CN113087408A - Ceramic-like glass plate and preparation method thereof - Google Patents
Ceramic-like glass plate and preparation method thereof Download PDFInfo
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- CN113087408A CN113087408A CN202110354878.5A CN202110354878A CN113087408A CN 113087408 A CN113087408 A CN 113087408A CN 202110354878 A CN202110354878 A CN 202110354878A CN 113087408 A CN113087408 A CN 113087408A
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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
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- 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
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
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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
- C03C17/3435—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 a nitride, oxynitride, boronitride or carbonitride
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- 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
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/0021—Reactive sputtering or evaporation
- C23C14/0036—Reactive sputtering
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/021—Cleaning or etching treatments
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
- C23C14/0611—Diamond
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0641—Nitrides
- C23C14/0652—Silicon nitride
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0676—Oxynitrides
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/10—Glass or silica
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/12—Organic material
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- 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
- C03C2218/15—Deposition methods from the vapour phase
- C03C2218/154—Deposition methods from the vapour phase by sputtering
Abstract
The utility model provides an imitative ceramic glass board, includes the glass substrate layer, has the colour printing ink layer at the one side spraying on the glass substrate layer, has plated the transparent hard coating that adds of silicon nitride, DLC rete and AF rete in proper order at the another side on the glass substrate layer, and the transparent hard coating that adds of silicon nitride includes the silica layer, is equipped with several layers of silicon nitride layer and several layers of silicon oxynitride layer on the silica layer in proper order, and silicon nitride layer and silicon oxynitride layer adopt the mutual layer mode setting in interval. During preparation, the coating is cleaned, sprayed with color ink, dried and cleaned again, then a silicon nitride transparent hard coating film is plated under certain conditions, and finally a DLC film and an AF film are sequentially plated. According to the invention, the silicon oxynitride is adopted to meet the optical design requirement of low-refraction superposition high-refractive index, and the oxygen/nitrogen ratio is controlled during the preparation of the silicon oxynitride layer, so that the problems of poor hardness and poor color matching of the ceramic-like decorative coating on the surface of the rear cover plate of the mobile phone are solved.
Description
Technical Field
The invention belongs to the technical field of vacuum sputtering ceramic-like coating, and particularly relates to a ceramic-like glass plate and a preparation method thereof.
Background
At present, the surface decorative films and antireflection films in the industries of mobile phone glass cover plates and touch screens are all glare films and AR films formed by overlapping silicon nitride (SI 3N4) and silicon oxide (SIO 2), the problem of poor film hardness (the surface hardness of common glass is 8G Pa, and the nano hardness of the common film is less than 12G Pa) exists, and the films are easily scratched by being contacted with hard objects such as keys, cosmetic shells, coins and the like in daily life. As the number of scratches increases, the appearance and performance of the product are affected as shown in fig. 1. In addition, researchers can achieve the expected color effect by superposing a color film by titanium pentoxide and silicon dioxide and then plating a DLC layer and an AF layer, but the problems of film falling and intensive scratching can occur after vibration and friction.
Disclosure of Invention
The invention aims to provide a ceramic-like glass plate and a preparation method thereof, and solves the problems of poor hardness and poor color matching of a ceramic-like decorative coating film on the surface of a rear cover plate of a mobile phone.
The technical scheme adopted by the invention is as follows:
the utility model provides an imitative ceramic glass board, includes the glass substrate layer, has the colour printing ink layer at the one side spraying of glass substrate layer, has plated the transparent hard coating that adds of silicon nitride, DLC rete and AF rete in proper order at the another side on glass substrate layer, the transparent hard coating that adds of silicon nitride includes the silica layer, is equipped with several layers of silicon nitride layer and several layers of silicon oxynitride layer on the silica layer in proper order, and silicon nitride layer and silicon oxynitride layer adopt the setting of interval interbedded mode (be one deck silicon nitride earlier promptly, plate one deck silicon oxynitride again, repeated many times).
Furthermore, the number of layers of the silicon nitride layer is 3-8, and the number of layers of the silicon oxynitride layer is 3-8.
Furthermore, the thickness of the single layer of the silicon nitride layer is 30-300 nanometers, and the thickness of the single layer of the silicon oxynitride layer is 15-100 nanometers.
Further, the thickness of the color printing ink layer is 15-25 microns.
Further, the color of the color ink layer is one of black, green, blue, white and red.
A preparation method of a ceramic-like glass plate comprises the following steps:
the method comprises the following steps: immersing glass in pure water, cleaning by ultrasonic waves (the ultrasonic frequency is 40KHZ, and the current is 2A-2.5A) for 30-40 min, and then drying by using hot air at 120 ℃;
step two: spraying colored ink with the thickness of 15-25 microns on one surface of the glass by using an ink-jet machine;
step three: putting the glass sprayed with the ink into an oven, and baking for 60min at 150 ℃;
step four: cleaning the glass with the ink solidified in the third step by adopting the first step again, and manually checking after cleaning (requiring that the non-ink-jet surface is free from dirt, scratches and the like);
step five: fixing the cleaned glass in the fourth step on a film coating machine (HOLDER plate) by using a high-temperature adhesive tape (capable of resisting 120 ℃ and not dropping the adhesive) to perform film coating;
step six: when the vacuum degree of a film coating machine reaches 0.00085 Pa, a silicon target/ICP (oxidation source) starts to work, meanwhile, oxygen, argon and nitrogen are injected, in the process, a 20-60 nanometer silicon dioxide layer is firstly manufactured (set by a machine) as a connecting layer, single-layer nanometer silicon oxynitride is prepared (set by the machine), then a single-layer nanometer silicon nitride film layer is prepared, the two materials are repeatedly and alternately superposed, and when the number of the film layers set by the machine is reached, the film coating of the silicon nitride transparent hardening layer is finished;
step seven: after the operation of the sixth step is finished, the carbon target starts to plate the DLC film layer, nano-scale carbon atoms are sputtered and deposited on the outer surface of the silicon nitride transparent hardened layer, the deposition rate of the carbon atoms is controlled to be 0.05 nm/s-0.1 nm/s, and the thickness of the DLC film layer is 3-5 nm;
step eight: and (4) plating an AF film layer with the thickness of 20-30 nanometers on the outer surface of the DLC film layer in the step seven by using an evaporation method, wherein the AF film layer is made of perfluoropolyether siloxane.
Further, in the sixth step, when the nano silicon dioxide (SIO 2) layer is manufactured, the power of the silicon target is 12-15KW, and the flow of the silicon target sputtering argon is 300-; the power of an oxidation source (ICP) is 2.5-5KW, and the injection flow ratio of the argon and the oxygen for reaction is as follows: 50-200 SCCM: 600-1000 SCCM; when silicon nitride (SI 3N4) is prepared, the power of a silicon target is 12-15KW, the flow of argon for sputtering the silicon target is 120-400SCCM, the power of an oxidation source (ICP) is 2.5-5KW, and the injection flow ratio of the argon and the nitrogen for reaction is as follows: 50-200 SCCM: 200-300 SCCM; when silicon oxynitride (SION) is prepared, the power of a silicon target is 12-15KW, the flow of silicon target sputtering argon is 120-400SCCM, the power of an oxidation source (ICP) is 2.5-5KW, and the injection flow ratio of oxygen, nitrogen and argon in reaction is as follows: 100-160 SCCM: 200-300 SCCM: 50-200 SCCM.
Further, when the DLC film is manufactured in the seventh step, the power of the carbon target is 6-15KW, and the injection flow of the sputtering argon of the target is as follows: 200-400 SCCM; the power of an oxidation source (ICP) is 0.5-1KW, and the flow of argon is 50-150 SCCM.
Furthermore, the purity of the silicon target and the purity of the DLC (carbon target) target are both more than 99.99 percent; the purity of oxygen, argon and nitrogen reaches more than 99.999 percent.
Further, in the step eight, the vacuum degree of the evaporated AF is below 0.002 Pa, the ion source is cleaned for 20-200 seconds, and the power of the ion source is as follows: the device comprises 16-20A of neutralization current, 250MA of ion beam current, 300MA of electron beam current, 200-250V of acceleration voltage, 350V of screen electrode voltage, 1-20A of acceleration current, 9-11A of cathode current, 60-90V of anode voltage and 2-4A of anode current.
The invention has the beneficial effects that:
the invention utilizes a relaxation sputtering (NSC-2350 DL) machine to realize a high-compactness silicon nitride/silicon oxynitride film layer, so that the nano hardness of the film layer on the surface of the glass reaches more than 18 Gpa, and simultaneously utilizes the characteristic of high refraction and high hardness of silicon nitride (SI 3N4) to overlap a low-refractive-index high-hardness silicon oxynitride (SION) film material to plate a film on the surface of the glass, the reflection/transmission color is nearly colorless, the A value is 0 +/-5, the B value is 0 +/-5 as the reflection curve of a graph 2, and any color effect (such as ceramic black, ceramic green, ceramic blue, ceramic white, ceramic red and other appearance effects) can be matched with the back color ink. The color of the surface coating film is not influenced by the reflection of the glass, thereby achieving the effect of imitating ceramic. And finally, DLC + AF plating is added on the surface of the film layer to ensure that the surface of the glass is better protected, and the film layer can not fall off and be densely scratched after a vibration friction instrument is used for 150 minutes (the vibration friction condition refers to a lower page test report), as shown in figure 3. The invention is used for the rear cover plate of the mobile phone, and can solve the problems of poor hardness and poor color matching of the imitation ceramic decorative coating film on the surface of the rear cover plate of the mobile phone.
The invention mainly adopts silicon oxynitride (SION) to replace silicon oxide with low refractive index to meet the requirement of optical design and improve the hardness. To meet the requirement of low-refractive-index and high-refractive-index optical design, the refractive index of silicon oxynitride is less than 1.75, which is one of the innovative points in material selection. In addition, the silicon oxynitride layer is prepared under the condition that the oxygen/nitrogen ratio charged in the reaction of the oxidation source (ICP) must be in the following range: oxygen flow rate (100-: nitrogen flow (200- & lt300- & gt) SCCM.
Drawings
Fig. 1 is a picture of a glass plate manufactured by the conventional common process, which is subjected to vibration friction to generate dense scratches.
FIG. 2 is a graph of reflectance versus wavelength.
FIG. 3 is a picture of a ceramic-like glass plate prepared by the process of the present invention after vibration rubbing (no obvious scratch).
FIG. 4 is a structural diagram of a ceramic-like glass plate prepared according to the present invention.
FIG. 5 is a screenshot of a test effect report of a coated ceramic-like glass plate prepared according to the present invention.
Detailed Description
Example 1
As shown in fig. 4, a ceramic-like glass plate comprises a glass substrate layer, wherein a 15-micron black ink layer is sprayed on one surface of the glass substrate layer, a silicon nitride transparent hard layer, a DLC film layer and an AF film layer are sequentially plated on the other surface of the glass substrate layer, the silicon nitride transparent hard layer comprises a silicon dioxide layer, 3 silicon nitride layers and 3 silicon oxynitride layers are sequentially arranged on the silicon dioxide layer, the silicon nitride layers and the silicon oxynitride layers are arranged in an interval mutual layer mode (namely, one layer of silicon nitride is firstly plated, and then one layer of silicon oxynitride is plated, and the repetition is repeated for multiple times), the single-layer thickness of the silicon nitride layer is 300 nanometers, and the single-layer thickness of the silicon oxynitride layer is 100 nanometers.
A method of making a ceramic-like glass sheet comprising the steps of:
the method comprises the following steps: immersing glass in pure water, cleaning with ultrasonic wave (ultrasonic frequency is 40KHZ, current is 2A-2.5A), drying with 120 deg.C hot air after 30 min;
step two: spraying colored ink on one surface of the glass by using an ink-jet machine;
step three: putting the glass sprayed with the ink into an oven, and baking for 60min at 150 ℃;
step four: cleaning the glass with the ink solidified in the third step by adopting the first step again, and manually checking after cleaning (requiring that the non-ink-jet surface is free from dirt, scratches and the like);
step five: fixing the cleaned glass on a film plating machine (HOLDER plate) by using a high-temperature adhesive tape (capable of resisting 120 ℃ and not dropping the adhesive);
step six: when the vacuum degree of a film coating machine reaches 0.00085 Pa, a silicon target/ICP (oxidation source) starts to work, meanwhile, oxygen, argon and nitrogen are injected, in the process, a 20-nanometer silicon dioxide layer is firstly manufactured (set by a machine) as a connecting layer, single-layer nanometer silicon oxynitride is prepared (set by the machine), then a single-layer nanometer silicon nitride film layer is prepared, the two materials are repeatedly and alternately superposed, and when the number of the film layers set by the machine is reached, the film coating of the transparent and hard silicon nitride layer is finished;
when the nano silicon dioxide (SIO 2) layer is manufactured, the power of a silicon target is 12KW, and the flow of sputtering argon of the silicon target is 300 SCCM; the power of an oxidation source (ICP) is 2.5KW, and the injection flow ratio of the argon to the oxygen for reaction is as follows: 50 SCCM: 600 SCCM;
when the silicon nitride (SI 3N4) layer is made, the silicon target power is 12KW, the silicon target sputtering argon flow is 120SCCM, the oxidation source (ICP) power is 2.5KW, and the injection flow ratio of the argon and nitrogen of the reaction is as follows: 50 SCCM: 200 SCCM;
when the silicon oxynitride (SION) layer is manufactured, the power of a silicon target is 12KW, the flow of argon for sputtering the silicon target is 120SCCM, the power of an oxidation source (ICP) is 2.5KW, and the injection flow proportion of oxygen, nitrogen and argon for reaction is as follows: 100 SCCM: 200 SCCM: 50 SCCM.
Step seven: after the operation of the sixth step is finished, the carbon target starts to work, nano-scale carbon atoms are sputtered and deposited on the outer surface of the silicon nitride transparent hardened layer, the deposition rate of the carbon atoms is controlled to be 0.05nm/s, and the thickness of the DLC film layer is 3 nanometers; when the DLC film is manufactured, the power of a carbon target is 6KW, and the injection flow of sputtering argon of the target is as follows: 200 SCCM; oxidation source (ICP) power 0.5KW, argon flow 50 SCCM.
Step eight: and (4) plating an AF film layer with the thickness of 20 nanometers on the outer surface of the DLC film layer in the step seven by using an evaporation method, wherein the AF film layer is made of perfluoropolyether siloxane. The vacuum degree of the evaporated AF is below 0.002 Pa, the ion source is cleaned for 20 seconds, and the power of the ion source is as follows: the neutralization current is 16A, the ion beam current is 250MA, the electron beam current is 300MA, the acceleration voltage is 200V, the screen electrode voltage is 350V, the acceleration current is 5A, the cathode current is 9A, the anode voltage is 60V, and the anode current is 2A.
The purity of the silicon target and the purity of the DLC (carbon target) target are both more than 99.99 percent; the purity of oxygen, argon and nitrogen is more than 99.999. The model of the photorelaxation sputtering machine is (NSC-2350 DL) or (NSC-1650 DL).
Example 2
As shown in fig. 4, a ceramic-like glass plate comprises a glass substrate layer, wherein a 20 micron green ink layer is sprayed on one surface of the glass substrate layer, a silicon nitride transparent hard layer, a DLC film layer and an AF film layer are sequentially plated on the other surface of the glass substrate layer, the silicon nitride transparent hard layer comprises a silicon dioxide layer, 5 silicon nitride layers and 5 silicon oxynitride layers are sequentially arranged on the silicon dioxide layer, the silicon nitride layers and the silicon oxynitride layers are arranged in an interval mutual layer mode (namely, one silicon nitride layer is firstly plated, and then one silicon oxynitride layer is plated for a plurality of times), the single-layer thickness of the silicon nitride layers is 200 nanometers, and the single-layer thickness of the silicon oxynitride layers is 70 nanometers.
A method of making a ceramic-like glass sheet comprising the steps of:
the method comprises the following steps: immersing glass in pure water, cleaning with ultrasonic wave (ultrasonic frequency is 40KHZ, current is 2A-2.5A), drying with 120 deg.C hot air after 30 min;
step two: spraying colored ink on one surface of the glass by using an ink-jet machine;
step three: putting the glass sprayed with the ink into an oven, and baking for 60min at 150 ℃;
step four: cleaning the glass with the ink solidified in the third step by adopting the first step again, and manually checking after cleaning (requiring that the non-ink-jet surface is free from dirt, scratches and the like);
step five: fixing the cleaned glass on a film plating machine (HOLDER plate) by using a high-temperature adhesive tape (capable of resisting 120 ℃ and not dropping the adhesive);
step six: when the vacuum degree of a film coating machine reaches 0.00085 Pa, a silicon target/ICP (oxidation source) starts to work, meanwhile, oxygen, argon and nitrogen are injected, in the process, a 40-nanometer silicon dioxide layer is firstly manufactured (set by a machine) as a connecting layer, single-layer nanometer silicon oxynitride is prepared (set by the machine), then a single-layer nanometer silicon nitride film layer is prepared, the two materials are repeatedly and alternately superposed, and when the number of the film layers set by the machine is reached, the film coating of the transparent and hard silicon nitride layer is finished;
when the nano silicon dioxide (SIO 2) layer is manufactured, the power of a silicon target is 12KW, and the flow of sputtering argon of the silicon target is 400 SCCM; the power of an oxidation source (ICP) is 2.5KW, and the injection flow ratio of the argon to the oxygen for reaction is as follows: 100 SCCM: 800 SCCM;
when the silicon nitride (SI 3N4) layer is manufactured, the power of a silicon target is 15KW, the flow of argon for sputtering the silicon target is 200SCCM, the power of an oxidation source (ICP) is 2.5) KW, and the injection flow ratio of the argon and the nitrogen for reaction is as follows: 100 SCCM: 220 SCCM;
when the silicon oxynitride (SION) layer is manufactured, the power of a silicon target is 15KW, the flow of argon for sputtering the silicon target is 200SCCM, the power of an oxidation source (ICP) is 5KW, and the injection flow proportion of oxygen, nitrogen and argon for reaction is as follows: 120 SCCM: 230 SCCM: 100 SCCM.
Step seven: after the operation of the sixth step is finished, the carbon target starts to work, nano-scale carbon atoms are sputtered and deposited on the outer surface of the silicon nitride transparent hardened layer, the deposition rate of the carbon atoms is controlled to be 0.06nm/s, and the thickness of the DLC film layer is 4 nanometers; when the DLC film is manufactured, the power of a carbon target is 8KW, and the injection flow of sputtering argon of the target is as follows: 300 SCCM; oxidation source (ICP) power 0.5KW, argon flow 90 SCCM.
Step eight: and (4) plating an AF film layer with the thickness of 25 nanometers on the outer surface of the DLC film layer in the step seven by using an evaporation method, wherein the AF film layer is made of perfluoropolyether siloxane. The vacuum degree of the evaporated AF is below 0.002 Pa, the ion source is cleaned for 100 seconds, and the power of the ion source is as follows: neutralization current 18A, ion beam current 250MA, electron beam current 300MA, acceleration voltage 200V, screen electrode voltage 350V, acceleration current 10A, cathode current 10A, anode voltage 70V and anode current 3A.
The purity of the silicon target and the purity of the DLC (carbon target) target are both more than 99.99 percent; the purity of oxygen, argon and nitrogen is more than 99.999. The model of the photorelaxation sputtering machine is (NSC-2350 DL) or (NSC-1650 DL).
Example 3
As shown in fig. 4, a ceramic-like glass plate comprises a glass substrate layer, wherein a 25-micron blue ink layer is sprayed on one surface of the glass substrate layer, a silicon nitride transparent hard layer, a DLC film layer and an AF film layer are sequentially plated on the other surface of the glass substrate layer, the silicon nitride transparent hard layer comprises a silicon dioxide layer, 6 silicon nitride layers and 6 silicon oxynitride layers are sequentially arranged on the silicon dioxide layer, and the silicon nitride layers and the silicon oxynitride layers are arranged in an interval mutual layer mode (namely, one layer of silicon nitride is firstly plated, and then one layer of silicon oxynitride is plated, and the process is repeated for multiple times). The single-layer thickness of the silicon nitride layer is 100 nanometers, and the single-layer thickness of the silicon oxynitride layer is 40 nanometers.
A method of making a ceramic-like glass sheet comprising the steps of:
the method comprises the following steps: immersing glass in pure water, and ultrasonic cleaning (ultrasonic frequency is 40KHZ, current is 2A-2.5A, time is 40min, and then drying with 120 deg.C hot air;
step two: spraying colored ink on one surface of the glass by using an ink-jet machine;
step three: putting the glass sprayed with the ink into an oven, and baking for 60min at 150 ℃;
step four: cleaning the glass with the ink solidified in the third step by adopting the first step again, and manually checking after cleaning (requiring that the non-ink-jet surface is free from dirt, scratches and the like);
step five: fixing the cleaned glass on a film plating machine (HOLDER plate) by using a high-temperature adhesive tape (capable of resisting 120 ℃ and not dropping the adhesive);
step six: when the vacuum degree of a film coating machine reaches 0.00085 Pa, a silicon target/ICP (oxidation source) starts to work, meanwhile, oxygen, argon and nitrogen are injected, in the process, a 50-nanometer silicon dioxide layer is firstly manufactured (set by a machine) as a connecting layer, single-layer nanometer silicon oxynitride is prepared (set by the machine), then a single-layer nanometer silicon nitride film layer is prepared, the two materials are repeatedly and alternately superposed, and when the number of the film layers set by the machine is reached, the film coating of the transparent and hard silicon nitride layer is finished;
when the nano silicon dioxide (SIO 2) layer is manufactured, the power of a silicon target is 15KW, and the flow of sputtering argon of the silicon target is 500 SCCM; the power of an oxidation source (ICP) is 5KW, and the injection flow ratio of the argon and the oxygen for reaction is as follows: 150 SCCM: 900 SCCM;
when the silicon nitride (SI 3N4) layer is manufactured, the silicon target power is 15KW, the silicon target sputtering argon flow is 300SCCM, the oxidation source (ICP) power is 5KW, and the injection flow ratio of the argon and the nitrogen for reaction is as follows: 150 SCCM: 250 SCCM;
when the silicon oxynitride (SION) layer is manufactured, the power of a silicon target is 12KW, the flow of argon for sputtering the silicon target is 300SCCM, the power of an oxidation source (ICP) is 2.5KW, and the injection flow proportion of oxygen, nitrogen and argon for reaction is as follows: 140 SCCM: 260 SCCM: 150 SCCM.
Step seven: after the operation of the sixth step is finished, the carbon target starts to work, nano-scale carbon atoms are sputtered and deposited on the outer surface of the silicon nitride transparent hardened layer, the deposition rate of the carbon atoms is controlled to be 0.08nm/s, and the thickness of the DLC film layer is 5 nanometers; when the DLC film is manufactured, the power of a carbon target is 10KW, and the injection flow of sputtering argon of the target is as follows: 350 SCCM; oxidation source (ICP) power 1KW, argon flow 120 SCCM.
Step eight: and (4) plating an AF film layer with the thickness of 28 nanometers on the outer surface of the DLC film layer in the step seven by using an evaporation method, wherein the AF film layer is made of perfluoropolyether siloxane. The vacuum degree of the evaporated AF is below 0.002 Pa, the ion source is cleaned for 150 seconds, and the power of the ion source is as follows: neutralizing current 20A, ion beam current 250MA, electron beam current 300MA, accelerating voltage 250V, screen electrode voltage 350V, accelerating current 20A, cathode current 11A, anode voltage 90V and anode current 4A.
The purity of the silicon target and the purity of the DLC (carbon target) target are both more than 99.99 percent; the purity of oxygen, argon and nitrogen is more than 99.999. The model of the photorelaxation sputtering machine is (NSC-2350 DL) or (NSC-1650 DL).
Example 4
As shown in fig. 4, a ceramic-like glass plate comprises a glass substrate layer, wherein a 25 micron red ink layer is sprayed on one surface of the glass substrate layer, a silicon nitride transparent hard layer, a DLC film layer and an AF film layer are sequentially plated on the other surface of the glass substrate layer, the silicon nitride transparent hard layer comprises a silicon dioxide layer, 8 silicon nitride layers and 8 silicon oxynitride layers are sequentially arranged on the silicon dioxide layer, and the silicon nitride layers and the silicon oxynitride layers are arranged in an interval mutual layer mode (namely, one layer of silicon nitride is firstly plated, and then one layer of silicon oxynitride is plated, and the process is repeated for multiple times). The thickness of the single layer of the silicon nitride layer is 30 nanometers, and the thickness of the single layer of the silicon oxynitride layer is 15 nanometers.
A method of making a ceramic-like glass sheet comprising the steps of:
the method comprises the following steps: immersing glass in pure water, and ultrasonic cleaning (ultrasonic frequency is 40KHZ, current is 2A-2.5A, time is 40min, and then drying with 120 deg.C hot air;
step two: spraying colored ink on one surface of the glass by using an ink-jet machine;
step three: putting the glass sprayed with the ink into an oven, and baking for 60min at 150 ℃;
step four: cleaning the glass with the ink solidified in the third step by adopting the first step again, and manually checking after cleaning (requiring that the non-ink-jet surface is free from dirt, scratches and the like);
step five: fixing the cleaned glass on a film plating machine (HOLDER plate) by using a high-temperature adhesive tape (capable of resisting 120 ℃ and not dropping the adhesive);
step six: when the vacuum degree of a film coating machine reaches 0.00085 Pa, a silicon target/ICP (oxidation source) starts to work, meanwhile, oxygen, argon and nitrogen are injected, in the process, a 60-nanometer silicon dioxide layer is firstly manufactured (set by a machine) as a connecting layer, single-layer nanometer silicon oxynitride is prepared (set by the machine), then a single-layer nanometer silicon nitride film layer is prepared, the two materials are repeatedly and alternately superposed, and when the number of the film layers set by the machine is reached, the film coating of the transparent and hard silicon nitride layer is finished;
when the nano silicon dioxide (SIO 2) layer is manufactured, the power of a silicon target is 15KW, and the flow of sputtering argon of the silicon target is 600 SCCM; the power of an oxidation source (ICP) is 5KW, and the injection flow ratio of the argon and the oxygen for reaction is as follows: 200 SCCM: 1000 SCCM;
when the silicon nitride (SI 3N4) layer is manufactured, the power of a silicon target is 12KW, the flow of argon for sputtering the silicon target is 400SCCM, the power of an oxidation source (ICP) is 5KW, and the injection flow ratio of the argon and the nitrogen for reaction is as follows: 200 SCCM: 300 SCCM;
when the silicon oxynitride (SION) layer is manufactured, the power of a silicon target is 12KW, the flow of argon for sputtering the silicon target is 400SCCM, the power of an oxidation source (ICP) is 5KW, and the injection flow proportion of oxygen, nitrogen and argon for reaction is as follows: 160 SCCM: 300 SCCM: 200 SCCM.
Step seven: after the operation of the sixth step is finished, the carbon target starts to work, nano-scale carbon atoms are sputtered and deposited on the outer surface of the silicon nitride transparent hardened layer, the deposition rate of the carbon atoms is controlled to be 0.1nm/s, and the thickness of the DLC film layer is 5 nanometers; when the DLC film is manufactured, the power of a carbon target is 15KW, and the injection flow of sputtering argon of the target is as follows: 400 SCCM; oxidation source (ICP) power 1KW, argon flow 150 SCCM.
Step eight: and (4) plating an AF film layer with the thickness of 30 nanometers on the outer surface of the DLC film layer in the step seven by using an evaporation method, wherein the AF film layer is made of perfluoropolyether siloxane. The vacuum degree of the evaporated AF is below 0.002 Pa, the ion source is cleaned for 200 seconds, and the power of the ion source is as follows: neutralizing current 20A, ion beam current 250MA, electron beam current 300MA, accelerating voltage 250V, screen electrode voltage 350V, accelerating current 20A, cathode current 11A, anode voltage 90V and anode current 4A.
The purity of the silicon target and the purity of the DLC (carbon target) target are both more than 99.99 percent; the purity of oxygen, argon and nitrogen is more than 99.999. The model of the photorelaxation sputtering machine is (NSC-2350 DL) or (NSC-1650 DL).
The ceramic-like glass plate prepared in example 4 was subjected to a vibration friction test (see fig. 3) and a professional test (see fig. 5 for effect), and the ceramic-like glass plate was not significantly scratched after the vibration friction test and had a good professional test effect.
Claims (10)
1. The utility model provides an imitative ceramic glass board, its characterized in that includes the glass substrate layer, has the colour printing ink layer at the one side spraying on the glass substrate layer, has plated the transparent hard coating of silicon nitride, DLC rete and AF rete in proper order at the another side on the glass substrate layer, the transparent hard coating of silicon nitride includes the silica layer, is equipped with several layers of silicon nitride layer and several layers of silicon oxynitride layer on the silica layer in proper order, and silicon nitride layer and silicon oxynitride layer adopt the mutual layer mode setting in interval.
2. The ceramic-like glass plate according to claim 1, wherein the number of silicon nitride layers is 3 to 8, and the number of silicon oxynitride layers is 3 to 8.
3. The ceramic-like glass plate according to claim 1, wherein the silicon nitride layer has a single thickness of 30 to 300 nm, and the silicon oxynitride layer has a single thickness of 15 to 100 nm.
4. The ceramic-like glass plate according to claim 1, wherein the thickness of the color ink layer is 15 to 25 μm.
5. The ceramic-like glass plate according to claim 1, wherein the color ink layer has a color selected from the group consisting of black, green, blue, white, and red.
6. A method for producing a ceramic-like glass sheet as claimed in any one of claims 1 to 5, characterized by comprising the steps of:
the method comprises the following steps: immersing glass in pure water, cleaning for 30-40 min by ultrasonic waves, and drying by hot air at 120 ℃;
step two: spraying colored ink on one surface of the glass dried in the step I by using an ink jet machine;
step three: putting the glass sprayed with the ink into an oven, and baking for 60min at 150 ℃;
step four: cleaning the glass with the ink solidified in the third step by adopting the first step again, and manually checking after cleaning to require that the surface without the ink sprayed is free from dirt and scratches;
step five: fixing the cleaned glass in the fourth step on a film coating machine by using a high-temperature adhesive tape for coating;
step six: when the vacuum degree of a film coating machine reaches 0.00085 Pa, a silicon target/ICP starts to work, meanwhile, oxygen, argon and nitrogen are injected, in the process, a silicon dioxide layer with the thickness of 20-60 nanometers is firstly manufactured as a connecting layer, a single-layer nano silicon oxynitride film layer is prepared, a single-layer nano silicon nitride film layer is prepared, the two materials are repeatedly and alternately superposed, and when the number of the film layers set by the machine is reached, the film coating of the silicon nitride transparent hardening layer is finished;
step seven: after the operation of the sixth step is finished, the carbon target starts to plate the DLC film layer, nano-scale carbon atoms are sputtered and deposited on the outer surface of the silicon nitride transparent hardened layer, the deposition rate of the carbon atoms is controlled to be 0.05 nm/s-0.1 nm/s, and the thickness of the DLC film layer is 3-5 nm;
step eight: and (4) plating an AF film layer with the thickness of 20-30 nanometers on the outer surface of the DLC film layer in the step seven by using an evaporation method, wherein the AF film layer is made of perfluoropolyether siloxane.
7. The method for preparing a ceramic-like glass plate according to claim 6, wherein in the sixth step, when the nano silicon dioxide layer is prepared, the power of the silicon target is 12-15KW, and the flow of sputtering argon of the silicon target is 300-600 SCCM; the power of an oxidation source is 2.5-5KW, and the injection flow ratio of the argon and the oxygen for reaction is as follows: 50-200 SCCM: 600-1000 SCCM;
when the silicon nitride is prepared, the power of a silicon target is 12-15KW, the flow of argon for sputtering the silicon target is 120-400SCCM, the power of an oxidation source is 2.5-5KW, and the injection flow ratio of the argon and the nitrogen for reaction is as follows: 50-200 SCCM: 200-300 SCCM;
when the silicon oxynitride is prepared, the power of a silicon target is 12-15KW, the flow of argon for sputtering the silicon target is 120-400SCCM, the power of an oxidation source is 2.5-5KW, and the injection flow proportion of oxygen, nitrogen and argon for reaction is as follows: 100-160 SCCM: 200-300 SCCM: 50-200 SCCM.
8. The method for preparing a ceramic-like glass plate according to claim 6, wherein the power of the carbon target is 6-15KW when the DLC film is prepared in the seventh step, and the injection flow of the argon sputtered from the target is as follows: 200-400 SCCM; the power of the oxidation source is 0.5-1KW, and the flow of argon is 50-150 SCCM.
9. The method for preparing a ceramic-like glass plate according to claim 6, wherein the purity of the silicon target and the purity of the carbon target are both more than 99.99%; the purity of oxygen, argon and nitrogen reaches more than 99.999 percent.
10. The method for producing a ceramic-like glass plate according to claim 6, wherein the vacuum degree of the deposition AF in the eighth step is 0.002 Pa or less, the ion source is cleaned for 20 to 200 seconds, and the power of the ion source is: the ion beam current is 16-20A, the ion beam current is 250MA, the electron beam current is 300MA, the acceleration voltage is 200-250V, the screen electrode voltage is 350V, the acceleration current is 1-20A, the cathode current is 9-11A, the anode voltage is 60-90V, and the anode current is 2-4A.
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