminium secondary butylate 24.6g is added in 85 DEG C of 180g distilled water, magnetic agitation is used
30min, then pH is adjusted as 2 using nitric acid 6ml, magnetic agitation 30min, obtains alumina sol at 85 DEG C, and colloidal sol ageing is treated for 5 days
With；
2) preparation of glass carrier：Load fragment is taken respectively with ethyl acetate 100ml, 95% ethanol 100ml, deionized water
100ml cleans 30min, dried for standby in ultrasonoscope successively；
3) plated film is repeated：With spray-on process on glass carrier plated film, drying at room temperature 1 day, it is sintered with Muffle furnace,
Initial temperature is set to 50 DEG C, heating rate 1 DEG C/min, 200 DEG C of insulations 30min, 350 DEG C of insulations 30min, 550 DEG C of insulation 3h,
Repeat plated film 2~30 times, sinter 2~30 times, obtain film；
4) spray-on process chemical attack：By step 3) in obtained film be placed directly in the panel heater of temperature-adjustable
On, 0.5ml is sprayed in film surface with the sprayer for loading salpeter solution, film body is obtained；
5) organic-alumina composite film is plated：By hexadecyl trimethoxy silane using mass percent concentration as 100%
Ethanol dissolved as solvent, be configured to mass percent concentration be 10% hexadecyl trimethoxy silane solution, take this
Hexadecyl trimethoxy silane solution 2.5g, while taking step 1) in obtained alumina sol 2.5g, in step 4) in
Then the film body surface alternating spray-on process plated film arrived, the heat drying in plated film is heat-treated 30min, Muffle in Muffle furnace
Furnace temperature is set to 160 DEG C, and hydrophobic rub resistance translucent alumina film is made.
Embodiment 2
The method that aluminium secondary butylate makes aluminum hydroxide sol comprises the following steps：
1) preparation of alumina sol：Aluminium secondary butylate 49.2g is added in 85 DEG C of 360g distilled water, magnetic agitation is used
30min, then pH is adjusted as 2 using nitric acid 12ml, magnetic agitation 30min, obtains alumina sol at 85 DEG C, and the colloidal sol is aged 5 days
It is stand-by；
2) preparation of glass carrier：Load fragment is taken respectively with ethyl acetate 100ml, 95% ethanol 100ml, deionized water
100ml cleans 30min, dried for standby in ultrasonoscope successively；
3) plated film is repeated：With spray-on process on glass carrier plated film, drying at room temperature 1 day, it is sintered with Muffle furnace,
Initial temperature is set to 50 DEG C, heating rate 1 DEG C/min, 200 DEG C of insulations 30min, 350 DEG C of insulations 30min, 550 DEG C of insulation 1h,
Repeat plated film 2~30 times, sinter 2~30 times, obtain film；
4) spray-on process chemical attack：By step 3) in obtained film be placed directly in the panel heater of temperature-adjustable
On, 0.5ml is sprayed in film surface with the sprayer for filling out hydrochloric acid solution；
5) organic-alumina composite film is plated：By hexadecyl trimethoxy silane using mass percent concentration as 100%
Ethanol dissolved as solvent, be configured to mass percent concentration be 10% hexadecyl trimethoxy silane solution, take this
Hexadecyl trimethoxy silane solution 2.5g, while taking step 1) in obtained alumina sol 2.5g, in step 4) in
Then the film body surface alternating spray-on process plated film arrived, the heat drying in plated film is heat-treated 30min, Muffle in Muffle furnace
Furnace temperature is set to 160 DEG C, and hydrophobic rub resistance translucent alumina film is made.
Embodiment 3
The method that aluminium secondary butylate makes aluminum hydroxide sol comprises the following steps：
1) preparation of alumina sol：Aluminium secondary butylate 147.8g is added in 85 DEG C of 1080g distilled water, stirred with magnetic force
30min is mixed, then pH is adjusted as 2 using nitric acid 18ml, magnetic agitation 30min, obtains alumina sol at 85 DEG C, and the colloidal sol is aged into 5
It is stand-by；
2) preparation of glass carrier：Load fragment is taken respectively with ethyl acetate 100ml, 95% ethanol 100ml, deionized water
100ml cleans 30min, dried for standby in ultrasonoscope successively；
3) plated film is repeated：With spray-on process on glass carrier plated film, drying at room temperature 1 day, it is sintered with Muffle furnace,
Initial temperature is set to 50 DEG C, heating rate 1 DEG C/min, 200 DEG C of insulations 30min, 350 DEG C of insulations 30min, 550 DEG C of insulation 3h,
Repeat plated film 2~30 times, sinter 2~30 times, obtain film；
4) spray-on process chemical attack：By step 3) in obtained film be placed directly in the panel heater of temperature-adjustable
On, 0.5ml is sprayed in film surface with the sprayer for loading potassium hydroxide solution；
5) organic-alumina composite film is plated：By hexadecyl trimethoxy silane using mass percent concentration as 100%
Ethanol dissolved as solvent, be configured to mass percent concentration be 10% hexadecyl trimethoxy silane solution, take this
Hexadecyl trimethoxy silane solution 2.5g, while taking step 1) in obtained alumina sol 2.5g, in step 4) in
Then the film body surface alternating spray-on process plated film arrived, the heat drying in plated film is heat-treated 30min, Muffle in Muffle furnace
Furnace temperature is set to 160 DEG C, and hydrophobic rub resistance translucent alumina film is made.
Aluminum hydroxide sol is made using aluminium secondary butylate in the present invention, colloidal sol Production Time is short, and aluminium secondary butylate is cheap,
Manpower, financial resources can be saved in actual production；Using multiple coating method, and surface microporous structure can be increased, can effectively controlled again
Thickness；Etch is heated using atomizing, it is to avoid the large area corrosion of film in the solution；The use of film can effectively be extended
Life-span.
The roll angle contact angle of this film and water produced by the present invention is 137.4 °, after 4.76N ball mills friction 300S,
Contact angle stills remain in 110 °, and other hydrophobic film contact angles that rubbed under equal conditions drop to less than 85 °.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the simply explanation described in above-described embodiment and specification is originally
The principle of invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (8)
1. a kind of hydrophobic rub resistance translucent alumina film, it is characterised in that each raw material including following parts by weight：Sec-butyl alcohol
8~12 parts of aluminium, 800~1200 parts of distilled water, 2~4 parts of nitric acid, 80~120 parts of ethyl acetate, mass percent concentration is 95%
80~120 parts of ethanol, 80~120 parts of deionized water, 80~120 parts of sour corrosion solution, caustic corrosion solution 0.5~1.5
Part, 1~3 part of hexadecyl trimethoxy silane.
2. hydrophobic rub resistance translucent alumina film according to claim 1, it is characterised in that including following parts by weight
Each raw material：10 parts of aluminium secondary butylate, 1000 parts of distilled water, 3 parts of nitric acid, 100 parts of ethyl acetate, mass percent concentration is 95%
100 parts of ethanol, 100 parts of deionized water, 100 parts of sour corrosion solution, 1 part of caustic corrosion solution, hexadecyl trimethoxy
2 parts of silane.
3. a kind of preparation method of hydrophobic rub resistance translucent alumina film as claimed in claim 1, it is characterised in that specific
Comprise the following steps：
1) preparation of alumina sol：In the distilled water that aluminium secondary butylate is added to 85 DEG C, magnetic agitation 30min is used, then with nitre
Acid for adjusting pH is magnetic agitation 30min at 2,85 DEG C, obtains alumina sol, by the colloidal sol be aged 5 days it is stand-by；
2) preparation of glass carrier：Load fragment is taken respectively with ethyl acetate 100ml, 95% ethanol 100ml, deionized water 100ml
30min, dried for standby are cleaned in ultrasonoscope successively；
3) plated film is repeated：With spray-on process on glass carrier plated film, drying at room temperature 1 day, it is sintered with Muffle furnace, initially
Temperature setting is 50 DEG C, and heating rate is 1 DEG C/min, 200 DEG C of insulations 30min, 350 DEG C of insulations 30min, 550 DEG C of insulation 3h, weight
Plated film 2~30 times, sinters 2~30 times, obtains film again；
4) spray-on process chemical attack：By step 3) in obtained film be placed directly on the panel heater of temperature-adjustable,
Film surface sprays any one in sour corrosion solution or caustic corrosion solution, obtains film body；
5) organic-alumina composite film is plated：Second by hexadecyl trimethoxy silane using mass percent concentration as 100%
Alcohol dissolves as solvent, be configured to mass percent concentration be 10% hexadecyl trimethoxy silane solution, take this 16
Alkyl trimethoxysilane solution 2.5g, while taking step 1) in obtained alumina sol 2.5g, in step 4) in obtain
Spray-on process plated film is alternately used in film body surface, the heat drying in plated film, then with 160 DEG C of heat treatment 30min, system in Muffle furnace
Obtain hydrophobic rub resistance translucent alumina film.
4. the preparation method of hydrophobic rub resistance translucent alumina film according to claim 3, it is characterised in that step
4) solution of sour corrosion described in is any one in hydrochloric acid solution, sulfuric acid solution, salpeter solution or acetum.
5. the preparation method of hydrophobic rub resistance translucent alumina film according to claim 3, it is characterised in that step
4) caustic corrosion solution described in is any one in sodium hydroxide solution or potassium hydroxide solution.
6. the preparation method of hydrophobic rub resistance translucent alumina film according to claim 3, it is characterised in that step
4) instrument that film surface sprinkling sour corrosion solution or caustic corrosion solution are used in is sprayer.
7. the preparation method of hydrophobic rub resistance translucent alumina film according to claim 3, it is characterised in that step
5) muffle furnace is set to 160 DEG C in.
8. the preparation method of hydrophobic rub resistance translucent alumina film according to claim 3, it is characterised in that step
2) mass percent concentration of ethanol is 95% in.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710552749.0A CN107244814B (en) | 2017-07-07 | 2017-07-07 | Preparation method of hydrophobic friction-resistant semitransparent alumina film |
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| CN201710552749.0A CN107244814B (en) | 2017-07-07 | 2017-07-07 | Preparation method of hydrophobic friction-resistant semitransparent alumina film |
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| CN107244814A true CN107244814A (en) | 2017-10-13 |
| CN107244814B CN107244814B (en) | 2020-07-03 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112225467A (en) * | 2020-10-15 | 2021-01-15 | 云南开放大学 | Preparation method of ultra-smooth aluminum oxide film |
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| CN112225467A (en) * | 2020-10-15 | 2021-01-15 | 云南开放大学 | Preparation method of ultra-smooth aluminum oxide film |
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