CN115893866A - Method and system for continuously preparing AG membrane, AR membrane and AF membrane - Google Patents

Abstract

The invention relates to the technical field of cover glass manufacturing, in particular to a method and system for continuously preparing AG films, AR films and AF films. The method includes: (1) introducing the substrate to be coated into the chamber A for first cleaning to obtain a substrate I with a surface water drop angle not greater than 20°, and spraying an anti-glare coating on the surface of the substrate I to obtain a film containing AG (2) introducing the substrate II into the chamber B for curing treatment to obtain the substrate III; (3) introducing the substrate III into the chamber C to perform the second cleaning and drying treatment sequentially to obtain the substrate IV; (4) The substrate IV is introduced into the chamber D to form an AR film and an AF film. The method provided by the invention can continuously prepare AG film, AR film and AF film on the glass cover plate, and the prepared products have the characteristics of high yield rate, stable performance and good uniformity.

Description

A method and system for continuously preparing AG film, AR film and AF film

technical field

The invention relates to the technical field of cover glass manufacturing, in particular to a method and system for continuously preparing AG films, AR films and AF films.

Background technique

With the development of outdoor and automotive displays, anti-glare (AG) + anti-reflection and anti-reflection (AR) + anti-fingerprint (AF) cover plates with anti-glare, high light transmission and anti-fingerprint are very popular. At present, in the AG+AR+AF film structure, the AR film structure of multi-layer Si ₃ N ₄ and SiO ₂ is superimposed on the AG glass by using the new Kelong RAS sputtering coating machine, and the surface layer is SiO ₂ , and then the AF is vacuum evaporated. However, the hardness of SiO ₂ film is not as good as that of glass, so the wear resistance of AG+AR+AF is not as good as that of AG+AF.

The core of RAS coating technology is that the oxidation-reduction reaction of the coating process is controlled on the surface of the glass substrate, which can greatly improve the adhesion between the film and the substrate, and the adhesion between the film and the film, and make the film in a microcrystalline state. The film layer has a hardness unmatched by evaporation coatings and ordinary magnetron sputtering coatings. Controlling the oxidation-reduction reaction to occur on the substrate is currently only possible on batch-type single-chamber discontinuous coating equipment.

The glass substrate rotates with the drum at high speed, and the Si material plated on the substrate does not exceed one molecular layer per revolution, and N ⁺ or O ⁺ ions can completely nitrogen/oxidize it. In the continuous coating machine, the glass is conveyed in the multi-chamber, and each cathode-plated material has several molecular layers (if it is controlled within one molecular layer, the production efficiency is extremely low), it can no longer be completely N ⁺ or O ⁺ ion nitrogen / oxidation. Therefore, the production capacity of RAS technology is very low, and it cannot be applied to a high-efficiency continuous coating line.

In addition, there is another solution to achieve the superhard surface of AR by adding diamond film DLC or graphite on the surface of AR surface SiO ₂ . However, the diamond-like film DLC and graphite are composed of carbon, and carbon and AF cannot be combined by chemical bonds. The two can only be physically adsorbed, and AF is easy to fall off during the friction test. The adhesion between AF and AR is very poor, and AF peels off and the AR layer is not damaged in the abrasion test. Therefore, although AR is wear-resistant, the anti-fouling ability of the glass surface will decrease and the color will change after AF falls off, which has not been widely used so far.

Moreover, the production equipment and processing methods of the cover plate coated with three kinds of film layers in the prior art are not ideal. The anti-glare layer and the anti-reflection and anti-reflection layer need to cross several major processes such as curing, cleaning and transfer. When there are anti-glare layer, anti-reflection and anti-reflection layer and anti-fingerprint layer products, the production efficiency and production yield are greatly reduced.

Contents of the invention

The purpose of the present invention is to solve the problems of low production efficiency and good product rate in the preparation of AG+AR+AF film cover plates in the prior art.

In order to achieve the above object, the first aspect of the present invention provides a method for continuously preparing AG film, AR film and AF film, the method comprising:

(1) Introduce the substrate to be coated into the chamber A for the first cleaning to obtain a substrate I with a surface water drop angle not greater than 20°, and spray an anti-glare coating on the surface of the substrate I to obtain a substrate containing an AG film II;

(2) introducing the substrate II into the chamber B for curing treatment to obtain the substrate III;

(3) introducing the substrate III into the chamber C to perform the second cleaning and drying treatment sequentially to obtain the substrate IV;

(4) introducing the substrate IV into the chamber D to form an AR film and an AF film; wherein, the method for forming the AR film includes: in the presence of a protective atmosphere, alternately depositing metal oxide layers and silicon on the surface of the substrate IV oxide layer, and the oxygen content in the metal oxide layer is lower than the oxygen content in the silicon oxide layer.

Preferably, in step (4), the oxygen content in the metal oxide layer is 40-60% by volume lower than the oxygen content in the silicon oxide layer.

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 water drop angle on the surface of the substrate I is not greater than 10°.

Preferably, in step (1), plasma cleaning is used for the first cleaning, and the power of the plasma cleaning is 500-1500W, preferably 700-1200W.

Preferably, in step (1), the method further includes: before performing the first cleaning, preheating the substrate to be coated.

Preferably, in step (1), the conditions of the preheating treatment include at least: a temperature of 20-400°C, preferably 30-120°C; and a time of 12-60s.

Preferably, in step (1), the spraying is carried out under the condition that the substrate I is rotated, and the surface linear velocity of the substrate I is 300-1200mm/s.

Preferably, in step (1), the spraying conditions at least include: the spraying distance is 80-150mm, the temperature is 20-130°C, the spray gun atomization pressure is 0.1-0.6MPa, and the spray gun fan pressure is 0.1-0.6MPa , the supply pressure of the anti-glare coating is 0.1-0.6MPa, and the flow rate of the anti-glare coating is 1-30g/min.

Preferably, in step (2), the conditions of the curing treatment at least include: a temperature of 130-400° C. and a time of 20-60 minutes.

Preferably, in step (3), the second cleaning includes cleaning I with neutral detergent, cleaning II with water and cleaning III with acetone.

Preferably, in step (3), the conditions of the drying treatment at least include: a temperature of 100-180° C. and a time of 10-30 minutes.

Preferably, 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°C.

The second aspect of the present invention provides a system for continuously preparing AG film, AR film and AF film, the system comprising:

jig, the jig is used to fix the substrate to be coated;

Chamber A, a plasma cleaning gun array and an anti-glare spray gun array are arranged side by side in the chamber A, and the plasma cleaning gun array includes at least 2 plasma cleaning guns, and the distance between two adjacent plasma cleaning guns is 40- 80mm; the anti-glare spray gun array includes at least 2 anti-glare spray guns, and the distance between two adjacent anti-glare spray guns is 60-100mm, and the chamber A is used for the first cleaning of the substrate to be coated and the formation of an AG film;

A chamber B, at least two heating tubes are uniformly arranged inside the chamber B, and the distance between two adjacent heating tubes is 20-100mm, and the chamber B is used for curing the AG film;

The chamber C is provided with a cleaning spray gun, a hair brush and a hot air knife, the cleaning spray gun is vertically arranged on the inner wall of the chamber C, and the nozzle of the cleaning spray gun is vertically arranged towards the substrate III, so The brush is arranged tangentially to the jig, the hot air knife is vertically arranged on the inner wall of the chamber C, and the air outlet of the hot air knife is arranged toward the substrate III, and the chamber C is further below Equipped with a liquid gas recovery port;

A chamber D is provided with a metal target, a silicon target and a tray for placing AF agents, and the chamber D is used for forming an AR film and an AF film.

Preferably, the system further includes a transfer mechanism capable of transferring the jig between chambers, and the transfer mechanism is a robot arm.

The method provided by the invention can continuously prepare AG film, AR film and AF film on the glass cover plate, and the prepared products have the characteristics of high yield rate, stable performance and good uniformity.

In particular, the method provided by the invention can process AG film, AR film and AF film in one piece, avoiding the problems of slow efficiency and low yield due to loading and unloading and intermediate processes during production.

Description of 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.

Explanation of reference signs

1. Fixture 2. Substrate to be coated

3. Transfer mechanism 4. Plasma cleaning gun

5. Anti-glare spray gun 6. Heating tube

7. Cleaning spray gun 8. Brush

9. Hot air knife 10. Metal target

11. Silicon target 12. Tray

Detailed ways

Neither the endpoints nor any values of the ranges disclosed herein are limited to such precise ranges or values, and these ranges or values are understood to include values approaching these ranges or values. For numerical ranges, between the endpoints of each range, between the endpoints of each range and individual point values, and between individual point values can be combined with each other to obtain one or more new numerical ranges, these values Ranges should be considered as specifically disclosed herein.

In the present invention, unless stated otherwise, the room temperature or normal temperature both means 25±2°C.

As mentioned above, the first aspect of the present invention provides a method for continuously preparing AG film, AR film and AF film, the method comprising:

(1) Introduce the substrate to be coated into the chamber A for the first cleaning to obtain a substrate I with a surface water drop angle not greater than 20°, and spray an anti-glare coating on the surface of the substrate I to obtain a substrate containing an AG film II;

(2) introducing the substrate II into the chamber B for curing treatment to obtain the substrate III;

(3) introducing the substrate III into the chamber C to perform the second cleaning and drying treatment sequentially to obtain the substrate IV;

(4) introducing the substrate IV into the chamber D to form an AR film and an AF film; wherein, the method for forming the AR film includes: in the presence of a protective atmosphere, alternately depositing metal oxide layers and silicon on the surface of the substrate IV oxide layer, and the oxygen content in the metal oxide layer is lower than the oxygen content in the silicon oxide layer.

Preferably, the average thickness of the AG film is 50nm-300nm.

Preferably, the average thickness of the AR film is 200-300 nm, preferably 230-270 nm.

Preferably, the average thickness of the AF film is 10-40 nm.

Preferably, in step (4), the oxygen content in the metal oxide layer is 40-60% by volume lower than the oxygen content in the silicon oxide layer. The inventors found that under this preferred condition, a glass cover plate with better light transmittance and stable color scale 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 of the silicon oxide layer is silicon dioxide.

According to a particularly preferred embodiment of the present invention, in step (4), the AR film is formed by magnetron sputtering.

According to a particularly preferred embodiment of the present invention, in step (1), the conditions of the first cleaning are controlled so that the water droplet angle on the surface of the substrate I is not greater than 10°.

Preferably, in step (1), plasma cleaning is used for the first cleaning, and the power of the plasma cleaning is 500-1500W, more preferably 700-1200W. The inventors have found that by adopting the preferred embodiment, not only can a good cleaning effect be obtained, but at the same time, no damage will be caused to the surface of the substrate.

The present invention has no particular limitation on the type of plasma cleaning, which can be performed by using known types in the art. Preferably, the first cleaning uses rotary spray gun plasma cleaning or linear plasma cleaning.

It should be noted that when the first cleaning adopts rotary spray gun plasma cleaning, the vertical distance between the spray gun and the surface of the substrate to be coated is 5-30mm, preferably 10-20mm; when the first cleaning adopts linear plasma cleaning , the vertical distance between the linear plasma generating port and the surface of the substrate to be coated is 1-5mm, preferably 2-3mm.

In the present invention, the type of carrier gas used in the plasma cleaning process is not particularly limited, and the type of carrier gas known in the art can be used, for example, argon gas can be used.

Preferably, in step (1), the method further includes: before performing the first cleaning, preheating the substrate to be coated.

Preferably, in step (1), the conditions of the preheating treatment include at least: a temperature of 20-400°C, preferably 30-120°C; and a time of 12-60s.

Preferably, in step (1), the spraying is carried out under the condition that the substrate I is rotated, and the surface linear velocity of the substrate I is 300-1200mm/s.

Preferably, in step (1), the spraying conditions at least include: the spraying distance is 80-150mm, the temperature is 20-130°C, the spray gun atomization pressure is 0.1-0.6MPa, and the spray gun fan pressure is 0.1-0.6MPa , the supply pressure of the anti-glare coating is 0.1-0.6MPa, and the flow rate of the anti-glare coating is 1-30g/min.

Among the present invention, in step (1), spraying distance refers to the vertical distance from the nozzle of the spray gun to the surface of the substrate 1.

Preferably, in step (2), the conditions of the curing treatment at least include: a temperature of 130-400° C. and a time of 20-60 minutes.

Preferably, in step (3), the second cleaning includes cleaning I with neutral detergent, cleaning II with water and cleaning III with acetone.

It should be noted that the present invention has no special requirements on the type of neutral lotion, and neutral lotion known in the art can be used. Exemplarily, the present invention uses a glass-specific detergent with a pH value of 6-8. lotion. The present invention has no special requirement on the consumption of the neutral lotion, water and acetone, as long as the purpose of cleaning can be achieved. The present invention has no special requirements on the conditions of the second cleaning, and the second cleaning can be performed according to the actual situation. Exemplarily, the time of the second cleaning is 2-5 minutes.

Preferably, in step (3), the conditions of the drying treatment at least include: a temperature of 100-180° C. and a time of 10-30 minutes.

Preferably, 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°C.

It should be noted that the present invention has no special requirements on the type of AF agent used to form the AF film, and AF agents known in the art can be used. Exemplarily, the AF agent described in the present invention is selected from , a compound of at least one of polyfluoroalkyl and polyfluoroalkylene.

The present invention has no special requirements on the amount of AF agent used to form the AF film, it only needs to be able to meet the needs of the present invention. Exemplarily, it only needs to be able to make the average thickness of the formed AF film be 10-40nm.

The present invention has no special requirements on the type of the substrate to be coated, and any substrate known in the art that needs to be coated can be used. Exemplarily, the substrate to be coated is selected from white glass substrates, glass with ink at least one of a substrate and a resin substrate.

As previously mentioned, the second aspect of the present invention provides a system for continuously preparing AG film, AR film and AF film, the system comprising:

jig 1, said jig 1 is used to fix the substrate 2 to be coated;

Chamber A, a plasma cleaning gun array and an anti-glare spray gun array are arranged side by side in the chamber A, and the plasma cleaning gun array includes at least 2 plasma cleaning guns 4, and the distance between two adjacent plasma cleaning guns 4 is 40-80mm; the anti-glare spray gun array includes at least two anti-glare spray guns 5, and the distance between two adjacent anti-glare spray guns 5 is 60-100mm, and the chamber A is used for the first cleaning of the substrate 2 to be coated And form AG film;

A chamber B, at least two heating tubes 6 are uniformly arranged inside the chamber B, and the distance between two adjacent heating tubes 6 is 20-100mm, and the chamber B is used for curing the AG film;

The chamber C is provided with a cleaning spray gun 7, a brush 8 and a hot air knife 9, the cleaning spray gun 7 is vertically arranged on the inner wall of the chamber C, and the nozzles of the cleaning spray gun 7 are vertically facing The base plate III is set, the brush 8 is set tangentially to the jig 1, the hot air knife 9 is vertically set on the inner wall of the chamber C, and the air outlet of the hot air knife 9 is set towards the base plate III , the bottom of the chamber C is also provided with a liquid gas recovery port;

A chamber D is provided with a metal target 10 , a silicon target 11 and a tray 12 for placing AF agents, and the chamber D is used for forming an AR film and an AF film.

Adopting the aforementioned system provided by the present invention can process AG film, AR film and AF film in one piece, completely avoiding the curing of the anti-glare layer of the anti-glare layer after the spraying of the anti-glare layer, the cleaning of the manual rotating frame and the AR coating of the artificial rotating frame, reducing the The time the substrate is exposed to the environment improves efficiency and yield.

It should be noted that, in the chamber A, the distance between two adjacent plasma cleaning guns and the distance between two adjacent anti-glare spray guns can be determined according to the spray area of the spray guns; It can be increased or decreased according to the cavity size.

It should be noted that, in the chamber B, there are no special requirements on the length and diameter of the heating tube, as long as it can meet the requirements of the present invention, in order to ensure that the radiation covers the effective area and maintain the chamber The temperature in the chamber B is constant. For example, relative to the chamber B with an inner cavity height of 900-1800 mm and an inner cavity diameter of 800-1500 mm, the length of each heating tube 6 is 1000-1500 mm, each The diameter of the heating pipe 6 is 10-30mm.

The specific operation method for forming the AR film in detail in conjunction with the structure of the chamber D below includes:

Oxygen and an inert gas are introduced into the chamber D, and the metal target 10 is energized first, so that the metal and oxygen form a metal oxide, which is bombarded and deposited on the surface of the substrate IV by inert gas molecules, and then the silicon target 11 Turn on electricity to make silicon and oxygen form silicon dioxide, and deposit it on the surface of substrate IV by bombardment of inert gas molecules. Repeat the above 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 each independently 3-5 W/cm ² .

It should be noted that, during 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 means of heating.

Preferably, the system further includes a transfer mechanism 3 capable of transferring the jig between chambers, and the transfer mechanism 3 is a manipulator.

The present invention has no special limitation on the type of the manipulator, it only needs to be able to realize the transfer of the jig between the chambers, and any manipulator known in the art can be used, and will not be repeated here. Those skilled in the art should not be construed as limiting the present invention

Preferably, the substrate to be coated 2 is pasted on the jig 1 .

In the present invention, a plurality of substrates 2 to be coated can be pasted on the jig 1 according to actual needs. Exemplarily, 20-100 substrates 2 to be coated are arranged on the jig 1, and two adjacent The distance between the substrates 2 to be coated is 20-40mm.

A particularly preferred embodiment of the method for continuously preparing AG film, AR film and AF film provided by the present invention in detail below in conjunction with Fig. 1:

(1) Stick the substrate 2 to be coated on the fixture 1, and introduce the fixture 1 with the substrate 2 to be coated into the chamber A through the transfer mechanism 3, and use the plasma cleaning gun 4 to clean the film to be coated. The surface of the substrate 2 is first cleaned to obtain a substrate I having a surface water droplet angle not greater than 20°, and an antiglare coating is sprayed on the surface of the substrate I by an antiglare spray gun 5 to obtain a substrate II containing an AG film;

(2) introducing the substrate II into the chamber B through the transfer mechanism 3, and performing curing treatment under the action of the heating tube 6 to obtain the substrate III;

(3) introducing the substrate III into the chamber C through the transfer mechanism 3, performing the second cleaning through the cooperation of the cleaning spray gun 7 and the brush 8, and then drying under the action of the hot air knife 9 to obtain the substrate IV;

(4) The substrate IV is introduced into the chamber D through the transfer mechanism 3, oxygen and inert gas are introduced, and the metal target 10 is energized first, so that the metal and oxygen form a metal oxide, and are bombarded by inert gas molecules Deposit on the surface of the substrate IV, and then energize the silicon target 11 to form silicon dioxide with silicon and oxygen, and deposit it on the surface of the substrate IV by bombardment of inert gas molecules, repeat the above steps until the thickness of the AR film reaches 230-270nm, and then The AF agent is placed in the tray 12, and the active ingredient is evaporated and deposited on the surface of the substrate IV by heating; wherein, the oxygen content in the metal oxide layer is lower than the oxygen content in the silicon oxide layer .

The present invention will be described in detail below by way of examples. In the following examples, unless otherwise specified, all raw materials and instruments used are commercially available.

Substrate to be coated: Panda MN228 glass from Sichuan Hongke Innovation Technology Co., Ltd.;

Antiglare coating: the grade is AG180, purchased from PPG Coatings (Tianjin) Co., Ltd.;

AF agent: the brand is H6500D, purchased from Shengyuan Lubricating Materials Co., Ltd.;

Neutral lotion: the brand is L-1012, purchased from Shenzhen Nanxiang Environmental Protection Technology Co., Ltd.;

In the following example, the inner cavity diameters of chamber A, chamber B, chamber C and chamber D are all 1500mm, and the inner cavity heights are all 1800mm;

In the chamber A, the distance between two adjacent plasma cleaning guns is 60 mm, and the distance between two adjacent anti-glare spray guns is 60 mm;

In the chamber B, the distance between two adjacent heating tubes is 40 mm, the length of each heating tube is 1200 mm, and the diameter of each heating tube is 20 mm;

In the following examples, the transfer mechanisms are all manipulators, and the power densities of the metal target and the silicon target are both 5W/cm ² .

Example 1

This embodiment provides a method for continuously preparing AG film, AR film and AF film, the method comprising:

(1) Paste 80 substrates to be coated on the jig, then preheat the jig with the substrate to be coated (at a temperature of 80°C, for 30s), and transfer the jig with the substrate to be coated The jig of the substrate to be coated is introduced into the chamber A, and the surface of the substrate to be coated is cleaned with a plasma cleaning gun to obtain a substrate I with a surface water droplet angle of 5°, and the anti-glare spray gun is used to clean the surface of the substrate to be coated. The dazzling coating is sprayed on the surface of the substrate I to obtain the substrate II containing the AG film; the average thickness of the AG film is 120nm;

Wherein, the first cleaning adopts rotary spray gun plasma cleaning, and the conditions of the first cleaning are: 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 conditions of the spraying are: the surface linear velocity of the substrate 1 is 1000mm/s, the spraying distance is 80mm, the temperature is 80°C, the spray gun atomization pressure is 0.4MPa, the spray gun fan pressure is 0.4MPa, the supply of the antiglare coating The pressure is 0.4MPa, and the flow rate of the antiglare coating is 10g/min;

(2) introducing the substrate II into the chamber B through the transfer mechanism, and performing curing treatment under the action of the heating tube to obtain the substrate III;

Among them, the conditions of curing treatment are: the temperature is 150°C, and the time is 60 minutes;

(3) introduce the substrate III into the chamber C through a transfer mechanism, use a cleaning spray gun to spray neutral lotion, deionized water and acetone in sequence, and clean the substrate III for 3 minutes, 5 minutes and 5 minutes, respectively. III 4min, during the aforementioned cleaning process, continue to rotate the brush to wipe the surface of the substrate III, and then dry it under the action of a hot air knife to obtain the substrate IV;

Wherein, the conditions of the drying treatment are: the temperature is 100° C., and the time is 30 minutes;

(4) The substrate IV is introduced into the chamber D through a transfer mechanism, and oxygen and argon are introduced, and the metal target is energized first, so that the metal and oxygen form a metal oxide, which is bombarded by argon molecules and deposited on the Substrate IV surface, and then energize the silicon target, so that silicon and oxygen form silicon dioxide, and deposit it on the substrate IV surface by bombardment of argon gas molecules, repeat the above steps until the thickness of the AR film reaches 260mm, and then place the AF agent on In the tray, under vacuum conditions (vacuum degree is 1×10 ^{- 5} Pa), the active ingredient in the AF agent is evaporated and deposited on the surface of the substrate IV; wherein, the average thickness of the AF film is 30nm, and the metal oxide layer The oxygen content is 50% by volume lower than the oxygen content in the silicon oxide layer.

Example 2

This embodiment provides a method for continuously preparing AG film, AR film and AF film, the method comprising:

(1) Paste 20 substrates to be coated on the jig, then preheat the jig with the substrates to be coated (at a temperature of 90°C, for 60s), and transfer the jig with the substrate to be coated The jig of the substrate to be coated is introduced into the chamber A, and the surface of the substrate to be coated is cleaned with a plasma cleaning gun to obtain a substrate I with a surface water droplet angle of 5°, and the anti-glare spray gun is used to clean the surface of the substrate to be coated. The dazzling coating is sprayed on the surface of the substrate I to obtain the substrate II containing the AG film; the average thickness of the AG film is 210nm;

Wherein, the first cleaning adopts rotary spray gun plasma cleaning, and the conditions of the first cleaning are: 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 conditions of the spraying are: the surface linear velocity of the substrate 1 is 800mm/s, the spraying distance is 90mm, the temperature is 90°C, the spray gun atomization pressure is 0.45MPa, the spray gun fan pressure is 0.45MPa, the supply of the antiglare coating The pressure is 0.4MPa, and the flow rate of the antiglare coating is 15g/min;

(2) introducing the substrate II into the chamber B through the transfer mechanism, and performing curing treatment under the action of the heating tube to obtain the substrate III;

Among them, the conditions of curing treatment are: the temperature is 200°C, and the time is 50 minutes;

(3) introduce the substrate III into the chamber C through a transfer mechanism, use a cleaning spray gun to spray neutral lotion, deionized water and acetone in sequence to the substrate III, and clean the substrate III in turn for 13 min, Cleaning II for 5 minutes and cleaning III for 4 minutes. During the aforementioned cleaning process, continuously rotate the brush to wipe the surface of the substrate III, and then perform drying treatment under the action of a hot air knife to obtain the substrate IV;

Wherein, the conditions of the drying treatment are: the temperature is 150° C., and the time is 20 minutes;

(4) The substrate IV is introduced into the chamber D through a transfer mechanism, and oxygen and argon are introduced, and the metal target is energized first, so that the metal and oxygen form a metal oxide, which is bombarded by argon molecules and deposited on the Substrate IV surface, then energize the silicon target to make silicon and oxygen form silicon dioxide, and deposit it on the substrate IV surface by bombardment of argon gas molecules, repeat the above steps until the thickness of the AR film reaches 240mm, and then place the AF agent on In the tray, under vacuum conditions (vacuum degree is 1×10 ^{- 5} Pa), the active ingredient in the AF agent is evaporated and deposited on the surface of the substrate IV; wherein, the average thickness of the AF film is 30nm, and the metal oxide layer The oxygen content is 40% by volume lower than the oxygen content in the silicon oxide layer.

Example 3

This embodiment provides a method for continuously preparing AG film, AR film and AF film, the method comprising:

(1) Paste 50 substrates to be coated on the jig, then preheat the jig with the substrate to be coated (at a temperature of 40°C and for 0.8 min), and transfer the set The jig with the substrate to be coated is introduced into the chamber A, and the surface of the substrate to be coated is cleaned with a plasma cleaning gun to obtain a substrate I with a surface water droplet angle of 8°, and the surface of the substrate to be coated is cleaned by an anti-glare spray gun. The anti-glare paint is sprayed on the surface of the substrate I to obtain the substrate II containing the AG film; the average thickness of the AG film is 300nm;

Wherein, the first cleaning adopts rotary spray gun plasma cleaning, and the conditions of the first cleaning are: 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 conditions of the spraying are: the surface linear velocity of the substrate 1 is 600mm/s, the spraying distance is 110mm, the temperature is 40°C, the spray gun atomization pressure is 0.5MPa, the spray gun fan pressure is 0.5MPa, the supply of the antiglare coating The pressure is 0.5MPa, and the flow rate of the antiglare coating is 20g/min;

(2) introducing the substrate II into the chamber B through the transfer mechanism, and performing curing treatment under the action of the heating tube to obtain the substrate III;

Among them, the conditions of curing treatment are: the temperature is 350°C, and the time is 30 minutes;

(3) introduce the substrate III into the chamber C through a transfer mechanism, use a cleaning spray gun to spray neutral lotion, deionized water and acetone in sequence to the substrate III, and clean the substrate III in turn for 13 min, Cleaning II for 5 minutes and cleaning III for 4 minutes. During the aforementioned cleaning process, continuously rotate the brush to wipe the surface of the substrate III, and then perform drying treatment under the action of a hot air knife to obtain the substrate IV;

Wherein, the conditions of the drying treatment are: the temperature is 180° C., and the time is 10 minutes;

(4) The substrate IV is introduced into the chamber D through a transfer mechanism, and oxygen and argon are introduced, and the metal target is energized first, so that the metal and oxygen form a metal oxide, which is bombarded by argon molecules and deposited on the Substrate IV surface, then energize the silicon target to make silicon and oxygen form silicon dioxide, and deposit it on the substrate IV surface by bombardment of argon gas molecules, repeat the above steps until the thickness of the AR film reaches 250mm, and then place the AF agent on In the tray, under vacuum conditions (vacuum degree is 1×10 ^{- 5} Pa), the active ingredient in the AF agent is evaporated and deposited on the surface of the substrate IV; wherein, the average thickness of the AF film is 30nm, and the metal oxide layer The oxygen content is 60% by volume lower than the oxygen content in the silicon oxide layer.

Example 4

Prepare AG film, AR film and AF film continuously according to the method for embodiment 1, difference is, in step (1), control the condition of described first cleaning, so that the surface drop angle of described substrate 1 is 15 °.

Example 5

AG film, AR film and AF film were prepared continuously according to the method of Example 1, except that in step (1), the power of the first cleaning was 500W.

Example 6

AG film, AR film and AF film are prepared continuously according to the method of Example 1, the difference is that in step (4), the oxygen content in the metal oxide layer is higher than the oxygen content in the oxide layer of silicon The content is as low as 80% by volume.

Comparative example 1

Prepare AG film, AR film and AF film continuously according to the method for embodiment 1, difference is, in step (1), control the condition of described first cleaning, so that the surface water drop angle of described substrate 1 is 25 °.

Comparative example 2

Continuously prepare AG film, AR film and AF film according to the method of Example 1, the difference is that in step (4), the oxygen content in the metal oxide layer is the same as the oxygen content in the oxide layer of silicon The content is the same.

Comparative example 3

AG film, AR film and AF film are prepared continuously according to the method of Example 1, the difference is that in step (4), the oxygen content in the metal oxide layer is higher than the oxygen content in the oxide layer of silicon The content is higher than 40% by volume.

test case 1

Two substrates II containing the AG film prepared in Example 1 were randomly selected for performance testing, and a control group was set up. The specific test results are shown in Table 1.

Wherein, the setting method of the control group is: the method is similar to step (1) in Example 1, the difference is that in the process of spraying the anti-glare coating, the film substrate 1 is placed parallel to the ground, and then the anti-glare spray gun is used Antiglare coating is sprayed on the surface of described substrate 1;

The test method for 60° gloss is: BYK 60° gloss meter, measure 2 points for each piece of sample;

The test method of haze is: BYK4775 transmission haze meter, each sample is measured at 2 points;

The test method for the thickness of the AG film layer is: Mitutoyo SJ-410 tester, Free condition measurement, 2 points for each sample.

Table 1

From the results in Table 1, it can be seen that the AG film obtained by the method provided by the present invention still maintains stable film thickness uniformity under different glossiness and haze.

test case 2

One piece of the substrate II containing the AG film prepared in Example 1, Example 2 and Example 3 was randomly selected for performance testing, and three measurement points were randomly selected on each substrate. The specific test results are shown in Table 2.

Among them, the test method of pencil hardness is: Japan Mitsubishi pencil, load 750g, angle 45°, the pencil to be tested passes 5 traces of 2cm, and scratches ≤ 2 passes;

橡皮擦，载重500g，速度40次/min，摩擦1500次，目视及显微镜观察膜层表现；The test method of friction resistance is:

Eraser, load 500g, speed 40 times/min, rub 1500 times, visually and microscopically observe the performance of the film layer;

The test method of adhesion (100 grids) is as follows: on the surface of the AG layer, 11 horizontal and vertical lines are carved with a carving knife to form a square area containing 100 squares. The tape is pasted repeatedly for 3 times, and the surface does not fall off, which is recorded as 5B.

Table 2

As can be seen from the results in Table 2, the hardness, friction resistance and adhesion (100 grids) tests of the AG film layer obtained by the method provided by the present invention all meet the standards, and the film layer has good stability.

Test case 3

One AR film prepared in Example 1, Example 2, and Example 3 was randomly selected for performance testing, and two measurement points were randomly selected on each substrate. The specific test results are shown in Table 3.

Among them, the method of testing L, a, b and y values by SCI method is: SPECTROPHOTOMETER CM-26d color measuring instrument, each piece of sample is tested at two points, and the SCI mode data is recorded;

The method for testing L, a, b and y values by SCE method is: SPECTROPHOTOMETER CM-26d color measuring instrument, two points are tested for each sample, and the SCE mode data is recorded.

table 3

It can be seen from the results in Table 3 that the AR film obtained by the method provided by the present invention has good stability of L, a, b and y values.

Test case 4

The substrates containing AG film, AR film and AF film prepared in Examples and Comparative Examples were tested for performance, and the specific test results are shown in Table 4.

Among them, the test method of pencil hardness is: Japan Mitsubishi pencil, load 750g, angle 45°, the pencil to be tested passes 5 traces of 2cm, and scratches ≤ 2 passes;

The test method of friction resistance is: LIBERON0000# steel wool, load 500g, speed 40 times/min, rub 1500 times, test the water drop angle before and after friction, ≥110° before friction, and ≥100° after friction;

The test method of water drop angle is: SINDIN water contact angle measuring instrument measures the water drop angle at the same position before and after friction, and records the change.

Use the aforementioned pencil hardness test method to scratch ≤ 2 lines and the water drop angle after the friction resistance test is ≥ 100°, which is a good product; the calculation formula for the good product rate is: (number of good products/total number of samples) × 100%.

Table 4

pencil hardness Water drop angle before friction,° Water drop angle after friction,° Yield rate,% 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, the method provided by the invention can continuously prepare AG film, AR film and AF film on the glass cover plate, and the prepared product has high yield, stable performance and good uniformity features.

The preferred embodiments of the present invention have been described in detail above, however, the present invention is not limited thereto. Within the scope of the technical concept of the present invention, various simple modifications can be made to the technical solution of the present invention, including the combination of various technical features in any other suitable manner, and these simple modifications and combinations should also be regarded as the content disclosed in the present invention. All belong to the protection scope of the present invention.

Claims (10)

1. A method for continuously preparing AG film, AR film and AF film is characterized in that the method comprises: (1) Introduce the substrate to be coated into the chamber A for the first cleaning to obtain a substrate I with a surface water drop angle not greater than 20°, and spray an anti-glare coating on the surface of the substrate I to obtain a substrate containing an AG film II; (2) introducing the substrate II into the chamber B for curing treatment to obtain the substrate III; (3) introducing the substrate III into the chamber C to perform the second cleaning and drying treatment sequentially to obtain the substrate IV; (4) introducing the substrate IV into the chamber D to form an AR film and an AF film; wherein, the method for forming the AR film includes: in the presence of a protective atmosphere, alternately depositing metal oxide layers and silicon on the surface of the substrate IV oxide layer, and the oxygen content in the metal oxide layer is lower than the oxygen content in the silicon oxide layer. 2. The method according to claim 1, characterized in that, in step (4), the oxygen content in the metal oxide layer is 40-60% by volume lower than the oxygen content in the silicon oxide layer ; Preferably, in step (4), the main component of the metal oxide layer is niobium pentoxide and/or titanium dioxide. 3. method according to claim 1 and 2, is characterized in that, in step (1), the condition of described first cleaning is controlled, so that the surface drop angle of described substrate 1 is not more than 10 °; Preferably, in step (1), plasma cleaning is used for the first cleaning, and the power of the plasma cleaning is 500-1500W, preferably 700-1200W. 4. The method according to any one of claims 1-3, characterized in that, in step (1), the method further comprises: before performing the first cleaning, preheating the substrate to be coated deal with; Preferably, in step (1), the conditions of the preheating treatment include at least: a temperature of 20-400°C, preferably 30-120°C; and a time of 12-60s. 5. according to the method described in any one in claim 1-4, it is characterized in that, in step (1), described spraying carries out under the condition that described substrate 1 rotates, and the surface line of described substrate 1 The speed is 300-1200mm/s; Preferably, in step (1), the spraying conditions at least include: the spraying distance is 80-150mm, the temperature is 20-130°C, the spray gun atomization pressure is 0.1-0.6MPa, and the spray gun fan pressure is 0.1-0.6MPa , the supply pressure of the anti-glare coating is 0.1-0.6MPa, and the flow rate of the anti-glare coating is 1-30g/min. 6. The method according to any one of claims 1-5, characterized in that, in step (2), the conditions of the curing treatment at least include: a temperature of 130-400° C. and a time of 20-60 minutes. 7. according to the method described in any one in claim 1-6, it is characterized in that, in step (3), described second cleaning comprises adopting neutral lotion to clean I, adopting water to clean II and using Acetone for cleaning III; Preferably, in step (3), the conditions of the drying treatment at least include: a temperature of 100-180° C. and a time of 10-30 minutes. 8. The method according to any one of claims 1-7, characterized in that, 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°C. 9. A system for continuously preparing AG film, AR film and AF film, characterized in that the system comprises: jig, the jig is used to fix the substrate to be coated; Chamber A, a plasma cleaning gun array and an anti-glare spray gun array are arranged side by side in the chamber A, and the plasma cleaning gun array includes at least 2 plasma cleaning guns, and the distance between two adjacent plasma cleaning guns is 40- 80mm; the anti-glare spray gun array includes at least 2 anti-glare spray guns, and the distance between two adjacent anti-glare spray guns is 60-100mm, and the chamber A is used for the first cleaning of the substrate to be coated and the formation of an AG film; A chamber B, at least two heating tubes are uniformly arranged inside the chamber B, and the distance between two adjacent heating tubes is 20-100mm, and the chamber B is used for curing the AG film; The chamber C is provided with a cleaning spray gun, a hair brush and a hot air knife, the cleaning spray gun is vertically arranged on the inner wall of the chamber C, and the nozzle of the cleaning spray gun is vertically arranged towards the substrate III, so The brush is arranged tangentially to the jig, the hot air knife is vertically arranged on the inner wall of the chamber C, and the air outlet of the hot air knife is arranged toward the substrate III, and the chamber C is further below Equipped with a liquid gas recovery port; A chamber D is provided with a metal target, a silicon target and a tray for placing AF agents, and the chamber D is used for forming an AR film and an AF film. 10 . The system according to claim 9 , further comprising a transfer mechanism capable of transferring the jig between chambers, and the transfer mechanism is a robot arm. 11 .

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