CN115893866B - Method and system for continuously preparing AG film, AR film and AF film - Google Patents
Method and system for continuously preparing AG film, AR film and AF film Download PDFInfo
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- CN115893866B CN115893866B CN202211337958.0A CN202211337958A CN115893866B CN 115893866 B CN115893866 B CN 115893866B CN 202211337958 A CN202211337958 A CN 202211337958A CN 115893866 B CN115893866 B CN 115893866B
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- 239000001301 oxygen Substances 0.000 claims description 36
- 229910052760 oxygen Inorganic materials 0.000 claims description 36
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 27
- 238000000151 deposition Methods 0.000 claims description 17
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000012298 atmosphere Substances 0.000 claims description 3
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 3
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical group [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 claims description 3
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- Surface Treatment Of Glass (AREA)
Abstract
The invention relates to the technical field of cover plate glass manufacturing, in particular to a method and a system for continuously preparing an AG film, an AR film and an AF film. The method comprises the steps of (1) introducing a substrate to be coated into a chamber A for first cleaning to obtain a substrate I with a surface water drop angle not larger than 20 degrees, spraying anti-dazzle paint on the surface of the substrate I to obtain a substrate II containing an AG film, (2) introducing the substrate II into the chamber B for curing treatment to obtain a substrate III, (3) introducing the substrate III into the chamber C for sequentially carrying out second cleaning and drying treatment to obtain a substrate IV, and (4) introducing the substrate IV into the chamber D to form an AR film and an AF film. The method provided by the invention can be used for continuously preparing the AG film, the AR film and the AF film on the glass cover plate, and the prepared product has the characteristics of high yield, stable performance and good uniformity.
Description
Technical Field
The invention relates to the technical field of cover plate glass manufacturing, in particular to a method and a system for continuously preparing an AG film, an AR film and an AF film.
Background
With the development of outdoor and vehicle-mounted displays, an anti-dazzle layer (AG) +an anti-reflection and anti-reflection layer (AR) +an anti-fingerprint layer (AF) cover plate with anti-dazzle, high light transmittance and anti-fingerprint functions is favored by people. At present, in the AG+AR+AF film system structure, a novel Color RAS sputter coating machine is adopted to superimpose the AR film system structure of multiple layers of Si 3N4 and SiO 2 on AG glass, the surface layer of SiO 2 is adopted, and AF is subjected to vacuum evaporation plating. However, siO 2 has a lower hardness than glass, resulting in AG+AR+AF having lower wear resistance than AG+AF.
The RAS coating technology is characterized in that the oxidation-reduction reaction in the coating process is controlled on the surface of the glass substrate, so that the adhesion of the film layer to the substrate and the adhesion of the film layer to the film layer can be greatly improved, the film layer is in a micro-crystallization state, and the film layer has hardness which is incomparable with that of the evaporation coating and the common magnetron sputtering coating. The oxidation-reduction reaction is controlled to occur on the substrate, and only Batch type single-cavity discontinuous film plating equipment can be realized currently.
The glass substrate rotates at a high speed along with the rotating drum, and the Si material plated on the substrate does not exceed one molecular layer every time the glass substrate rotates, and N + or O + ions can completely oxidize the Si material. The continuous coating machine, the glass is conveyed in a multi-chamber, each material plated by one cathode has a plurality of molecular layers (if one molecular layer is controlled, the production efficiency is extremely low), and the material can not be completely oxidized by N + or O + ions. Therefore, RAS technology is low in productivity and cannot be applied to high-efficiency continuous film coating lines.
In addition, the purpose of superhard AR surface layer is achieved by adding diamond film DLC or graphite on the surface of the surface SiO 2 of AR. However, the diamond-like carbon film DLC and graphite have carbon components, the carbon and AF cannot be combined by chemical bonds, the carbon and AF can only be physically adsorbed, and the AF is very easy to fall off during friction test. The AF and AR have poor adhesion, and AF falls off and the AR layer is not damaged in the abrasion test. Therefore, although AR is wear-resistant, AF falls off to cause the reduction of the anti-fouling capability and the color change of the glass surface, and thus far cannot be widely applied.
Moreover, the production equipment and the processing mode of the cover plate plated with the three film layers in the prior art are not ideal, and a plurality of processes such as solid baking, cleaning and transferring are needed to be spanned between the anti-glare layer and the anti-reflection layer, so that when the product with the anti-glare layer, the anti-reflection layer and the anti-fingerprint layer is processed, the production efficiency and the production yield are greatly reduced.
Disclosure of Invention
The invention aims to solve the problems of low production efficiency and low yield in the preparation of AG+AR+AF film cover plates in the prior art.
In order to achieve the above object, a first aspect of the present invention provides a method for continuously producing an AG film, an AR film and an AF film, the method comprising:
(1) Introducing a substrate to be coated into a chamber A for first cleaning to obtain a substrate I with a surface water drop angle not more than 20 degrees, and spraying anti-dazzle paint on the surface of the substrate I to obtain a substrate II containing AG films;
(2) Introducing the substrate II into a chamber B for curing treatment to obtain a substrate III;
(3) Introducing the substrate III into a chamber C to sequentially perform second cleaning and drying treatment to obtain a substrate IV;
(4) The substrate IV is introduced into a chamber D to form an AR film and an AF film, wherein the method for forming the AR film comprises alternately depositing metal oxide layers and silicon oxide layers on the surface of the substrate IV in the presence of a protective atmosphere, and the oxygen content in the metal oxide layers is lower than that in the silicon oxide layers.
Preferably, in step (4), the oxygen content in the metal oxide layer is 40-60% by volume lower than the oxygen content in the oxide layer of silicon.
Preferably, in step (4), the main component of the metal oxide layer is niobium pentoxide and/or titanium dioxide.
Preferably, in step (1), the conditions of the first cleaning are controlled so that the surface water drop angle of the substrate I is not more than 10 °.
Preferably, in step (1), the first cleaning is a plasma cleaning, and the power of the plasma cleaning is 500-1500W, preferably 700-1200W.
Preferably, in the step (1), the method further comprises the step of preheating the substrate to be coated before the first cleaning.
Preferably, in step (1), the conditions of the preheating treatment include at least a temperature of 20-400 ℃, preferably 30-120 ℃, and a time of 12-60s.
Preferably, in the step (1), the spraying is performed under the condition that the substrate I rotates, and the surface linear velocity of the substrate I is 300-1200mm/s.
Preferably, in the step (1), the spraying condition at least comprises a spraying distance of 80-150mm, a temperature of 20-130 ℃, a spray gun atomization pressure of 0.1-0.6MPa, a spray gun sector pressure of 0.1-0.6MPa, a supply pressure of 0.1-0.6MPa and a flow rate of 1-30g/min.
Preferably, in the step (2), the curing treatment condition at least comprises a temperature of 130-400 ℃ and a time of 20-60min.
Preferably, in step (3), the second washing comprises washing I with a neutral wash, washing II with water, and washing III with acetone.
Preferably, in the step (3), the condition of the drying treatment at least comprises the temperature of 100-180 ℃ and the time of 10-30min.
Preferably, in the step (4), the AF film is formed by vacuum evaporation, and the conditions of the vacuum evaporation at least include a temperature of 300-600 ℃.
In a second aspect, the present invention provides a system for continuously preparing an AG film, an AR film and an AF film, comprising:
the jig is used for fixing the substrate to be coated;
The anti-dazzle spray gun array comprises at least 2 anti-dazzle spray guns, the distance between every two adjacent anti-dazzle spray guns is 60-100mm, and the chamber A is used for carrying out first cleaning on a substrate to be coated and forming an AG film;
the device comprises a chamber B, wherein at least two heating pipes are uniformly arranged in the chamber B, the distance between every two adjacent heating pipes is 20-100mm, and the chamber B is used for curing an AG film;
The cleaning spray gun is vertically arranged on the inner wall of the chamber C, a nozzle of the cleaning spray gun is vertically arranged towards the substrate III, the brush is tangentially arranged with the jig, the hot air knife is vertically arranged on the inner wall of the chamber C, an air outlet of the hot air knife is arranged towards the substrate III, and a liquid-air recovery port is further arranged below the chamber C;
and a chamber D, wherein a metal target, a silicon target and a tray for placing AF medicament are arranged in the chamber D, and the chamber D is used for forming an AR film and an AF film.
Preferably, the system further comprises a transfer mechanism capable of transferring the jig between the chambers, and the transfer mechanism is a manipulator.
The method provided by the invention can be used for continuously preparing the AG film, the AR film and the AF film on the glass cover plate, and the prepared product has the characteristics of high yield, stable performance and good uniformity.
Particularly, the AG film, the AR film and the AF film can be integrally processed by adopting the method provided by the invention, so that the problems of low efficiency and low yield caused by feeding and discharging and intermediate procedures during production are avoided.
Drawings
FIG. 1 is a particularly preferred embodiment of the method for continuously preparing AG film, AR film and AF film provided by the present invention.
Description of the reference numerals
1. Jig 2 and substrate to be coated
3. Transfer mechanism 4 and plasma cleaning gun
5. Anti-dazzle spray gun 6 and heating pipe
7. Cleaning spray gun 8 and brush
9. Hot air knife 10 and metal target
11. Silicon target 12, tray
Detailed Description
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
In the present invention, unless otherwise stated, the room temperature or the normal temperature represents 25±2 ℃.
As described above, the first aspect of the present invention provides a method for continuously producing AG film, AR film and AF film, the method comprising:
(1) Introducing a substrate to be coated into a chamber A for first cleaning to obtain a substrate I with a surface water drop angle not more than 20 degrees, and spraying anti-dazzle paint on the surface of the substrate I to obtain a substrate II containing AG films;
(2) Introducing the substrate II into a chamber B for curing treatment to obtain a substrate III;
(3) Introducing the substrate III into a chamber C to sequentially perform second cleaning and drying treatment to obtain a substrate IV;
(4) The substrate IV is introduced into a chamber D to form an AR film and an AF film, wherein the method for forming the AR film comprises alternately depositing metal oxide layers and silicon oxide layers on the surface of the substrate IV in the presence of a protective atmosphere, and the oxygen content in the metal oxide layers is lower than that in the silicon oxide layers.
Preferably, the AG film has an average thickness of 50nm to 300nm.
Preferably, the average thickness of the AR film is 200-300nm, preferably 230-270nm.
Preferably, the AF film has an average thickness of 10-40nm.
Preferably, in step (4), the oxygen content in the metal oxide layer is 40-60% by volume lower than the oxygen content in the oxide layer of silicon. The inventors found that in this preferable case, a glass cover plate having a better light transmittance and a stable color patch value can be obtained.
Preferably, in step (4), the main component of the metal oxide layer is niobium pentoxide and/or titanium dioxide.
Preferably, in step (4), the main component in the oxide layer of silicon is silicon dioxide.
According to a particularly preferred embodiment of the present invention, in step (4), an AR film is formed using a magnetron sputtering method.
According to a particularly preferred embodiment of the present invention, in step (1), the condition of the first cleaning is controlled so that the surface water drop angle of the substrate I is not more than 10 °.
Preferably, in step (1), the first cleaning is a plasma cleaning, and the power of the plasma cleaning is 500-1500W, more preferably 700-1200W. The inventors found that with this preferred embodiment, not only a good cleaning effect can be obtained, but also no damage can be caused to the substrate surface.
The type of plasma cleaning in the present invention is not particularly limited, and may be performed using a type known in the art, and preferably, the first cleaning is a rotary torch plasma cleaning or a linear plasma cleaning.
When the first cleaning is performed by using a rotary spray gun for plasma cleaning, the vertical distance between the spray gun and the surface of the substrate to be coated is 5-30mm, preferably 10-20mm, and when the first cleaning is performed by using a linear plasma cleaning, the vertical distance between the linear plasma generating opening and the surface of the substrate to be coated is 1-5mm, preferably 2-3mm.
The kind of carrier gas used in the plasma cleaning process of the present invention is not particularly limited, and may be carried out using a kind of carrier gas known in the art, and for example, argon may be used.
Preferably, in the step (1), the method further comprises the step of preheating the substrate to be coated before the first cleaning.
Preferably, in step (1), the conditions of the preheating treatment include at least a temperature of 20-400 ℃, preferably 30-120 ℃, and a time of 12-60s.
Preferably, in the step (1), the spraying is performed under the condition that the substrate I rotates, and the surface linear velocity of the substrate I is 300-1200mm/s.
Preferably, in the step (1), the spraying condition at least comprises a spraying distance of 80-150mm, a temperature of 20-130 ℃, a spray gun atomization pressure of 0.1-0.6MPa, a spray gun sector pressure of 0.1-0.6MPa, a supply pressure of 0.1-0.6MPa and a flow rate of 1-30g/min.
In the invention, the spraying distance in the step (1) refers to the vertical distance from the spray gun nozzle to the surface of the substrate I.
Preferably, in the step (2), the curing treatment condition at least comprises a temperature of 130-400 ℃ and a time of 20-60min.
Preferably, in step (3), the second washing comprises washing I with a neutral wash, washing II with water, and washing III with acetone.
The neutral lotion of the present invention is not particularly limited in kind, and neutral lotions of the kind known in the art can be used, and, for example, glass-specific lotions having a pH of 6 to 8 can be used in the present invention. The invention has no special requirement on the dosage of the neutral lotion, the water and the acetone, and can achieve the cleaning purpose only. The condition of the second cleaning is not particularly required, and the second cleaning can be performed according to actual conditions, and the second cleaning time is 2-5min for example.
Preferably, in the step (3), the condition of the drying treatment at least comprises the temperature of 100-180 ℃ and the time of 10-30min.
Preferably, in the step (4), the AF film is formed by vacuum evaporation, and the conditions of the vacuum evaporation at least include a temperature of 300-600 ℃.
The AF agent used for forming the AF film of the present invention is not particularly limited, and AF agents of a type known in the art may be used, and exemplified by compounds containing at least one of a polyfluoropolyether group, a polyfluoroalkyl group, and a polyfluoroalkylene group.
The present invention has no particular requirement on the amount of the AF agent used for forming the AF film, and is only required to satisfy the needs of the present invention, and for example, the AF film to be formed only needs to have an average thickness of 10 to 40 nm.
The present invention is not particularly limited in the kind of the substrate to be coated, and any substrate to be coated known in the art may be used, and the substrate to be coated is exemplified by at least one selected from a white glass substrate, a glass substrate with ink, and a resin substrate.
As described above, the second aspect of the present invention provides a system for continuously preparing an AG film, an AR film and an AF film, the system comprising:
The jig 1 is used for fixing the substrate 2 to be coated;
The anti-dazzle spray gun array comprises at least 2 anti-dazzle spray guns 5, wherein the distance between every two adjacent anti-dazzle spray guns 5 is 60-100mm, and the chamber A is used for carrying out first cleaning on a substrate 2 to be coated and forming an AG film;
The device comprises a chamber B, wherein at least two heating pipes 6 are uniformly arranged in the chamber B, the distance between every two adjacent heating pipes 6 is 20-100mm, and the chamber B is used for curing AG films;
The cleaning spray gun 7, the hairbrush 8 and the hot air knife 9 are arranged in the cavity C, the cleaning spray gun 7 is vertically arranged on the inner wall of the cavity C, the nozzle of the cleaning spray gun 7 is vertically arranged towards the substrate III, the hairbrush 8 is tangentially arranged with the jig 1, the hot air knife 9 is vertically arranged on the inner wall of the cavity C, the air outlet of the hot air knife 9 is arranged towards the substrate III, and the liquid-gas recovery port is further arranged below the cavity C;
A chamber D in which a metal target 10, a silicon target 11, and a tray 12 for placing an AF agent are provided, the chamber D being for forming an AR film and an AF film.
By adopting the system provided by the invention, the AG film, the AR film and the AF film can be integrally processed, the solidification of the anti-dazzle layer of the manual rotating frame, the cleaning of the manual rotating frame and the AR film plating of the manual rotating frame are completely avoided after the spraying of the anti-dazzle layer is finished, the time of exposing the substrate in the environment is reduced, and the efficiency and the yield are improved.
In the chamber a, the distance between two adjacent plasma cleaning guns and the distance between two adjacent antiglare guns may be determined according to the spray area of the guns, and the number of the two guns may be increased or decreased according to the size of the chamber.
In the chamber B, there is no particular requirement for the length and diameter of the heating pipes, but only the requirement of the present invention is satisfied, and in order to ensure the radiation coverage of the effective area and to keep the temperature in the chamber B constant, the length of each heating pipe 6 is 1000-1500mm, and the diameter of each heating pipe 6 is 10-30mm, with respect to the chamber B having an inner cavity height of 900-1800mm and an inner cavity diameter of 800-1500mm, for example.
The following describes in detail the specific operation of forming the AR film in conjunction with the structure of the chamber D, including:
And introducing oxygen and inert gas into the chamber D, electrifying the metal target 10 to enable metal and oxygen to form metal oxide, bombarding and depositing the metal oxide on the surface of the substrate IV through inert gas molecules, electrifying the silicon target 11 to enable silicon and oxygen to form silicon dioxide, bombarding and depositing the silicon dioxide on the surface of the substrate IV through inert gas molecules, and repeating the steps until the thickness of the AR film reaches 200-300nm.
Preferably, the power densities of the metal target 10 and the silicon target 11 are respectively 3-5W/cm 2.
In the actual operation, the AF agent is placed in the tray 12, and the active ingredient therein is evaporated and deposited on the surface of the substrate IV by heating.
Preferably, the system further comprises a transfer mechanism 3 capable of transferring the jig between the chambers, and the transfer mechanism 3 is a manipulator.
The invention has no special limitation on the types of the manipulators, and only needs to realize that the jig can be transported between the chambers, any manipulator known in the art can be adopted, and the manipulator is not repeated herein, and the person skilled in the art should not understand the limitation of the invention
Preferably, the substrate to be coated 2 is adhered to the fixture 1.
According to the invention, a plurality of substrates 2 to be coated can be adhered on the jig 1 according to actual needs, and illustratively, 20-100 substrates 2 to be coated are arranged on the jig 1, and the distance between two adjacent substrates 2 to be coated is 20-40mm.
A particularly preferred embodiment of the method for continuously producing AG film, AR film and AF film according to the present invention is described in detail below with reference to fig. 1:
(1) Adhering a substrate 2 to be coated on a jig 1, introducing the jig 1 fixed with the substrate 2 to be coated into a chamber A through a transfer mechanism 3, performing first cleaning on the surface of the substrate 2 to be coated by using a plasma cleaning gun 4 to obtain a substrate I with a surface water drop angle not more than 20 degrees, and spraying anti-dazzle paint on the surface of the substrate I through an anti-dazzle spray gun 5 to obtain a substrate II containing AG films;
(2) Introducing the substrate II into the chamber B through the transfer mechanism 3, and curing under the action of the heating pipe 6 to obtain a substrate III;
(3) Introducing the substrate III into the chamber C through the transfer mechanism 3, performing second cleaning through the cooperation of the cleaning spray gun 7 and the brush 8, and then performing drying treatment under the action of the hot air knife 9 to obtain a substrate IV;
(4) Introducing the substrate IV into a chamber D through a transfer mechanism 3, introducing oxygen and inert gas, electrifying the metal target 10 to enable metal and oxygen to form metal oxide, bombarding and depositing the metal oxide on the surface of the substrate IV through inert gas molecules, electrifying the silicon target 11 to enable silicon and oxygen to form silicon dioxide, bombarding and depositing the silicon and oxygen on the surface of the substrate IV through inert gas molecules, repeating the steps until the thickness of an AR film reaches 230-270nm, placing an AF medicament into a tray 12, and evaporating and depositing active ingredients in the AF medicament on the surface of the substrate IV through a heating mode, wherein the oxygen content in the metal oxide layer is lower than that in the silicon oxide layer.
The invention will be described in detail below by way of examples. In the following examples, various materials and instruments were used as commercial products unless otherwise specified.
The substrate to be coated is panda MN228 glass, which is from Sichuan iridaceae, innovative technology limited company;
the antiglare coating is AG180, and is purchased from PPG coating (Tianjin) Co., ltd;
AF agent, trade name H6500D, purchased from Shengyuan lubricating materials Co., ltd;
The neutral lotion is purchased from Shenzhen Nanxiang environmental protection technology Co., ltd with the brand L-1012;
In the following examples, the diameters of the inner cavities of the cavity A, the cavity B, the cavity C and the cavity D are 1500mm, and the heights of the inner cavities are 1800mm;
in the chamber A, the distance between two adjacent plasma cleaning guns is 60mm, and the distance between two adjacent anti-dazzle guns is 60mm;
in the cavity B, the distance between two adjacent heating pipes is 40mm, the length of each heating pipe is 1200mm, and the diameter of each heating pipe is 20mm;
In the following examples, the transfer mechanisms are manipulators, and the power densities of the metal target and the silicon target are 5W/cm 2.
Example 1
The present embodiment provides a method for continuously preparing an AG film, an AR film, and an AF film, the method comprising:
(1) Adhering 80 substrates to be coated on a jig, preheating the jig provided with the substrates to be coated (the temperature is 80 ℃ and the time is 30 s), introducing the jig provided with the substrates to be coated into a chamber A through a transfer mechanism, performing first cleaning on the surfaces of the substrates to be coated by using a plasma cleaning gun to obtain a substrate I with a surface water drop angle of 5 ℃, and spraying anti-dazzle paint on the surfaces of the substrate I by using an anti-dazzle spray gun to obtain a substrate II containing AG films, wherein the average thickness of the AG films is 120nm;
The first cleaning adopts rotary spray gun plasma cleaning, and the first cleaning condition is that the vertical distance between the spray gun and the surface of the substrate to be coated is 10mm, the carrier gas is argon, and the power is 800W;
The spraying condition is that the surface linear speed of the substrate I is 1000mm/s, the spraying distance is 80mm, the temperature is 80 ℃, the spray gun atomization pressure is 0.4MPa, the spray gun sector pressure is 0.4MPa, the supply pressure of the anti-dazzle coating is 0.4MPa, and the flow rate of the anti-dazzle coating is 10g/min;
(2) Introducing the substrate II into the chamber B through a transfer mechanism, and performing curing treatment under the action of a heating pipe to obtain a substrate III;
wherein, the curing treatment condition is that the temperature is 150 ℃ and the time is 60min;
(3) Introducing the substrate III into a chamber C through a transfer mechanism, sequentially spraying neutral lotion, deionized water and acetone by adopting a cleaning spray gun, sequentially cleaning the substrate III for I3 min, II 5min and III 4min, continuously rotating a hairbrush in the cleaning process to wipe the surface of the substrate III, and then drying under the action of a hot air knife to obtain a substrate IV;
Wherein, the condition of the drying treatment is that the temperature is 100 ℃ and the time is 30min;
(4) Introducing the substrate IV into a chamber D through a transfer mechanism, introducing oxygen and argon, electrifying the metal target, enabling metal and oxygen to form metal oxide, bombarding and depositing the metal oxide on the surface of the substrate IV through argon molecules, electrifying the silicon target, enabling silicon and oxygen to form silicon dioxide, bombarding and depositing the silicon and oxygen on the surface of the substrate IV through argon molecules, repeating the steps until the thickness of an AR film reaches 260mm, placing an AF medicament in a tray, and evaporating and depositing active ingredients in the AF medicament on the surface of the substrate IV under a vacuum condition (the vacuum degree is 1X 10 - 5 Pa), wherein the average thickness of the AF film is 30nm, and the oxygen content in the metal oxide layer is 50 vol% lower than the oxygen content in the silicon oxide layer.
Example 2
The present embodiment provides a method for continuously preparing an AG film, an AR film, and an AF film, the method comprising:
(1) Adhering 20 substrates to be coated on a jig, preheating the jig provided with the substrates to be coated (the temperature is 90 ℃ and the time is 60 s), introducing the jig provided with the substrates to be coated into a chamber A through a transfer mechanism, performing first cleaning on the surfaces of the substrates to be coated by using a plasma cleaning gun to obtain a substrate I with a surface water drop angle of 5 ℃, and spraying anti-dazzle paint on the surfaces of the substrate I by using an anti-dazzle spray gun to obtain a substrate II containing AG films, wherein the average thickness of the AG films is 210nm;
The first cleaning adopts rotary spray gun plasma cleaning, and the first cleaning condition is that the vertical distance between the spray gun and the surface of the substrate to be coated is 15mm, the carrier gas is argon, and the power is 1000W;
The spraying condition is that the surface linear speed of the substrate I is 800mm/s, the spraying distance is 90mm, the temperature is 90 ℃, the spray gun atomization pressure is 0.45MPa, the spray gun sector pressure is 0.45MPa, the supply pressure of the anti-dazzle coating is 0.4MPa, and the flow rate of the anti-dazzle coating is 15g/min;
(2) Introducing the substrate II into the chamber B through a transfer mechanism, and performing curing treatment under the action of a heating pipe to obtain a substrate III;
Wherein, the curing treatment condition is that the temperature is 200 ℃ and the time is 50min;
(3) Introducing the substrate III into a chamber C through a transfer mechanism, sequentially spraying neutral lotion, deionized water and acetone to the substrate III by adopting a cleaning spray gun, sequentially cleaning the substrate III for I3 min, cleaning the substrate III for II 5min and cleaning the substrate III for 4min, continuously rotating a brush in the cleaning process to wipe the surface of the substrate III, and then drying under the action of a hot air knife to obtain a substrate IV;
wherein, the condition of the drying treatment is that the temperature is 150 ℃ and the time is 20min;
(4) Introducing the substrate IV into a chamber D through a transfer mechanism, introducing oxygen and argon, electrifying the metal target, enabling metal and oxygen to form metal oxide, bombarding and depositing the metal oxide on the surface of the substrate IV through argon molecules, electrifying the silicon target, enabling silicon and oxygen to form silicon dioxide, bombarding and depositing the silicon and oxygen on the surface of the substrate IV through argon molecules, repeating the steps until the thickness of an AR film reaches 240mm, placing an AF medicament in a tray, and evaporating and depositing active ingredients in the AF medicament on the surface of the substrate IV under a vacuum condition (the vacuum degree is 1X 10 - 5 Pa), wherein the average thickness of the AF film is 30nm, and the oxygen content in the metal oxide layer is 40 vol% lower than the oxygen content in the silicon oxide layer.
Example 3
The present embodiment provides a method for continuously preparing an AG film, an AR film, and an AF film, the method comprising:
(1) Adhering 50 substrates to be coated on a jig, preheating the jig provided with the substrates to be coated (the temperature is 40 ℃ and the time is 0.8 min), introducing the jig provided with the substrates to be coated into a chamber A through a transfer mechanism, performing first cleaning on the surfaces of the substrates to be coated by using a plasma cleaning gun to obtain a substrate I with a surface water drop angle of 8 ℃, and spraying an anti-dazzle coating on the surfaces of the substrate I by using an anti-dazzle spray gun to obtain a substrate II containing AG films, wherein the average thickness of the AG films is 300nm;
The first cleaning adopts rotary spray gun plasma cleaning, and the first cleaning condition is that the vertical distance between the spray gun and the surface of the substrate to be coated is 20mm, the carrier gas is argon, and the power is 700W;
The spraying condition is that the surface linear speed of the substrate I is 600mm/s, the spraying distance is 110mm, the temperature is 40 ℃, the spray gun atomization pressure is 0.5MPa, the spray gun sector pressure is 0.5MPa, the supply pressure of the anti-dazzle coating is 0.5MPa, and the flow rate of the anti-dazzle coating is 20g/min;
(2) Introducing the substrate II into the chamber B through a transfer mechanism, and performing curing treatment under the action of a heating pipe to obtain a substrate III;
Wherein, the curing treatment condition is that the temperature is 350 ℃ and the time is 30min;
(3) Introducing the substrate III into a chamber C through a transfer mechanism, sequentially spraying neutral lotion, deionized water and acetone to the substrate III by adopting a cleaning spray gun, sequentially cleaning the substrate III for I3 min, cleaning the substrate III for II 5min and cleaning the substrate III for 4min, continuously rotating a brush in the cleaning process to wipe the surface of the substrate III, and then drying under the action of a hot air knife to obtain a substrate IV;
Wherein, the condition of the drying treatment is that the temperature is 180 ℃ and the time is 10min;
(4) Introducing the substrate IV into a chamber D through a transfer mechanism, introducing oxygen and argon, electrifying the metal target, enabling metal and oxygen to form metal oxide, bombarding and depositing the metal oxide on the surface of the substrate IV through argon molecules, electrifying the silicon target, enabling silicon and oxygen to form silicon dioxide, bombarding and depositing the silicon and oxygen on the surface of the substrate IV through argon molecules, repeating the steps until the thickness of an AR film reaches 250mm, placing an AF medicament in a tray, and evaporating and depositing active ingredients in the AF medicament on the surface of the substrate IV under a vacuum condition (the vacuum degree is 1X 10 - 5 Pa), wherein the average thickness of the AF film is 30nm, and the oxygen content in the metal oxide layer is 60 volume percent lower than the oxygen content in the silicon oxide layer.
Example 4
AG film, AR film and AF film were continuously produced in the same manner as in example 1 except that in step (1), the conditions of the first cleaning were controlled so that the surface water drop angle of the substrate I was 15 °.
Example 5
AG film, AR film and AF film were continuously prepared in the same manner as in example 1 except that in step (1), the power of the first washing was 500W.
Example 6
AG film, AR film and AF film were continuously produced according to the method of example 1, except that in step (4), the oxygen content in the metal oxide layer was 80% by volume lower than that in the silicon oxide layer.
Comparative example 1
AG film, AR film and AF film were continuously produced in the same manner as in example 1 except that in step (1), the conditions of the first cleaning were controlled so that the surface water drop angle of the substrate I was 25 °.
Comparative example 2
AG film, AR film and AF film were continuously prepared according to the method of example 1, except that in step (4), the oxygen content in the metal oxide layer was the same as that in the silicon oxide layer.
Comparative example 3
AG film, AR film and AF film were continuously produced according to the method of example 1, except that in step (4), the oxygen content in the metal oxide layer was 40% by volume higher than that in the silicon oxide layer.
Test example 1
2 Substrates II containing AG films prepared in example 1 were randomly selected for performance testing, and a control group was set, and specific test results are shown in Table 1.
The method is similar to the step (1) in the embodiment 1, except that in the process of spraying the anti-dazzle coating, the film substrate I is placed in parallel with the ground, and then the anti-dazzle coating is sprayed on the surface of the substrate I by adopting an anti-dazzle spray gun;
The 60 DEG gloss test method comprises measuring 2 points of each sample by BYK60 DEG gloss meter;
The haze test method comprises measuring 2 points of each sample by BYK4775 transmission haze meter;
the AG film thickness test method comprises the steps of measuring a Mitutoyo SJ-410 tester and Free conditions, and measuring 2 points of each sample.
TABLE 1
As can be seen from the results of Table 1, the AG film obtained by the method provided by the invention still maintains stable film thickness uniformity under different glossiness and haze.
Test example 2
1 Substrate II containing AG film prepared in example 1, example 2 and example 3 was randomly selected for performance test, 3 measurement points were randomly selected on each substrate, and specific test results are shown in Table 2.
The pencil hardness testing method comprises the steps of drawing a pencil with the hardness to be tested through a track of 5 tracks for 2cm by using a Japanese Mitsubishi pencil with a load of 750g and an included angle of 45 degrees, wherein the scratch is less than or equal to 2 qualified tracks;
The method for testing the friction resistance comprises the following steps: eraser, load 500g, speed 40 times/min, rub 1500 times, observe the membranous layer appearance visually and microscope;
The adhesive force (hundred lattice) test method is that the AG layer surface, the nicking tool nicks 11 times horizontally and vertically to form a square area containing 100 square lattices, the adhesive tape is repeatedly stuck for 3 times, the surface is free from falling, and the mark is 5B.
TABLE 2
As can be seen from the results in Table 2, the AG film hardness, abrasion resistance and adhesion (hundred) test obtained by the method provided by the invention all meet the standards, and the film stability is good.
Test example 3
The AR films prepared in example 1, example 2 and example 3 were randomly selected for performance test, and 2 measurement points were randomly selected on each substrate, and specific test results are shown in table 3.
The method for testing the L, a, b and y values by the SCI method comprises SPECTROPHOTOMETER CM-26d color measuring instrument, testing two points of each sample, and recording SCI mode data;
the method for testing the L, a, b and y values by the SCE method comprises the steps of SPECTROPHOTOMETER CM-26d color measuring instrument, testing two points of each sample, and recording SCE mode data.
TABLE 3 Table 3
As can be seen from the results of Table 3, the AR films L, a, b and y obtained by the method provided by the invention have good stability.
Test example 4
The substrates containing AG film, AR film and AF film prepared in examples and comparative examples were subjected to performance test, and specific test results are shown in table 4.
The pencil hardness testing method comprises the steps of drawing a pencil with the hardness to be tested through a track of 5 tracks for 2cm by using a Japanese Mitsubishi pencil with a load of 750g and an included angle of 45 degrees, wherein the scratch is less than or equal to 2 qualified tracks;
the method for testing the friction resistance comprises LIBERON # 0000 steel wool, carrying 500g, carrying 40 times/min, rubbing 1500 times, testing the water drop angle before and after rubbing, and judging whether the friction angle is more than or equal to 110 degrees or more and more than or equal to 100 degrees after rubbing;
The water drop angle test method is that SINDIN water contact angle measuring instrument measures the water drop angle at the same position before and after friction, and records the change condition.
The pencil hardness testing method is adopted to scratch less than or equal to 2 times, the water drop angle after the abrasion resistance performance test is more than or equal to 100 degrees, and the pencil hardness testing method is used to obtain good products, and the calculation formula of the good products rate is (number of good products/total number of samples) ×100%.
TABLE 4 Table 4
| Hardness of pencil | Angle of water drop before friction ° | Angle of water drop after friction ° | Yield of percent | |
| Example 1 | 8H | 112.7 | 103.5 | 100% |
| Example 2 | 8H | 111.6 | 102.2 | 100% |
| Example 3 | 8H | 112.7 | 103.4 | 100% |
| Example 4 | 7H | 110.1 | 101.5 | 90% |
| Example 5 | 7H | 110.3 | 101.4 | 90% |
| Example 6 | 6H | 110.5 | 91.8 | 60% |
| Comparative example 1 | 6H | 110.9 | 90.1 | 50% |
| Comparative example 2 | 5H | 110.7 | 54.5 | 0 |
| Comparative example 3 | 4H | 110.1 | 53.2 | 0 |
As can be seen from the results in Table 4, AG film, AR film and AF film can be continuously prepared on the glass cover plate by the method provided by the invention, and the prepared product has the characteristics of high yield, stable performance and good uniformity.
The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, a number of simple variants of the technical solution of the invention are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the invention, all falling within the scope of protection of the invention.
Claims (14)
1. A method for continuously producing an AG film, an AR film and an AF film, comprising:
(1) Introducing a substrate to be coated into a chamber A for first cleaning to obtain a substrate I with a surface water drop angle not more than 20 degrees, and spraying anti-dazzle paint on the surface of the substrate I to obtain a substrate II containing AG films;
(2) Introducing the substrate II into a chamber B for curing treatment to obtain a substrate III;
(3) Introducing the substrate III into a chamber C to sequentially perform second cleaning and drying treatment to obtain a substrate IV;
(4) The substrate IV is introduced into a chamber D to form an AR film and an AF film, wherein the method for forming the AR film comprises alternately depositing metal oxide layers and silicon oxide layers on the surface of the substrate IV in the presence of a protective atmosphere, and the oxygen content in the metal oxide layers is 40-60 vol% lower than that in the silicon oxide layers.
2. The method according to claim 1, wherein in step (4), the main component of the metal oxide layer is niobium pentoxide and/or titanium dioxide.
3. The method according to claim 1 or 2, wherein in step (1), the conditions of the first cleaning are controlled so that the surface water drop angle of the substrate I is not more than 10 °.
4. The method according to claim 1 or 2, wherein in step (1), the first cleaning is a plasma cleaning, and the power of the plasma cleaning is 500-1500W.
5. The method of claim 4, wherein the plasma cleaning power is 700-1200W.
6. The method according to claim 1 or 2, wherein in the step (1), the method further comprises subjecting the substrate to be coated to a preheating treatment before the first cleaning.
7. The method according to claim 6, wherein the conditions for the preheating treatment include at least a temperature of 20 to 400 ℃ for a time of 12 to 60 seconds.
8. The method according to claim 7, wherein the conditions for the preheating treatment include at least a temperature of 30 to 120 ℃.
9. The method according to claim 1 or 2, wherein in step (1), the spraying is performed under the condition that the substrate I is rotated, and the surface linear velocity of the substrate I is 300-1200mm/s.
10. The method according to claim 9, wherein the spraying conditions include at least a spraying distance of 80 to 150mm, a temperature of 20 to 130 ℃, a spray gun atomizing pressure of 0.1 to 0.6MPa, a spray gun sector pressure of 0.1 to 0.6MPa, a supply pressure of 0.1 to 0.6MPa, and a flow rate of 1 to 30g/min.
11. The method according to claim 1 or 2, wherein in the step (2), the curing treatment conditions include at least a temperature of 130 to 400 ℃ for 20 to 60 minutes.
12. The method according to claim 1 or 2, wherein in step (3), the second washing comprises washing I with a neutral wash, washing II with water, and washing III with acetone.
13. The method according to claim 1 or 2, wherein in the step (3), the conditions of the drying treatment include at least a temperature of 100 to 180 ℃ for a time of 10 to 30 minutes.
14. The method according to claim 1 or 2, wherein in step (4), the AF film is formed by vacuum evaporation, and the conditions of the vacuum evaporation include at least a temperature of 300-600 ℃.
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