CN107500562A - A kind of high grade of transparency glass for touch-screen and preparation method thereof - Google Patents
A kind of high grade of transparency glass for touch-screen and preparation method thereof Download PDFInfo
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- CN107500562A CN107500562A CN201710643459.7A CN201710643459A CN107500562A CN 107500562 A CN107500562 A CN 107500562A CN 201710643459 A CN201710643459 A CN 201710643459A CN 107500562 A CN107500562 A CN 107500562A
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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
- C03C17/3429—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 at least one of the coatings being a non-oxide coating
- C03C17/3441—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 at least one of the coatings being a non-oxide coating comprising carbon, a carbide or oxycarbide
-
- 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
- C03C2217/73—Anti-reflective coatings with specific characteristics
-
- 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
- C03C2217/77—Coatings having a rough surface
-
- 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
-
- 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
Abstract
The present invention relates to touch screen technology field, more particularly to a kind of high grade of transparency glass for touch-screen and preparation method thereof, high grade of transparency glass includes clear glass substrate, and the graphene film and SiO being in turn attached on glass baseplate2Film, the thickness of the graphene film is 5nm~12nm, the SiO2Film surface has rough micro-structural, and graphene film is to be formed on the glass substrate using liquid level sedimentation dry solidification, the SiO2Film is by SiO2Masking liquid is sprayed on what dry solidification on graphene film was formed.The present invention forms graphene film and SiO using liquid level sedimentation and spraying process in clear glass substrate2Film, process are easily controlled, and the glass transparent degree produced is high, good, the durable of anti-glare properties energy, can be applied in the preparation assembling of touch-screen.
Description
Technical field
The present invention relates to touch screen technology field, more particularly to it is a kind of for the high grade of transparency glass of touch-screen and its preparation
Method.
Background technology
Touch-screen is also known as " touch screen ", " contact panel ", is a kind of induction type glass for receiving the input signals such as contact
Glass liquid crystal display device, when contacting the graphic button on screen, the haptic feedback system on screen can be according to preprogramming
Formula drive various attachment means, be substituted for mechanical push button panel, and manufacture and be born by liquid crystal display picture
Dynamic visual and sound effects.Touch-screen as a kind of newest computer input apparatus, it be it is most simple at present, conveniently, it is naturally a kind of
Man-machine interaction mode, it imparts multimedia with brand-new looks, is extremely attractive brand-new multimedia interactive equipment, extensively
Applied to portable electronic devices such as mobile phone, digital camera, personal digital assistant (PDA), tablet personal computer and notebook computers, with
While this high speed development, there are distinct issues in the use of touch-screen：Environment and extraneous light, which are radiated at, to be touched on panel glass
Easily cause dazzle, dazzle can cause the functions such as the contrast impressions of eyes, eyesight, recognition speed to decline, it is also possible to cause cornea
Inflammation, damage eyes.
In order to avoid glare effects vision, the technological means of solution is to apply atomization process to the shiny surface of glass.Citing
For, atomizing type common at present has following several：
1st, one layer of PET film is attached in the shiny surface of strengthened glass, although such a mode has equipment (laminator) cost low
With yield it is high the advantages that；But EC regulations gradually disable PET now；On the other hand, must be simultaneously using more during volume production
Platform laminator, thus extend floor space and human side.
2nd, using physical vapour deposition (PVD) (PVD) technology in the anti-dazzling film of shiny surface coating one of strengthened glass, such a mode
Although have the advantages that the uniformity of anti-dazzling film is good good with adhesive force；But physical gas phase deposition technology is used except it
Equipment and medicament it is expensive outside, also affect the penetration of strengthened glass.
3rd, using coating (spray coating) technology in the anti-dazzling film of shiny surface coating one of strengthened glass, Ci Zhongfang
Although formula has the advantages of equipment is cheap；But the anti-dazzling film formed using coating method is except the uniformity is poor, easily drops
And easily caused by colourity is uneven various vestiges phenomenon.
Therefore, there is an urgent need to one kind both to have the high grade of transparency, and the glass of the enough anti-dazzles of and can is used for the preparation skill of touch-screen
In art.
The content of the invention
In view of this, it is an object of the invention to provide a kind of high grade of transparency glass for touch-screen and preparation method thereof,
The preparation method is simple and easy to control, and the glass transparent degree prepared is high, and anti-glare properties can good, durable.
The present invention solves above-mentioned technical problem by following technological means：
A kind of high grade of transparency glass for touch-screen, including clear glass substrate, and it is in turn attached to glass baseplate
On graphene film and SiO2Film, the thickness of the graphene film is 5nm~12nm, the SiO2Film surface has
Rough micro-structural.
Further, the graphene film is to be formed on the glass substrate using liquid level sedimentation dry solidification, described
SiO2Film is by SiO2Masking liquid is sprayed on what dry solidification on graphene film was formed.
Further, the SiO2Masking liquid includes 2%~5% SiO2Gel, 82%~90% ethanol and 6%~15%
Petroleum ether.
In addition, the invention also discloses a kind of preparation method of the high grade of transparency glass for touch-screen, including following step
Suddenly：
The preparation of graphene oxide, in ice-water bath by natural flake graphite after microwave expansion is handled, adding volume ratio is
17:In 3 concentrated sulfuric acid and the mixed solution of phosphoric acid, stirring is abundant, adds KMnO4, 30min is stirred, oil bath heating is to 35 DEG C
2h is stirred, is again heated to 90 DEG C of stirring 1.5h, the dense degree of volume is then slowly added dropwise as 10% H2O2The aqueous solution, it is added dropwise
Afterwards, it is transferred in supercentrifuge and is centrifugally separating to obtain sediment, sediment is washed with HCl solution, then is washed with deionized
To pH=5.5~6.5, vacuum freeze drying obtains graphene oxide, adds in the ethanol solution that every liter of volumetric concentration is 80%
Enter 0.4g graphene oxides ultrasonic disperse and form graphene oxide dispersion, stored under 2 DEG C~5 DEG C environment.
SiO2The preparation of masking liquid, takes SiO2Gel adds the in the mixed solvent stirring of petroleum ether and ethanol, obtains SiO2Apply
Liquid, temperature is stored in as in 2 DEG C~5 DEG C environment.
The formation of graphene oxide film, the glass baseplate through Surface Treatment with Plasma is placed on to the substrate frame of film balance
On, deionized water is added, 1mL graphene oxide dispersions are slowly added dropwise, 1.5h~3h is stood, with 10mm/min~13mm/min
Speed slow membrane graphene oxide is adhered on the glass substrate, be repeatedly injected graphene oxide dispersion and membrane 3~8
After secondary, in 80 DEG C~95 DEG C dry 6h, i.e., graphene oxide film is obtained on the glass substrate.
SiO2The formation of film, using flush coater by SiO2Masking liquid mixes with the pressure-air in nozzle, in 3kg/cm2's
Spraying swath pressure even application is put into tube furnace on graphene oxide film, in air atmosphere with 3 DEG C/min speed liter
Temperature is heat-treated 5h to 250 DEG C~350 DEG C, stands cooling, that is, obtains having graphene film and SiO2The high grade of transparency glass of film
Glass.
Further, the rotating speed of centrifuge is 7000r/min~8500r/min in the preparation process of the graphene oxide.
Further, the SiO2The preparation method of gel is as follows：Water intaking glass and deionized water press 1:5.0 mass ratio mixes
Stirring 10min is closed, pentaerythrite is added and stirs to whole dissolvings, adds second acid for adjusting pH to 6.2~6.8, after stirring 20min,
2h is stood, obtains SiO2Wet gel, by SiO2Wet gel is transferred to aging 72h in 40 DEG C~50 DEG C baking boxs, and taking-up is put into ethanol solution
Middle progress solvent displacement, places into and modification is soaked in hydrophobic modifier HMDO, carried out once every 6h, carried out altogether
After 5 times, washed with ethanol solution, in 65 DEG C of dry 18h, obtain SiO2Gel.
Further, the addition of the pentaerythrite is the 4.5% of waterglass quality.
Further, the SiO2In 25 DEG C~30 DEG C of temperature in the forming step of film, relative humidity 55%~65%
Sprayed in environment.
Further, the SiO2The quantity for spray of masking liquid is 4cc/min~7cc/min, and flush coater X-axis translational speed is
400mm/s~600mm/s.
Glass baseplate is first carried out Surface Treatment with Plasma by the present invention, then is solidified on the glass substrate using liquid level sedimentation
Graphene film is formed, can so strengthen the graphene film fastness Nian Jie with glass baseplate, avoid coming off.Graphene is
A kind of bi-dimensional cellular shape carbon material of an only carbon atom thickness, the absorption to white light is only π α ≈ 2.3%, therefore is had
High translucency, for being attached to glass, there is higher transparency, suitable for touch screen technology field.
The present invention, using pentaerythrite as crosslinking agent, makes system in the preparation of silica dioxide gel before gel is formed
In be uniformly distributed pentaerythrite, then carry out gel, this compound can make whole gel network structure become more solid, with
Resist drying process in due to solvent volatilization caused by capillary pressure and surface hydroxyl further polycondensation and caused body
Product is shunk, so as to reduce the cleavage rate and cubical contraction of gel monolith to a certain extent.Silica has delustring
Property, the masking liquid containing silica dioxide gel is sprayed on graphene oxide film, surface shrinkage when solvent volatilizees, silica
Particle volume concentration increase, therefore the increase of paint film viscosity, viscoelastic property improve.But coating surface is still protected by surface tension
Water holding is put down, and collecting particulate in this process moves downward, and with the increase of viscoelastic power, particulate moves downward speed reduction；With when
Between increase, chemical reaction degree increase, when surface tension can not maintain surface level so that surface wrinkling.Now particulate
Retard motion, surface volume are reduced, and final particulate oriented alignment in film makes film coated surface coarse, are formed rough micro-
It structure, can cause to diffuse during reflected light projects, thus improve the glare effect caused by strong light, while can also reduce grease and attach
On glass, there is fingerprint-proof function.
Embodiment
Below with reference to specific embodiment, the present invention is described in detail：
A kind of high grade of transparency glass for touch-screen of the present invention, including clear glass substrate, and be in turn attached to
Graphene film and SiO on glass baseplate2Film, graphene film are to be dried admittedly using liquid level sedimentation on the glass substrate
Change what is formed, the thickness of graphene film is 5nm~12nm.SiO2Film is by SiO2Masking liquid is sprayed on graphene film and done
It is dry to be formed by curing, SiO2Film surface has rough micro-structural.SiO2Masking liquid is using ethanol as primary solvent, is disperseed
There is SiO2Gel, the SiO2Gel passes through hydrophobically modified, and its preparation method is as follows：
Embodiment one：SiO2The preparation of gel
Take 20mL waterglass and 100mL deionized waters to add in beaker, beaker is put on magnetic stirring apparatus and stirs 10min
Afterwards, 0.9g pentaerythrites are added, whole dissolvings is continued stirring until, obtains predecessor；Acetic acid is added as catalyst, regulation
PH to 6.2, after stirring 20min, stop stirring, solution left standstill reaction 2h, obtain silica wet gel；Silica is wet solidifying
Glue is transferred to aging 72h in the baking box that temperature is 40 DEG C, and it is co-continuous that taking-up is put into progress solvent displacement, each 6h in ethanol solution
Displacement 4 times, place into and modification is soaked in the ethanol solution containing hydrophobic modifier HMDO, each 6h, carry out 5 altogether
After secondary, filtering is washed with ethanol solution, and 18h is dried in 65 DEG C of baking box, obtains SiO2Gel.
Embodiment two：SiO2The preparation of gel
Take 20mL waterglass and 100mL deionized waters to add in beaker, beaker is put on magnetic stirring apparatus and stirs 10min
Afterwards, 0.9g pentaerythrites are added, whole dissolvings is continued stirring until, obtains predecessor；Acetic acid is added as catalyst, regulation
PH to 6.8, after stirring 20min, stop stirring, solution left standstill reaction 2h, obtain silica wet gel；Silica is wet solidifying
Glue is transferred to aging 72h in the baking box that temperature is 50 DEG C, and it is co-continuous that taking-up is put into progress solvent displacement, each 6h in ethanol solution
Displacement 4 times, place into and modification is soaked in the ethanol solution containing hydrophobic modifier HMDO, each 6h, carry out 5 altogether
After secondary, filtering is washed with ethanol solution, and 18h is dried in 65 DEG C of baking box, obtains SiO2Gel.
Embodiment three：The preparation of high grade of transparency glass
The preparation method of the high grade of transparency glass of the present embodiment is as follows：
The preparation of graphene oxide, in ice-water bath, by natural flake graphite after microwave expansion is handled, add volume ratio
For 17:In 3 concentrated sulfuric acid and the mixed solution of phosphoric acid, 1g natural flake graphites are added the 85mL concentrated sulfuric acids and 15mL by the present embodiment
In the mixed solution of phosphoric acid, stirring is abundant, adds 6gKMnO4, 30min is stirred, oil bath heating reheats to 35 DEG C of stirring 2h
To 90 DEG C of stirring 1.5h, the H that volumetric concentration is 10% is then slowly added dropwise2O2The aqueous solution, after being added dropwise, it is transferred to high speed centrifugation
To be centrifuged under 7500r/min rotating speed in machine, obtained sediment is washed with 1mol/L HCl solution, then is spent
Ion water washing to pH=6.0, vacuum freeze drying obtains graphene oxide, in the ethanol solution that every liter of volumetric concentration is 80%
Middle addition 0.4g graphene oxides ultrasonic disperse forms graphene oxide dispersion, is stored under 2 DEG C~5 DEG C environment.
SiO2The preparation of masking liquid, the SiO for taking the embodiment one that percetage by weight is 5% to prepare2Gel, 82% ethanol and
13% petroleum ether mixes, and obtains SiO2Masking liquid, temperature is stored in as in 2 DEG C~5 DEG C environment.
The formation of graphene oxide film, the glass baseplate through Surface Treatment with Plasma is placed on to the substrate frame of film balance
On, deionized water is added to glass baseplate is covered completely, and 1mL graphene oxide dispersions are slowly added dropwise by micro syringe,
2h is stood, until graphene oxide is evenly dispersed in deionized water surface, will be aoxidized with the slow membrane of 12mm/min speed
Graphene adheres on the glass substrate, after being repeatedly injected graphene oxide dispersion and membrane 6 times, is dried in 80 DEG C of baking oven
6h, graphene oxide film is obtained on the glass substrate.
SiO2The formation of film, SiO is carried out in 26 DEG C of temperature, the environment of relative humidity 55%2The spraying of masking liquid, use
Flush coater is by SiO2Masking liquid mixes with the pressure-air in nozzle, squeezes out superfine atomizing particle, and flush coater X-axis translational speed is
500mm/s, and with 4cc/min quantity for spray and 3kg/cm2Spraying swath pressure under, by SiO2Masking liquid even application is in graphite oxide
On alkene film, it is put into tube furnace, is warming up to 300 DEG C in air atmosphere with 3 DEG C/min speed, be heat-treated 5h, stands cold
But, that is, obtain having graphene film and SiO2The high grade of transparency glass of film.
Performance detection is carried out to high grade of transparency glass manufactured in the present embodiment, the thickness for detecting graphene film is 5nm.
SiO by transmission electron microscope to glass surface2Film is scanned, and finds SiO2The surface of film presents uneven
Micro-structural, there is anti-dazzle.In addition, the glossiness for measuring the high grade of transparency glass of the present embodiment is 80 (BYK luminosity
Meter), light transmittance is 93% (400nm~1000nm wave band), haze value 12；It is thin after being rubbed 2500 times with the steel wool of 1kg pressure
Film has good wearability without obvious damage.
Example IV：The preparation of high grade of transparency glass
The preparation method of the high grade of transparency glass of the present embodiment is as follows：
The preparation of graphene oxide, in ice-water bath, by 1.2g natural flake graphites after microwave expansion is handled, add
In the mixed solution of the 85mL concentrated sulfuric acids and 15mL phosphoric acid, stirring is abundant, adds 6gKMnO4, 30min is stirred, oil bath heating is extremely
35 DEG C of stirring 2h, 90 DEG C of stirring 1.5h are again heated to, the H that volumetric concentration is 10% is then slowly added dropwise2O2The aqueous solution, drip
Bi Hou, it is transferred in supercentrifuge to be centrifuged under 7000r/min rotating speed, obtained sediment is with 1mol/L's
HCl solution washs, then is washed with deionized to pH=5.5, vacuum freeze drying and obtains graphene oxide, dense in every liter of volume
Spend in the ethanol solution for 80% and add 0.4g graphene oxides ultrasonic disperse formation graphene oxide dispersion, in 2 DEG C~5 DEG C
Stored under environment.
SiO2The preparation of masking liquid, the SiO for taking the embodiment one that percetage by weight is 2% to prepare2Gel, 90% ethanol and
8% petroleum ether mixes, and obtains SiO2Masking liquid, temperature is stored in as in 2 DEG C~5 DEG C environment.
The formation of graphene oxide film, the glass baseplate through Surface Treatment with Plasma is placed on to the substrate frame of film balance
On, deionized water is added to glass baseplate is covered completely, and 1mL graphene oxide dispersions are slowly added dropwise by micro syringe,
1.5h is stood, until graphene oxide is evenly dispersed in deionized water surface, with the slow membrane of 10mm/min speed by oxygen
Graphite alkene adheres on the glass substrate, after being repeatedly injected graphene oxide dispersion and membrane 3 times, is done in 90 DEG C of baking oven
Dry 6h, obtains graphene oxide film on the glass substrate.
SiO2The formation of film, SiO is carried out in 25 DEG C of temperature, the environment of relative humidity 65%2The spraying of masking liquid, use
Flush coater is by SiO2Masking liquid mixes with the pressure-air in nozzle, squeezes out superfine atomizing particle, and flush coater X-axis translational speed is
400mm/s, and with 7cc/min quantity for spray and 3kg/cm2Spraying swath pressure under, by SiO2Masking liquid even application is in graphite oxide
On alkene film, it is put into tube furnace, is warming up to 250 DEG C in air atmosphere with 3 DEG C/min speed, be heat-treated 5h, stands cold
But, that is, obtain surface and have graphene film and SiO2The high grade of transparency glass of film.
Performance detection is carried out to high grade of transparency glass manufactured in the present embodiment, the thickness for detecting graphene film is
12nm.SiO by transmission electron microscope to glass surface2Film is scanned, and finds SiO2The surface of film presents concavo-convex
Uneven micro-structural, has the function that anti-dazzle.In addition, the glossiness for measuring the high grade of transparency glass of the present embodiment is 80 (BYK
Photometer), light transmittance is 95% (400nm~1000nm wave band), haze value 11；Rubbed 2600 times with the steel wool of 1kg pressure
Afterwards, film has good wearability without obvious damage.
Embodiment five：The preparation of high grade of transparency glass
The preparation method of the high grade of transparency glass of the present embodiment is as follows：
The preparation of graphene oxide, in ice-water bath, after the processing of 1.1g natural flake graphites microwave expansion, add 85mL
In the mixed solution of the concentrated sulfuric acid and 15mL phosphoric acid, stirring is abundant, adds 6gKMnO4, 30min is stirred, oil bath heating is to 35 DEG C
2h is stirred, 90 DEG C of stirring 1.5h is again heated to, the H that volumetric concentration is 10% is then slowly added dropwise2O2The aqueous solution, after being added dropwise,
It is transferred in supercentrifuge to be centrifuged under 8000r/min rotating speed, obtained sediment 1mol/L HCl solution
Washing, then is washed with deionized to pH=6, vacuum freeze drying and obtains graphene oxide, in every liter of volumetric concentration be 80%
Ethanol solution in add 0.4g graphene oxides ultrasonic disperses and form graphene oxide dispersion, stored up under 2 DEG C~5 DEG C environment
Deposit.
SiO2The preparation of masking liquid, the SiO for taking the embodiment two that percetage by weight is 4% to prepare2Gel, 90% ethanol and
6% petroleum ether mixes, and obtains SiO2Masking liquid, temperature is stored in as in 2 DEG C~5 DEG C environment.
The formation of graphene oxide film, the glass baseplate through Surface Treatment with Plasma is placed on to the substrate frame of film balance
On, deionized water is added to glass baseplate is covered completely, and 1mL graphene oxide dispersions are slowly added dropwise by micro syringe,
2.0h is stood, until graphene oxide is evenly dispersed in deionized water surface, with the slow membrane of 12mm/min speed by oxygen
Graphite alkene adheres on the glass substrate, after being repeatedly injected graphene oxide dispersion and membrane 6 times, is done in 95 DEG C of baking oven
Dry 6h, obtains graphene oxide film on the glass substrate.
SiO2The formation of film, SiO is carried out in 28 DEG C of temperature, the environment of relative humidity 60%2The spraying of masking liquid, use
Flush coater is by SiO2Masking liquid mixes with the pressure-air in nozzle, squeezes out superfine atomizing particle, and flush coater X-axis translational speed is
600mm/s, and with 5cc/min quantity for spray and 3kg/cm2Spraying swath pressure under, by SiO2Masking liquid even application is in graphite oxide
On alkene film, it is put into tube furnace, is warming up to 350 DEG C in air atmosphere with 3 DEG C/min speed, be heat-treated 5h, stands cold
But, that is, obtain having graphene film and SiO2The high grade of transparency glass of film.
Performance detection is carried out to high grade of transparency glass manufactured in the present embodiment, the thickness for detecting graphene film is 8nm.
SiO by transmission electron microscope to glass surface2Film is scanned, and finds SiO2The surface of film presents uneven
Micro-structural, there is anti-dazzle.In addition, the glossiness for measuring the high grade of transparency glass of the present embodiment is 78 (BYK luminosity
Meter), light transmittance is 92% (400nm~1000nm wave band), haze value 10；It is thin after being rubbed 2500 times with the steel wool of 1kg pressure
Film has good wearability without obvious damage.
Embodiment six：The preparation of high grade of transparency glass
The preparation method of the high grade of transparency glass of the present embodiment is as follows：
The preparation of graphene oxide, in ice-water bath, by 1g natural flake graphites after microwave expansion is handled, add 85mL
In the mixed solution of the concentrated sulfuric acid and 15mL phosphoric acid, stirring is abundant, adds 6gKMnO4, 30min is stirred, oil bath heating is to 35 DEG C
2h is stirred, 90 DEG C of stirring 1.5h is again heated to, the H that volumetric concentration is 10% is then slowly added dropwise2O2The aqueous solution, after being added dropwise,
It is transferred in supercentrifuge to be centrifuged under 8500r/min rotating speed, obtained sediment 1mol/L HCl solution
Washing, then be washed with deionized to pH=6.5, vacuum freeze drying and obtain graphene oxide, it is in every liter of volumetric concentration
0.4g graphene oxides ultrasonic disperse is added in 80% ethanol solution and forms graphene oxide dispersion, in 2 DEG C~5 DEG C environment
Lower storage.
SiO2The preparation of masking liquid, the SiO for taking the embodiment two that percetage by weight is 3% to prepare2Gel, 82% ethanol and
15% petroleum ether mixes, and obtains SiO2Masking liquid, temperature is stored in as in 2 DEG C~5 DEG C environment.
The formation of graphene oxide film, the glass baseplate through Surface Treatment with Plasma is placed on to the substrate frame of film balance
On, deionized water is added to glass baseplate is covered completely, and 1mL graphene oxide dispersions are slowly added dropwise by micro syringe,
3h is stood, until graphene oxide is evenly dispersed in deionized water surface, will be aoxidized with the slow membrane of 13mm/min speed
Graphene adheres on the glass substrate, after being repeatedly injected graphene oxide dispersion and membrane 8 times, is dried in 95 DEG C of baking oven
6h, graphene oxide film is obtained on the glass substrate.
SiO2The formation of film, SiO is carried out in 0 DEG C of temperature, the environment of relative humidity 60%2The spraying of masking liquid, using spray
Painting machine is by SiO2Masking liquid mixes with the pressure-air in nozzle, squeezes out superfine atomizing particle, and flush coater X-axis translational speed is
500mm/s, and with 5cc/min quantity for spray and 3kg/cm2Spraying swath pressure under, by SiO2Masking liquid even application is in graphite oxide
On alkene film, it is put into tube furnace, is warming up to 250 DEG C~350 DEG C in air atmosphere with 3 DEG C/min speed, is heat-treated 5h,
Cooling is stood, that is, obtains surface and has graphene film and SiO2The high grade of transparency glass of film.
Performance detection is carried out to high grade of transparency glass manufactured in the present embodiment, the thickness for detecting graphene film is
10nm.SiO by transmission electron microscope to glass surface2Film is scanned, and finds SiO2The surface of film presents concavo-convex
Uneven micro-structural, has the function that anti-dazzle.In addition, the glossiness for measuring the high grade of transparency glass of the present embodiment is 77 (BYK
Photometer), light transmittance is 93% (400nm~1000nm wave band), haze value 11；Rubbed 2500 times with the steel wool of 1kg pressure
Afterwards, film has good wearability without obvious damage.
The above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to preferred embodiment to this hair
It is bright to be described in detail, it will be understood by those within the art that, technical scheme can be modified
Or equivalent substitution, without departing from the objective and scope of technical solution of the present invention, it all should cover the claim in the present invention
Among scope.The present invention be not described in detail technology, shape, construction part be known technology.
Claims (9)
1. a kind of high grade of transparency glass for touch-screen, it is characterised in that including clear glass substrate, and be in turn attached to
Graphene film and SiO on glass baseplate2Film, the thickness of the graphene film is 5nm~12nm, the SiO2Film
Surface has rough micro-structural.
2. a kind of high grade of transparency glass for touch-screen according to claim 1, it is characterised in that the graphene is thin
Film is to be formed on the glass substrate using liquid level sedimentation dry solidification, the SiO2Film is by SiO2Masking liquid is sprayed on stone
Dry solidification is formed on black alkene film.
A kind of 3. high grade of transparency glass for touch-screen according to claim 2, it is characterised in that the SiO2Masking liquid
Including 2%~5% SiO2Gel, 82%~90% ethanol and 6%~15% petroleum ether.
A kind of 4. preparation method of high grade of transparency glass for touch-screen according to claim 3, it is characterised in that bag
Include following steps：
The preparation of graphene oxide, in ice-water bath by natural flake graphite after microwave expansion is handled, it is 17 to add volume ratio:3
The concentrated sulfuric acid and phosphoric acid mixed solution in, stirring is abundant, adds KMnO4, stir 30min, oil bath heating to 35 DEG C of stirrings
2h, 90 DEG C of stirring 1.5h are again heated to, the dense degree of volume is then slowly added dropwise as 10% H2O2The aqueous solution, after being added dropwise, turn
Enter and sediment is centrifugally separating to obtain in supercentrifuge, sediment is washed with HCl solution, then is washed with deionized to pH=
5.5~6.5, vacuum freeze drying obtains graphene oxide, and 0.4g is added in the ethanol solution that every liter of volumetric concentration is 80%
Graphene oxide ultrasonic disperse forms graphene oxide dispersion, is stored under 2 DEG C~5 DEG C environment；
SiO2The preparation of masking liquid, takes SiO2Gel adds the in the mixed solvent stirring of petroleum ether and ethanol, obtains SiO2Masking liquid, storage
Temperature is stored in as in 2 DEG C~5 DEG C environment；
The formation of graphene oxide film, the glass baseplate through Surface Treatment with Plasma is placed on the substrate frame of film balance,
Deionized water is added, 1mL graphene oxide dispersions are slowly added dropwise, 1.5h~3h is stood, with 10mm/min~13mm/min's
The slow membrane of speed adheres to graphene oxide on the glass substrate, is repeatedly injected graphene oxide dispersion simultaneously membrane 3~8 times
Afterwards, in 80 DEG C~95 DEG C dry 6h, i.e., graphene oxide film is obtained on the glass substrate；
SiO2The formation of film, using flush coater by SiO2Masking liquid mixes with the pressure-air in nozzle, in 3kg/cm2Spraying swath
Pressure even application is put into tube furnace on graphene oxide film, is warming up in air atmosphere with 3 DEG C/min speed
250 DEG C~350 DEG C, 5h is heat-treated, cooling is stood, that is, obtains having graphene film and SiO2The high grade of transparency glass of film.
A kind of 5. preparation method of high grade of transparency glass for touch-screen according to claim 4, it is characterised in that institute
The rotating speed for stating centrifuge in the preparation process of graphene oxide is 7000r/min~8500r/min.
A kind of 6. preparation method of high grade of transparency glass for touch-screen according to claim 5, it is characterised in that institute
State SiO2The preparation method of gel is as follows：Water intaking glass and deionized water press 1:5.0 mass ratio mixes 10min, adds
Pentaerythrite is stirred to whole dissolvings, is added second acid for adjusting pH to 6.2~6.8, after stirring 20min, is stood 2h, obtain SiO2It is wet
Gel, by SiO2Wet gel is transferred to aging 72h in 40 DEG C~50 DEG C baking boxs, and taking-up is put into progress solvent displacement in ethanol solution,
Place into soak in hydrophobic modifier HMDO and be modified, carried out once every 6h, it is molten with ethanol after carrying out 5 times altogether
Liquid washs, and in 65 DEG C of dry 18h, obtains SiO2Gel.
A kind of 7. preparation method of high grade of transparency glass for touch-screen according to claim 6, it is characterised in that institute
The addition for stating pentaerythrite is the 4.5% of waterglass quality.
A kind of 8. preparation method of high grade of transparency glass for touch-screen according to claim 7, it is characterised in that institute
State SiO2Sprayed in the forming step of film in 25 DEG C~30 DEG C of temperature, the environment of relative humidity 55%~65%.
A kind of 9. preparation method of high grade of transparency glass for touch-screen according to claim 8, it is characterised in that institute
State SiO2The quantity for spray of masking liquid is 4cc/min~7cc/min, and flush coater X-axis translational speed is 400mm/s~600mm/s.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102750998A (en) * | 2012-07-09 | 2012-10-24 | 深圳市贝特瑞纳米科技有限公司 | Transparent graphene conductive thin film and preparation method thereof |
| CN203276243U (en) * | 2013-05-17 | 2013-11-06 | 福建省辉锐材料科技有限公司 | Arc-shaped capacitive touch screen |
| CN106630667A (en) * | 2015-11-02 | 2017-05-10 | 夏成盛 | An anti-glare (AG) glass processing process adopting silicon oxide sedimentation |
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2017
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102750998A (en) * | 2012-07-09 | 2012-10-24 | 深圳市贝特瑞纳米科技有限公司 | Transparent graphene conductive thin film and preparation method thereof |
| CN203276243U (en) * | 2013-05-17 | 2013-11-06 | 福建省辉锐材料科技有限公司 | Arc-shaped capacitive touch screen |
| CN106630667A (en) * | 2015-11-02 | 2017-05-10 | 夏成盛 | An anti-glare (AG) glass processing process adopting silicon oxide sedimentation |
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