CN104611675A - Magnetron sputtering coating equipment and preparation method of ITO (indium tin oxide) glass - Google Patents
Magnetron sputtering coating equipment and preparation method of ITO (indium tin oxide) glass Download PDFInfo
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- CN104611675A CN104611675A CN201510014091.9A CN201510014091A CN104611675A CN 104611675 A CN104611675 A CN 104611675A CN 201510014091 A CN201510014091 A CN 201510014091A CN 104611675 A CN104611675 A CN 104611675A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/56—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
- C23C14/568—Transferring the substrates through a series of coating stations
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Abstract
The invention relates to magnetron sputtering coating equipment and a preparation method of ITO (indium tin oxide) glass. The magnetron sputtering coating equipment comprises a coating chamber, a first transition chamber, a second transition chamber, a buffer chamber and an outlet locking chamber that are sequentially connected, wherein the first transition chamber, the second transition chamber, the buffer chamber and the outlet locking chamber are internally provided with heaters. After an ITO film is coated in the coating chamber, a glass substrate coated with the ITO film sequentially passes through the first transition chamber, the second transition chamber, the buffer chamber and the outlet locking chamber to be gradually cooled, so that internal stress of the ITO film is released, the rigidity of the ITO film is reduced, and the ITO glass with relatively high flexibility is prepared.
Description
Technical field
The present invention relates to coating technique field, particularly relate to the preparation method of a kind of magnetic-controlled sputtering coating equipment and ito glass.
Background technology
ITO (tin indium oxide) is N-shaped polycrystalline state thin-film material, is transparent conductive material most widely used in flat pannel display, touch-control etc. at present.No matter be LCD, resistive touch screen or capacitive touch screen, adopt ito glass as its transparent conductive substrate at present all in a large number.Ito glass comprises glass substrate and is laminated in the ito thin film on glass substrate.
Along with the products such as Flexible Displays, touch-control such as Flexible Displays, flexible touch-control, curved-surface display, curved surface touch-control are increasing, new demand is proposed to the snappiness of transparent conductive substrate, flexible ability.
But, current ito glass many employings magnetron sputtering mode is produced, be limited by production unit and production technique, the internal stress of ito thin film is comparatively large, hardness is higher, and snappiness is not enough, phenomenons such as being difficult to avoid ito thin film not plan a successor in following process, use procedure, ftractureing, come off, is thus difficult to the demand meeting Flexible Displays product.
Summary of the invention
Based on this, be necessary to provide a kind of magnetic-controlled sputtering coating equipment, for the preparation of the ito glass that snappiness is higher.
Further, a kind of preparation method of ito glass is provided.
A kind of magnetic-controlled sputtering coating equipment, comprises plated film chamber connected successively, First Transition room, the second transition chamber, surge chamber and outlet lock chamber, is provided with well heater in described First Transition room, the second transition chamber, surge chamber and outlet lock chamber.
Wherein in an embodiment, the length of described First Transition room is 0.9m ~ 3.6m, and the length of described second transition chamber is 0.9m ~ 3.6m, and the length of described surge chamber is 0.9m ~ 3.6m, and the length of described outlet lock chamber is 0.9m ~ 3.6m.
Wherein in an embodiment, described plated film chamber is connected by the first valve with described First Transition room, described First Transition room is connected by the second valve with described second transition chamber, described second transition chamber is connected by the 3rd valve with described surge chamber, and described surge chamber is connected by the 4th valve with described outlet lock chamber.
Wherein in an embodiment, also comprise the heating chamber be connected with described outlet lock chamber and the 5th cooling room be connected with described heating chamber.
A preparation method for ito glass, comprises the steps:
Glass substrate is provided;
Make described glass substrate move in the plated film chamber of above-mentioned magnetic-controlled sputtering coating equipment, adopt magnetron sputtering to prepare ito thin film on described glass substrate, wherein, the design temperature of plated film chamber is 380 DEG C ~ 600 DEG C;
By having plated the described glass substrate of ito thin film successively by running out described magnetic-controlled sputtering coating equipment after described First Transition room, the second transition chamber, surge chamber and outlet lock chamber, obtain ito glass; Wherein, the design temperature that the design temperature controlling described First Transition room by described well heater is 300 DEG C ~ 500 DEG C, the design temperature of described second transition chamber is 250 DEG C ~ 400 DEG C, the design temperature of described surge chamber is 100 ~ 300 DEG C and described outlet lock chamber is 20 DEG C ~ 200 DEG C.
Wherein in an embodiment, described employing magnetron sputtering is prepared in the step of ito thin film on described glass substrate, and the travelling speed of described glass substrate is 0.6m/min ~ 2.5m/min.
Wherein in an embodiment, the described described glass substrate having plated ito thin film is 0.6m/min ~ 2.5m/min by the travelling speed running out described magnetic-controlled sputtering coating equipment after described First Transition room, the second transition chamber, surge chamber and outlet lock chamber successively.
Wherein in an embodiment, the opening time of the first valve of described magnetic-controlled sputtering coating equipment, the second valve, the 3rd valve and the 4th valve is 0.01s ~ 0.2s, and the turn-off time of described first valve, the second valve, the 3rd valve and the 4th valve is 0.01s ~ 0.2s.
Wherein in an embodiment, also be included in the heating chamber of described magnetic-controlled sputtering coating equipment the step described ito glass being heated and in described 5th cooling room, described ito glass is cooled, the design temperature of described heating chamber is 200 DEG C ~ 400 DEG C, the design temperature of described 5th cooling room is 50 DEG C ~ 300 DEG C, and the pressure in described heating chamber and described 5th cooling room is normal atmosphere.
Wherein in an embodiment, described ito glass is 0.6m/min ~ 5m/min at the operating rate of described heating chamber, and described ito glass is 0.6m/min ~ 5m/min at the operating rate of described 5th cooling room.
Above-mentioned magnetic-controlled sputtering coating equipment is by arranging the plated film chamber be connected successively, First Transition room, second transition chamber, surge chamber and outlet lock chamber, and First Transition room, second transition chamber, well heater is provided with in surge chamber and outlet lock chamber, First Transition room can be controlled respectively by well heater, second transition chamber, the temperature of surge chamber and outlet lock chamber, after making to be coated with ito thin film in plated film chamber, plate the glass substrate of ito thin film successively by First Transition room, second transition chamber, surge chamber and outlet lock chamber cool gradually, to discharge the internal stress of ito thin film, reduce the hardness of ito thin film, the ito glass that preparation snappiness is higher.
Accompanying drawing explanation
Fig. 1 is the structural representation of the magnetic-controlled sputtering coating equipment of an embodiment;
Fig. 2 is the schema of the preparation method of the ito glass of an embodiment.
Embodiment
For enabling above-mentioned purpose of the present invention, feature and advantage become apparent more, are described in detail the specific embodiment of the present invention below in conjunction with accompanying drawing.Set forth a lot of detail in the following description so that fully understand the present invention.But the present invention can be much different from alternate manner described here to implement, those skilled in the art can when without prejudice to doing similar improvement when intension of the present invention, therefore the present invention is by the restriction of following public concrete enforcement.
Refer to Fig. 1, the magnetic-controlled sputtering coating equipment 100 of an embodiment, comprise the plated film chamber 10, First Transition room 20, second transition chamber 30, surge chamber 40 and the outlet lock chamber 50 that are connected successively.Plated film chamber 10, First Transition room 20, second transition chamber 30, surge chamber 40 and the linearly formula arrangement of outlet lock chamber 50.
Plated film chamber 10 is for carrying out magnetron sputtering plating.Preferably, in present embodiment, plated film chamber 10 comprises and being connected successively and the first filming room 101, second coating chamber 102 of linearly formula arrangement, the 3rd coating chamber 103, the 4th coating chamber 104, the 5th coating chamber 105, the 6th coating chamber 106, the 7th coating chamber 107, the 8th coating chamber 108 and the 9th coating chamber 109.Wherein, the 9th coating chamber 109 is connected with First Transition room 20.
Arrange nine coating chambers and carry out plated film, be conducive to improving membrane uniformity, multiple cavity plated film, can minimize and divide equally plated film power, be convenient to avoid because the excessive stress in thin film that causes of plated film power is too high simultaneously.Coated heaters 60 (Fig. 1 only indicates one) is provided with, for controlling the temperature of glass substrate in the first filming room 101, second coating chamber 102, the 3rd coating chamber 103, the 4th coating chamber 104, the 5th coating chamber 105, the 6th coating chamber 106, the 7th coating chamber 107, the 8th coating chamber 108 and the 9th coating chamber 109.
Be appreciated that, the first filming room 101, second coating chamber 102, the 3rd coating chamber 103, the 4th coating chamber 104, the 5th coating chamber 105, the 6th coating chamber 106, the 7th coating chamber 107, the 8th coating chamber 108 and the 9th coating chamber 109 are all connected with vaccum-pumping equipment (scheming not mark), for vacuum of finding time to nine coating chambers, to carry out vacuum plating.
Well heater 70 is provided with in First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50.Well heater 70 is set for controlling the temperature of First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50, to realize the slow cooling of ito thin film.
Preferably, well heater 70 is Infrared heaters, to ensure the temperature homogeneity in above-mentioned four cooling rooms.
Preferably, First Transition room 20, second transition chamber 30, surge chamber 40 are all connected with vaccum-pumping equipment (scheming not mark) with outlet lock chamber 50, for controlling the vacuum tightness of First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50, be carry out slow cooling in device interior vacuum environment to make glass substrate and ito thin film.And through the family of power and influence of each transition chamber, realize the change of vacuum tightness between distinct device vacuum cavity, glass is transported to atmospheric pressure environment gradually by vacuum environment, avoid vacuum tightness change suddenly and the glass substrate that causes and ito thin film break.
Preferably, the length of First Transition room 20 is 0.9m ~ 3.6m, the length of the second transition chamber 30 is 0.9m ~ 3.6m, the length of surge chamber 40 is 0.9m ~ 3.6m, the length of outlet lock chamber 50 is 0.9m ~ 3.6m, the length of First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50 is rationally set, the glass substrate having plated ito thin film is made in First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50, to run the suitable time, to obtain good slow cooling effect with suitable operating rate.
Plated film chamber 10 is connected by the first valve (scheming not mark) with First Transition room 20, First Transition room 20 is connected by the second valve (figure does not mark) with the second transition chamber 30, second transition chamber 30 (figure does not mark) is connected by the 3rd valve (figure does not mark) with surge chamber 40, and surge chamber 30 is connected by the 4th valve (figure does not mark) with outlet lock chamber 50.In coating process, glass is fixed on plated film in substrate frame.Along with continuous multiple substrate frame move to different positions time, the first valve, the second valve, the 3rd valve and the 4th valve be in closedown or opened condition.When loading the substrate frame of having plated the glass of ito thin film and running to before a certain cooling room, corresponding valve opening, load the substrate frame of having plated the glass of ito thin film enter next cavity after the family of power and influence namely close.
Preferably, magnetic-controlled sputtering coating equipment 100 also comprises Controlling System (not shown), Controlling System is for controlling the opening and closing etc. of the operation of glass substrate, the work of vaccum-pumping equipment, plated film, the first valve, the second valve, the 3rd valve and the 4th valve, to realize automated job, raise the efficiency.
The glass substrate having plated film to be respectively the cooling time in First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50 cooling room length/operating rate+valve opening time+the valve closes time.Therefore, the first valve, the second valve, the 3rd valve and the opening time of the 4th valve and the length of turn-off time have a certain impact to cooling performance.But also also there is impact to the control of vacuum tightness in the first valve, the second valve, the 3rd valve and the opening time of the 4th valve and the length of turn-off time, therefore, opening time and the turn-off time of the first valve, the second valve, the 3rd valve and the 4th valve is reasonably controlled, reasonably to control vacuum tightness and cooling time by Controlling System.
Above-mentioned magnetic-controlled sputtering coating equipment 100 is by arranging the plated film chamber 10 be connected successively, First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50, and First Transition room 20, second transition chamber 30, well heater 70 is provided with in surge chamber 40 and outlet lock chamber 50, First Transition room 20 can be controlled respectively by well heater 70, second transition chamber 30, the temperature of surge chamber 40 and outlet lock chamber 50, after making to be coated with ito thin film in plated film chamber 10, plate the glass substrate of ito thin film successively by First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50 cool gradually, to discharge the stress of ito thin film, reduce the hardness of ito thin film, the ito glass that preparation snappiness is higher.Be appreciated that the ito glass that snappiness is higher refers to that the snappiness of the ito thin film of ito glass is higher.
Preferably, above-mentioned magnetic-controlled sputtering coating equipment 100 also comprises the heating chamber (not shown) be connected with outlet lock chamber 50 and the 5th cooling room (not shown) be connected with heating chamber.Heating chamber and the 5th cooling room are used for processing further ito glass, to discharge the stress of ito thin film further, improve the snappiness of ito thin film.
Refer to Fig. 2, the preparation method of the ito glass of an embodiment, comprise the steps that S110 is to step S30.
Step S110: glass substrate is provided.
Glass substrate can be the glass of float glass or other this area routines.Cleaning glass substrate is also dry, for subsequent use.
Step S120: glass substrate is fixed in substrate frame.Substrate frame moves in the plated film chamber 10 of above-mentioned magnetic-controlled sputtering coating equipment 100, and adopt magnetron sputtering to prepare ito thin film on the glass substrate, wherein, the design temperature of plated film chamber is 380 DEG C ~ 600 DEG C.
Preferably, under vacuum tightness is 0.1Pa ~ 0.5Pa, magnetron sputtering plating is carried out.The design temperature of plated film chamber is 380 ~ 600 DEG C.
Preferably, in coating process, the operating rate of glass substrate is 0.6m/min ~ 2.5m/min.
The sputtering voltage of the ITO target of magnetron sputtering is 200V ~ 450V, and power is 1Kw ~ 60Kw.
Step S130: by having plated the glass substrate of ito thin film successively by running out magnetic-controlled sputtering coating equipment 100 after First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50, plated the ito glass of film; Wherein, the design temperature that the design temperature controlling First Transition room 20 by well heater 70 is 300 DEG C ~ 500 DEG C, the design temperature of the second transition chamber 30 is 250 DEG C ~ 400 DEG C, the design temperature of surge chamber 40 is 100 DEG C ~ 300 DEG C and outlet lock chamber 50 is 20 DEG C ~ 200 DEG C.
The temperature being controlled First Transition room 20 by well heater 70 is 300 ~ 500 DEG C, the temperature of the second transition chamber 30 is 250 ~ 400 DEG C, the temperature of surge chamber 40 is 100 ~ 300 DEG C and the temperature that controls outlet lock chamber 50 is 20 ~ 200 DEG C, realize the processing condition set preferably, the glass substrate having plated ito thin film is cooled gradually, realize slow cooling, to discharge the internal stress of ito thin film, improve the snappiness of ito thin film.
Be appreciated that, the design temperature of plated film chamber can need any one temperature in selection 380 DEG C ~ 600 DEG C according to ITO resistance, the set temperature value of First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50 can be chosen respectively from said temperature scope, but should ensure that the design temperature of plated film chamber and the design temperature of First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50 reduce, successively to realize slow cooling.
Preferably, the design temperature of plated film chamber is 480 DEG C, and the design temperature of First Transition room 20 is 400 DEG C, and the design temperature of the second transition chamber 30 is 350 DEG C, and the design temperature of surge chamber 40 is 200 DEG C, and the design temperature of outlet lock chamber 50 is 20 DEG C.
Preferably, the glass substrate having plated ito thin film is 0.6m/min ~ 2.5m/min by the travelling speed running out magnetic-controlled sputtering coating equipment 100 after First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50 successively.
Preferably, the opening time of the first valve of magnetic-controlled sputtering coating equipment 100, the second valve, the 3rd valve and the 4th valve is 0.01s ~ 0.2s, and the turn-off time of the first valve, the second valve, the 3rd valve and the 4th valve is 0.01s ~ 0.2s.
By rationally arranging the temperature of First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50 and having plated the operating rate of glass substrate in First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50 of ito thin film, and accurately control opening time and the turn-off time of the first valve, the second valve, the 3rd valve and the 4th valve, to realize preferably slow cooling effect, to control the snappiness of ito thin film preferably.
Preferably, carrying out in the process cooled, the vacuum tightness of First Transition room 20 is 0.003Pa ~ 0.5Pa, the vacuum tightness of the second transition chamber 30 is 0.003Pa ~ 0.5Pa, and the vacuum tightness of surge chamber 40 is 0.003Pa ~ 0.5Pa, and the vacuum tightness of outlet lock chamber 50 is 0.003Pa ~ 0.5Pa.
The glass substrate having plated ito thin film, successively after the cooling of First Transition room 20, second transition chamber 30, surge chamber 40 and outlet lock chamber 50, obtains ito glass.In a preferred embodiment, step ito glass being heated and cools in the 5th cooling room is also comprised.
Preferably, the design temperature of heating chamber is 200 DEG C ~ 400 DEG C.When the temperature of ito glass is successively through First Transition room 20, second transition chamber 30, after cooling down after surge chamber 40 and outlet lock chamber 50, cooling ito glass enter in heating chamber, ito glass is heated to the Tc point more than 180 DEG C of ITO, then temperature is moved in the 5th cooling room higher than the ito glass of the Tc point more than 180 DEG C of ITO and cool, larger stress-difference is there is to avoid the internal layer of ito glass and skin, thus discharge ito glass internal stress as far as possible, avoid stress excessive and easy to crack, realize the flexible lifting of ito thin film.Preferably, the design temperature of the 5th cooling room is 50 DEG C ~ 300 DEG C.
Utilize heating chamber to carry out heating and utilize the 5th cooling room to carry out in the process cooled, the pressure in heating chamber and the 5th cooling room is normal atmosphere.
Preferably, ito glass is 0.6m/min ~ 5m/min at the operating rate of heating chamber, and ito glass is 0.6m/min ~ 5m/min at the operating rate of the 5th cooling room.
After the preparation method of above-mentioned ito glass prepares ito thin film at a higher temperature on the glass substrate, successively through First Transition room 20, second transition chamber 30 that excess temperature reduces gradually, surge chamber 40 and outlet lock chamber 50, temperature is reduced gradually, realize slow cooling, the mode of this slow cooling can discharge the internal stress of ito thin film, thus mentions the snappiness of ito thin film.
The preparation method of above-mentioned ito glass effectively can discharge the stress of ito thin film to improve the snappiness of ito thin film under the condition of crystalline state not changing ito thin film, can ensure the quality of ito thin film improving ito thin film flexible while.
Set forth further below by way of specific embodiment.
Embodiment 1
Prepare ito glass
1, by cleaning glass substrate and drying for standby.
2, make cleaning, dry glass substrate moves in the plated film chamber of magnetic-controlled sputtering coating equipment, magnetron sputtering is adopted to prepare ito thin film on the glass substrate, wherein, the design temperature of plated film chamber is 600 DEG C, vacuum tightness is 0.3Pa, the operating rate of glass substrate is 1.8m/min, and the voltage of magnetron sputtering is 315V, and power is 6Kw.
3, by having plated the glass substrate of ito thin film successively by running out magnetic-controlled sputtering coating equipment after First Transition room, the second transition chamber, surge chamber and outlet lock chamber, ito glass is obtained, wherein, the temperature being controlled First Transition room by well heater is 400 DEG C, the temperature of the second transition chamber is 350 DEG C, the temperature of surge chamber is the temperature of 300 DEG C and outlet lock chamber is 200 DEG C, the vacuum tightness of First Transition room is 0.05Pa, the vacuum tightness of the second transition chamber is 0.05Pa, the vacuum tightness of surge chamber is 0.008Pa, the vacuum tightness of outlet lock chamber is 0.3Pa, plate the glass substrate of ito thin film successively by First Transition room, second transition chamber, the operating rate running out magnetic-controlled sputtering coating equipment after surge chamber and outlet lock chamber is 1.8m/min, first valve, second valve, the opening time of the 3rd valve and the 4th valve is 0.05s, first valve, second valve, the turn-off time of the 3rd valve and the 4th valve is 0.05s.
Embodiment 2
Prepare ito glass
1, by cleaning glass substrate and drying for standby.
2, make cleaning, dry glass substrate moves in the plated film chamber of magnetic-controlled sputtering coating equipment, magnetron sputtering is adopted to prepare ito thin film on the glass substrate, wherein, coating temperature is 480 DEG C, vacuum tightness is 0.2Pa, the operating rate of glass substrate is 1.6m/min, and the voltage of magnetron sputtering is 350V, and power is 48Kw.
3, by having plated the glass substrate of ito thin film successively by running out magnetic-controlled sputtering coating equipment after First Transition room, the second transition chamber, surge chamber and outlet lock chamber, ito glass is obtained, wherein, the temperature being controlled First Transition room by well heater is 400 DEG C, the temperature of the second transition chamber is 350 DEG C, the temperature of surge chamber is the temperature of 300 DEG C and outlet lock chamber is 200 DEG C, the vacuum tightness of First Transition room is 0.08Pa, the vacuum tightness of the second transition chamber is 0.08Pa, the vacuum tightness of surge chamber is 0.08Pa, the vacuum tightness of outlet lock chamber is 0.009Pa, plate the glass substrate of ito thin film successively by First Transition room, second transition chamber, the operating rate running out magnetic-controlled sputtering coating equipment after surge chamber and outlet lock chamber is 1.5m/min, first valve, second valve, the opening time of the 3rd valve and the 4th valve is 0.05s, first valve, second valve, the turn-off time of the 3rd valve and the 4th valve is 0.05s.
4, above-mentioned ito glass being moved to temperature is in the heating chamber of 250 DEG C, ito glass is heated to 250 DEG C, then the ito glass of 250 DEG C being moved to temperature is in the 5th cooling room of 80 DEG C, ITO runs and leaves heating chamber and the operating rate entering the 5th cooling room is 0.6m/min, and it is 5m/min that ito glass runs the operating rate leaving the 5th cooling room.
Embodiment 3
Prepare ito glass
1, by cleaning glass substrate and drying for standby.
2, make cleaning, dry glass substrate moves in the plated film chamber of magnetic-controlled sputtering coating equipment, magnetron sputtering is adopted to prepare ito thin film on the glass substrate, wherein, coating temperature is 450 DEG C, vacuum tightness is 0.3Pa, the operating rate of glass substrate is 1.2m/min, and the voltage of magnetron sputtering is 350V, and power is 27Kw.
3, by having plated the glass substrate of ito thin film successively by running out magnetic-controlled sputtering coating equipment after First Transition room, the second transition chamber, surge chamber and outlet lock chamber, ito glass is obtained, wherein, the temperature being controlled First Transition room by well heater is 400 DEG C, the temperature of the second transition chamber is 350 DEG C, the temperature of surge chamber is the temperature of 300 DEG C and outlet lock chamber is 200 DEG C, the vacuum tightness of First Transition room is 0.1Pa, the vacuum tightness of the second transition chamber is 0.07Pa, the vacuum tightness of surge chamber is 0.07Pa, the vacuum tightness of outlet lock chamber 50 is 0.006Pa, plate the glass substrate of ito thin film successively by First Transition room, second transition chamber, the operating rate running out magnetic-controlled sputtering coating equipment after surge chamber and outlet lock chamber is 1.2m/min, first valve, second valve, the opening time of the 3rd valve and the 4th valve is 0.05s, first valve, second valve, the turn-off time of the 3rd valve and the 4th valve is 0.05s.
4, above-mentioned ito glass being moved to temperature is in the heating chamber of 300 DEG C, ito glass is heated to 300 DEG C, then the ito glass of 300 DEG C being moved to temperature is in the 5th cooling room of 50 DEG C, ITO runs and leaves heating chamber and the operating rate entering the 5th cooling room is 0.6m/min, and it is 4m/min that ito glass runs the operating rate leaving the 5th cooling room.
Comparative example 1
Prepare ito glass
1, by cleaning glass substrate and drying for standby.
2, make cleaning, dry glass substrate moves in the plated film chamber of magnetic-controlled sputtering coating equipment, magnetron sputtering is adopted to prepare ito thin film on the glass substrate, wherein, the design temperature of plated film chamber is 600 DEG C, vacuum tightness is 0.3Pa, the operating rate of glass substrate is 1.8m/min, and the voltage of magnetron sputtering is 315V, and power is 6Kw.
3, by having plated the glass substrate of ito thin film successively by running out magnetic-controlled sputtering coating equipment after First Transition room, the second transition chamber, surge chamber and outlet lock chamber, ito glass is obtained, wherein, First Transition room, second transition chamber, the temperature of surge chamber and outlet lock chamber is room temperature, the vacuum tightness of First Transition room is 0.08Pa, the vacuum tightness of the second transition chamber is 0.08Pa, the vacuum tightness of surge chamber is 0.08Pa, the vacuum tightness of outlet lock chamber is 0.005Pa, plate the glass substrate of ito thin film successively by First Transition room, second transition chamber, the operating rate running out magnetic-controlled sputtering coating equipment after surge chamber and outlet lock chamber is 1.8m/min, first valve, second valve, the opening time of the 3rd valve and the 4th valve is 0.05s, first valve, second valve, the turn-off time of the 3rd valve and the 4th valve is 0.05s.
Adopt pencil hardometer method to measure the hardness of the ito thin film of the ito glass of above-described embodiment 1 ~ 3 and comparative example 1, test result is as shown in table 1 below.
The hardness of the ito thin film of the ito glass of table 1 embodiment 1 ~ 3 and comparative example 1
| Embodiment and comparative example | Hardness (H) |
| Embodiment 1 | B |
| Embodiment 2 | B |
| Embodiment 3 | B |
| Comparative example 1 | 6H |
Can be found out by upper table 1, the hardness of the ito thin film of the ito glass of embodiment 1 ~ embodiment 3 is lower, illustrates that the snappiness of ito thin film is better, can be improved the snappiness of ito thin film by the mode cooled gradually.
The above embodiment only have expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a magnetic-controlled sputtering coating equipment, it is characterized in that, comprise plated film chamber connected successively, First Transition room, the second transition chamber, surge chamber and outlet lock chamber, in described First Transition room, the second transition chamber, surge chamber and outlet lock chamber, be provided with well heater.
2. magnetic-controlled sputtering coating equipment according to claim 1, it is characterized in that, the length of described First Transition room is 0.9m ~ 3.6m, and the length of described second transition chamber is 0.9m ~ 3.6m, the length of described surge chamber is 0.9m ~ 3.6m, and the length of described outlet lock chamber is 0.9m ~ 3.6m.
3. magnetic-controlled sputtering coating equipment according to claim 1, it is characterized in that, described plated film chamber is connected by the first valve with described First Transition room, described First Transition room is connected by the second valve with described second transition chamber, described second transition chamber is connected by the 3rd valve with described surge chamber, and described surge chamber is connected by the 4th valve with described outlet lock chamber.
4. magnetic-controlled sputtering coating equipment according to claim 1, is characterized in that, also comprises the heating chamber be connected with described outlet lock chamber and the 5th cooling room be connected with described heating chamber.
5. a preparation method for ito glass, comprises the steps:
Glass substrate is provided;
Make described glass substrate move in the plated film chamber of the magnetic-controlled sputtering coating equipment described in any one of Claims 1 to 4, adopt magnetron sputtering to prepare ito thin film on described glass substrate, wherein, the design temperature of plated film chamber is 380 DEG C ~ 600 DEG C;
By having plated the described glass substrate of ito thin film successively by running out described magnetic-controlled sputtering coating equipment after described First Transition room, the second transition chamber, surge chamber and outlet lock chamber, obtain ito glass; Wherein, the design temperature that the design temperature controlling described First Transition room by described well heater is 300 DEG C ~ 500 DEG C, the design temperature of described second transition chamber is 250 DEG C ~ 400 DEG C, the design temperature of described surge chamber is 100 DEG C ~ 300 DEG C and described outlet lock chamber is 20 DEG C ~ 200 DEG C.
6. the preparation method of ito glass according to claim 5, is characterized in that, described employing magnetron sputtering is prepared in the step of ito thin film on described glass substrate, and the travelling speed of described glass substrate is 0.6m/min ~ 2.5m/min.
7. the preparation method of ito glass according to claim 5, it is characterized in that, the described described glass substrate having plated ito thin film is 0.6m/min ~ 2.5m/min by the operating rate running out described magnetic-controlled sputtering coating equipment after described First Transition room, the second transition chamber, surge chamber and outlet lock chamber successively.
8. the preparation method of ito glass according to claim 5, it is characterized in that, the opening time of the first valve of described magnetic-controlled sputtering coating equipment, the second valve, the 3rd valve and the 4th valve is 0.01s ~ 0.2s, and the turn-off time of described first valve, the second valve, the 3rd valve and the 4th valve is 0.01s ~ 0.2s.
9. the preparation method of ito glass according to claim 5, it is characterized in that, also be included in the heating chamber of described magnetic-controlled sputtering coating equipment the step described ito glass being heated and in described 5th cooling room, described ito glass is cooled, the design temperature of described heating chamber is 200 DEG C ~ 400 DEG C, the design temperature of described 5th cooling room is 50 DEG C ~ 300 DEG C, and the pressure in described heating chamber and described 5th cooling room is normal atmosphere.
10. the preparation method of ito glass according to claim 9, it is characterized in that, described ito glass is 0.6m/min ~ 5m/min at the operating rate of described heating chamber, and described ito glass is 0.6m/min ~ 5m/min at the operating rate of described 5th cooling room.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03211275A (en) * | 1989-11-13 | 1991-09-17 | Optical Coating Lab Inc | Device and method for magnetron spattering |
| CN2773098Y (en) * | 2005-03-22 | 2006-04-19 | 无锡康力电子有限公司 | Vacuum cavity for magnetic-controlled sputtering film coating |
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2015
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03211275A (en) * | 1989-11-13 | 1991-09-17 | Optical Coating Lab Inc | Device and method for magnetron spattering |
| CN2773098Y (en) * | 2005-03-22 | 2006-04-19 | 无锡康力电子有限公司 | Vacuum cavity for magnetic-controlled sputtering film coating |
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