CN106637126A - Preparation method of transparent conducting thin film and transparent conducting thin film - Google Patents

Preparation method of transparent conducting thin film and transparent conducting thin film Download PDF

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Publication number
CN106637126A
CN106637126A CN201611021226.5A CN201611021226A CN106637126A CN 106637126 A CN106637126 A CN 106637126A CN 201611021226 A CN201611021226 A CN 201611021226A CN 106637126 A CN106637126 A CN 106637126A
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China
Prior art keywords
base material
transparent conductive
preparation
layer
conductive film
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CN201611021226.5A
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Inventor
李晨光
王培红
胡国栋
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Nanchang OFilm Display Technology Co Ltd
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Nanchang OFilm Display Technology Co Ltd
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Priority to CN201611021226.5A priority Critical patent/CN106637126A/en
Publication of CN106637126A publication Critical patent/CN106637126A/en
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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/56Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks
    • C23C14/562Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/02Pretreatment of the material to be coated
    • C23C14/021Cleaning or etching treatments
    • C23C14/022Cleaning or etching treatments by means of bombardment with energetic particles or radiation
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/06Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
    • C23C14/08Oxides
    • C23C14/086Oxides of zinc, germanium, cadmium, indium, tin, thallium or bismuth
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C14/00Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34Sputtering
    • C23C14/35Sputtering by application of a magnetic field, e.g. magnetron sputtering
    • C23C14/352Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Laminated Bodies (AREA)
  • Physical Vapour Deposition (AREA)

Abstract

The invention discloses a preparation method of a transparent conducting thin film. The preparation method comprises the following steps of loading a base material in a winding and coating machine, vacuumizing the inner part of the winding and coating machine; enabling the base material to enter a pre-treatment chamber, and generating plasma by enabling a gas to be subjected to glow discharge through a pre-treatment device in the pre-treatment chamber, thus removing water vapor on the surface of the base material; plating the surface of the base material with a medium layer and a conducting layer in sequence. Through pre-treatment, the water vapor on the surface of the base material is removed, ITO (Indium Tin Oxide) crystallization is promoted, and the crystallization performance of an ITO conducting thin film layer is increased; the medium layer and the conducting layer are applied on the surface of the base material one after another, and a prepared ITO conducting thin film is low in impedance and better in conductivity. The invention also provides the transparent conducting thin film.

Description

The preparation method and transparent conductive film of transparent conductive film
Technical field
The present invention relates to display technology field, more particularly, to the preparation method and electrically conducting transparent of a kind of transparent conductive film Film.
Background technology
The existing electronic equipment such as intelligent display device such as mobile phone, computer, electronic watch is provided with touch controllable function.Touch screen by Transparent conductive film is etched on the display device different pattern and is combined into touch control unit and electrically connects touch chip realizes touch-control Function, wherein, transparent conductive film it is the most frequently used for tin indium oxide (ITO) conductive film, the preparation technology of ITO conducting films affects The attributes such as resistance value, the transmitance of ITO conductive films, so as to affecting the touch accuracy of equipment, reaction speed, showing clear The characteristics such as degree, have consequence in the manufacture process of display screen.
In prior art, the preparation method of ITO conductive films is directly to be coated with ITO conductive membrane layers in substrate surface, should ITO conductive film impedances prepared by method are higher, and electric conductivity is poor, and the crystallinity of ITO conductive membrane layers is not good.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method and transparent conductive film of transparent conductive film, The ITO conductive film impedances prepared in solve prior art are higher, and electric conductivity is poor, and the knot of ITO conductive membrane layers The not good problem of crystalline substance.
To solve above-mentioned technical problem, on the one hand, the present invention provides a kind of preparation method of transparent conductive film, including:
By base material loaded in winding film coating machine, and will vacuumize inside the winding film coating machine;
The base material enters pre-treatment chamber, and by the pretreating device of the pre-treatment within the chamber gas glow discharge is made Plasma is produced, to remove the steam of the substrate surface;
Dielectric layer and conductive layer are plated successively on the surface of the base material.
It is further, described that " base material enters pre-treatment chamber, is made by the pretreating device of the pre-treatment within the chamber Gas glow discharge generation plasma, to remove the steam of the substrate surface " step includes:The pretreating device is utilized Oxygen and argon gas glow discharge produce the steam that plasma removes the substrate surface.
Further, it is characterised in that the vacuum of the pre-treatment chamber is 1 × 10-4Mbar~9 × 10-3mbar。
Further, described " by base material loaded in winding film coating machine, and vacuumizing inside the winding film coating machine " it Before, methods described also includes:Acryl resin layer is coated in the substrate surface.
Further, the dielectric layer is earth silicon material.
Further, the conductive layer uses In2O3-SnO2Ceramic target is made in the way of magnetron sputtering, and SnO2's Quality accounts for In2O3-SnO2The 0.3%~20% of ceramic target quality.
Further, the In2O3-SnO2In ceramic target, SnO2Quality account for In2O3-SnO2The 8% of ceramic target quality ~10%.
Further, the conductive layer is made using In-Sn metal targets in the way of magnetron sputtering.
It is further, described that " base material enters pre-treatment chamber, is made by the pretreating device of the pre-treatment within the chamber Gas glow discharge produces plasma, to remove the steam of the substrate surface " before, methods described also includes:Start institute The infrared heat riser of the plated film drum of winding film coating machine is stated, the base material is heated to 20 DEG C -250 DEG C, to improve pre-treatment, be coated with Dielectric layer, the effect for being coated with conductive layer.
Further, it is 400V~500V to be coated with the sputtering voltage used during conductive layer.
Further, magnetic control sputtering cathode adopts magnetism intensity for 200G~1000G when being coated with conductive layer.
On the other hand, the present invention also provides a kind of transparent conductive film, and the transparent conductive film includes stacking gradually setting Base material, dielectric layer and the conductive layer put, the base material is the plastic material of polyester resin, and the dielectric layer is inorganic matter or folding Organic matter of the rate between 1.3~1.65 is penetrated, for preventing the sodium ion on the base material from expanding into the liquid crystal cell of display device Dissipate, the conductive layer is tin indium oxide.
Further, the transparent conductive film also includes acryl resin layer, and the acryl resin layer is located at the base Between material and the dielectric layer, for reducing the roughness of the substrate surface.
Beneficial effects of the present invention are as follows:Pre-treatment removes the steam of substrate surface, is conducive to ITO to crystallize, and improves ITO The crystallinity of conductive membrane layer;Substrate surface is first coated with dielectric layer and is coated with conductive layer again, and the ITO conductive film impedances of preparation are low, Electric conductivity is preferable.
Description of the drawings
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing The accompanying drawing to be used needed for having technology description is briefly described, it should be apparent that, drawings in the following description are only this Some embodiments of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can be with Other substantially modes of texturing are obtained according to these accompanying drawings.
Fig. 1 is the flow chart of the preparation method of the transparent conductive film that the embodiment of the present invention one is provided.
Fig. 2 is the structural representation of winding film coating machine.
Fig. 3 is the stepped construction figure of transparent conductive film.
Fig. 4 is the flow chart of the preparation method of the transparent conductive film that the embodiment of the present invention two is provided.
Specific embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than the embodiment of whole.It is based on Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made Embodiment, belongs to the scope of protection of the invention.
Fig. 1 is the flow chart of the preparation method of the transparent conductive film that the embodiment of the present invention one is provided, as illustrated, the system The step of Preparation Method, is as follows:
Step 1, by base material loaded in winding film coating machine, and will vacuumize inside winding film coating machine.
Incorporated by reference to Fig. 2, winding film coating machine includes that what is be sequentially communicated unreels end 10, process part 20 and winding end 30, unreels End 10 is provided with and unreels rod axle 102, winding end 30 and be provided with winding rod axle 302, and process part 20 is provided with plated film drum 200, is processing Base material 11 is looped around and unreels on rod axle 102, and plating is looped around from one end of plated film drum 200 from the base material 11 that rod axle 102 stretches out is unreeled On the surface of film drum 200, base material 11 leaves plated film drum after the surface of plated film drum 200 is rounded from the other end of plated film drum 200 200, the base material 11 for leaving plated film drum 200 is looped around on winding rod axle 302.When winding rod axle 302 is rotated in one direction, receive Volume rod axle 302 is looped around base material 11 on winding rod axle 302, and drive unreels rod axle 102 and rotates, and leaves and unreels rod axle 102 Base material 11 around plated film drum 200 round after be contained on winding rod axle 302.
In present embodiment, process part 20 includes at least two laminating rod axles 22, and laminating rod axle 22 is pasted positioned at base material 11 The position of plated film drum 200 is left in the position and base material 11 of closing plated film drum 200, for reducing the tension force of base material 11, and makes base material 11 are more closely fitted on the surface of plated film drum 200.Further, process part 20 also includes multiple guide bars axles 24, leads It is located to rod axle 24 and unreels between rod axle 102 and plated film drum 200, winds between rod axle 302 and plated film drum 200, for stretching base Material 11 simultaneously guides base material 11 to enter process part 20 and from process part 20 into winding end from end 10 is unreeled along default direction 30, guide bars axle 24 can also reduce the tension force of base material 11.
Process part 20 includes pre-treatment chamber 202, dielectric layer coating chamber 204 and leads according to the order that base material 11 is entered Electric layer coating chamber 206, is respectively used to be processed before the surface of base material 11 is carried out, is coated with dielectric layer and is coated with conductive layer.Pre-treatment Chamber 202, dielectric layer coating chamber 204 and conductive layer coating chamber 206 are the process cavity of autonomous working, and each chamber Between there is certain isolation with ensure base material 11 each within the chamber singly complete manufacturing procedure and by other operations Affect, the present embodiment dielectric layer coating chamber 204 is more than 200 with the isolation of conductive layer coating chamber 206.Further, It is to improve plating membrane efficiency in the present embodiment, process part 20 includes successively 4 dielectric layer coating chambers 204 and 2 conductive layer platings Membrane cavity room 206.
In present embodiment, 1 × 10 is evacuated to inside winding film coating machine-6Below mbar, wherein pre-treatment chamber 202 take out Vacuum is to 1 × 10-4Mbar~9 × 10-3Mbar, dielectric layer coating chamber 204 and conductive layer coating chamber 206 be evacuated to 9 × 10-4Mbar~9 × 10-3mbar。
Base material 11 is loaded into winding film coating machine, and unprocessed base material is exported to process part 20 using rod axle 102 is unreeled 11, the base material 11 of completion of processing is reclaimed from process part 20 using winding rod axle 302, improve the operating efficiency of coating process; Winding film coating machine is vacuumized, and for pre-treatment and coating process necessary processing environment is provided, and is that follow-up work is prepared.
Step 2, base material 11 enter pre-treatment chamber 202, and by the pretreating device in pre-treatment chamber 202 gas brightness is made Light electric discharge produces plasma, to remove the steam on the surface of base material 11.
Before being coated with dielectric layer and conductive layer, base material 11 enters pre-treatment chamber 202 and cleans base material using pretreating device 11 surfaces, to be subsequently coated with dielectric layer and conductive layer the cleaning, the dry substrate 11 that are more easy to be coated with are provided.Specifically, pre-treatment chamber Pre-treatment working gas is filled in room 202, makes its glow discharge produce plasma to pre-treatment working gas applied voltage, works as base When plasma, plasma removes the steam on the surface of base material 11 to material 11, reaches the surface of activated substrate 11, increase ITO and leads Electrolemma provides the cleaning table for being easy to ITO crystallizations in the purpose of the surface adhesion force of base material 11 to be subsequently coated with dielectric layer and conductive layer Face.It is a kind of preferred embodiment in, pre-treatment gas using argon gas and oxygen mixed gas, pre-treatment chamber 202 takes out very It is empty to 1 × 10-4Mbar~9 × 10-3mbar。
In the present embodiment, before processing before carrying out, winding film coating machine starts the heat riser of plated film drum 200, plus hot dip The temperature of film drum 200, specifically, the heat riser of plated film drum 200 is infrared heat riser, and by base material 11 be heated to 20 DEG C~ 250 DEG C, in a kind of preferably embodiment, base material 11 is heated to 80 DEG C~150 DEG C by plated film drum 200.Heated substrate 11, is beneficial to Base material 11 carries out pre-treatment, is coated with dielectric layer, is coated with the operations such as conductive layer, can improve ITO conducting films and be coated with effect.
Step 3, base material 11 enter dielectric layer coating chamber 204, and Jie is coated with base material 11 by the way of magnetron sputtering Matter layer.
Dielectric layer is coated on base material 11 by the way of magnetron sputtering, and the material of dielectric layer can be inorganic matter, for example MgF2、CaF2、SiO2Deng, or organic matter of the refractive index between 1.3~1.65, such as acryl resin, polyurethane tree Fat, melmac etc., also or above-mentioned organic matter and the inorganic matter mixture.
In the present embodiment, dielectric layer material uses SiO2, dielectric layer coating chamber 204 and conductive layer coating chamber 206 it Between need to keep larger isolation, to ensure that the oxygen in dielectric layer coating chamber 204 does not interfere with the formation of ITO conductive layer, tool Body, dielectric layer coating chamber 204 is more than 200 with the isolation of conductive layer coating chamber 206.In a kind of preferred embodiment, it is situated between Matter layer coating chamber 204 is evacuated to 9 × 10-4Mbar~9 × 10-3Mbar, target material surface to the distance on the surface of base material 11 is 30mm~50mm, working gas using argon gas and oxygen mixed gas, the magnetism intensity of magnetic control sputtering cathode be 100G~ 1500G.The surface of base material 11 is first coated with dielectric layer and is coated with conductive layer again, and the ITO conductive film impedances of preparation are low, electric conductivity compared with It is good.
Step 4, base material 11 enter conductive layer coating chamber 206, the plating guidance on dielectric layer by the way of magnetron sputtering Electric layer.
In conductive layer coating chamber 206, adopt the mode of magnetron sputtering be coated with dielectric layer base material 11 on be coated with ITO Conductive film, the target for using for being coated with ITO conductive films is In2O3-SnO2Ceramic target or In-Sn metal targets.This reality In applying example, the use In of ITO conductive films is coated with2O3-SnO2Ceramic target, wherein SnO2Quality account for In2O3-SnO2Ceramic target The 0.3%~20% of material amount, in a kind of preferably embodiment, SnO2Quality account for In2O3-SnO2Ceramic target quality 8%~10%.Working gas used in this step adopts purity for the argon gas of 5N and the mixed gas of oxygen, equal beneficial to being formed Even conductive film layer.Also, the sputtering voltage that magnetron sputtering is adopted is for 400V~500V, conducting film coating chamber vacuum is 9 ×10-4Mbar~9 × 10-3Mbar, the temperature of base material 11 is 80 DEG C -150 DEG C.Magnetic control sputtering cathode adopts magnetism intensity for 200G ~1000G, wherein, 500G~800G best results.The ITO conductive film crystal properties of the conductive layer that this method is coated with technique Good, impedance is low, and electric conductivity is preferable.
Pre-treatment removes the steam on the surface of base material 11, is conducive to ITO to crystallize, and improves the crystallinity of ITO conductive membrane layers; The surface of base material 11 is first coated with dielectric layer and is coated with conductive layer again, and the ITO conductive films transmitance of preparation is high, and impedance is low, conductive Preferably, the impedance of ITO conductive membrane layers is about 100 Ω/ to performance, the impedance of the ITO conductive membrane layers prepared than prior art Little about 50 Ω/.
Fig. 3 show transparent conductive film prepared by the preparation method of the transparent conductive film of the offer of the embodiment of the present invention one Stepped construction schematic diagram.Transparent conductive film includes three layers, is followed successively by base material 11, dielectric layer 12 and conductive layer 13.This enforcement In example, base material 11 selects the plastic material of polyester resin, such as polyethylene terephthalate (Polyethylene Terephthalate, PET) plastics or cyclenes hydrocarbon type copolymer (COC) plastics, the plastics of polyester resin have good saturating Bright property, heat resistance and mechanical property.Preferably, the thickness of base material 11 selects 2mm~100mm.Dielectric layer 12 is inorganic matter or refraction Organic matter of the rate between 1.3~1.65, for preventing the sodium ion on base material 11 from spreading into the liquid crystal cell of display device, leads Electric layer 13 is tin indium oxide.
In the present embodiment, transparent conductive film also includes acryl resin layer, and acryl resin layer is located at base material 11 and is situated between Between matter layer 12, for reducing the roughness on the surface of base material 11.
Pre-treatment removes the steam on the surface of base material 11, is conducive to ITO to crystallize, and improves the crystallinity of ITO conductive membrane layers; The surface of base material 11 is first coated with dielectric layer and is coated with conductive layer again, and the ITO conductive films transmitance of preparation is high, and impedance is low, conductive Preferably, the impedance of ITO conductive membrane layers is about 100 Ω/ to performance, the impedance of the ITO conductive membrane layers prepared than prior art Little about 50 Ω/.
Fig. 4 is the flow chart of the preparation method of the transparent conductive film that the embodiment of the present invention two is provided, as illustrated, the system The step of Preparation Method, is as follows:
Step 1, offer base material, and coat acryl resin layer in substrate surface.
Substrate surface coats acryl resin layer, and acryl resin layer reduces base surface roughness, beneficial to being subsequently coated with Dielectric layer and conductive layer, while transparent conductive film reflectivity can be reduced with matching optics performance, improve transparent conductive film Transmitance.
Step 2, by base material loaded in winding film coating machine, and will vacuumize inside winding film coating machine.
Fig. 2 is referred to, winding film coating machine includes that what is be sequentially communicated unreels end 10, process part 20 and winding end 30, unreels End 10 is provided with and unreels rod axle 102, winding end 30 and be provided with winding rod axle 302, and process part 20 is provided with plated film drum 200, is processing Base material 11 is looped around and unreels on rod axle 102, and plating is looped around from one end of plated film drum 200 from the base material 11 that rod axle 102 stretches out is unreeled On the surface of film drum 200, base material 11 leaves plated film drum after the surface of plated film drum 200 is rounded from the other end of plated film drum 200 200, the base material 11 for leaving plated film drum 200 is looped around on winding rod axle 302.When winding rod axle 302 is rotated in one direction, receive Volume rod axle 302 is looped around base material 11 on winding rod axle 302, and drive unreels rod axle 102 and rotates, and leaves and unreels rod axle 102 Base material 11 around plated film drum 200 round after be contained on winding rod axle 302.
In present embodiment, process part 20 includes at least two laminating rod axles 22, and laminating rod axle 22 is pasted positioned at base material 11 The position of plated film drum 200 is left in the position and base material 11 of closing plated film drum 200, for reducing the tension force of base material 11, and makes base material 11 are more closely fitted on the surface of plated film drum 200.Further, process part 20 also includes multiple guide bars axles 24, leads It is located to rod axle 24 and unreels between rod axle 102 and plated film drum 200, winds between rod axle 302 and plated film drum 200, for stretching base Material 11 simultaneously guides base material 11 to enter process part 20 and from process part 20 into winding end from end 10 is unreeled along default direction 30, guide bars axle 24 can also reduce the tension force of base material 11.
Process part 20 includes pre-treatment chamber 202, dielectric layer coating chamber 204 and leads according to the order that base material 11 is entered Electric layer coating chamber 206, is respectively used to be processed before the surface of base material 11 is carried out, is coated with dielectric layer and is coated with conductive layer.Pre-treatment Chamber 202, dielectric layer coating chamber 204 and conductive layer coating chamber 206 are the process cavity of autonomous working, and each chamber Between there is certain isolation with ensure base material 11 each within the chamber singly complete manufacturing procedure and by other operations Affect, the present embodiment dielectric layer coating chamber 204 is more than 200 with the isolation of conductive layer coating chamber 206.Further, It is to improve plating membrane efficiency in the present embodiment, process part 20 includes successively 4 dielectric layer coating chambers 204 and 2 conductive layer platings Membrane cavity room 206.
In present embodiment, 1 × 10 is evacuated to inside winding film coating machine-6Below mbar, wherein pre-treatment chamber 202 take out Vacuum is to 1 × 10-4Mbar~9 × 10-3Mbar, dielectric layer coating chamber 204 and conductive layer coating chamber 206 be evacuated to 9 × 10-4Mbar~9 × 10-3mbar。
Base material 11 is loaded into winding film coating machine, and unprocessed base material is exported to process part 20 using rod axle 102 is unreeled 11, the base material 11 of completion of processing is reclaimed from process part 20 using winding rod axle 302, improve the operating efficiency of coating process; Winding film coating machine is vacuumized, and for pre-treatment and coating process necessary processing environment is provided, and is that follow-up work is prepared.
Step 3, base material 11 enter pre-treatment chamber 202, and by the pretreating device in pre-treatment chamber 202 gas brightness is made Light electric discharge produces plasma, to remove the steam of acryl resin layer surface.
Before being coated with dielectric layer and conductive layer, base material 11 enters pre-treatment chamber 202 using pretreating device cleaning Asia gram Power resin layer surface, to be subsequently coated with dielectric layer and conductive layer the cleaning, the dry substrate 11 that are more easy to be coated with are provided.Specifically, it is front Processing chamber housing 202 fills pre-treatment working gas, makes its glow discharge produce plasma to pre-treatment working gas applied voltage Body, when base material 11 is through plasma, plasma removes the steam of acryl resin layer surface, reaches the table of activated substrate 11 Face, increase ITO conducting films are provided easily in the purpose of acryl resin layer surface adhesive force to be subsequently coated with dielectric layer and conductive layer In the clean surface of ITO crystallizations.It is a kind of preferred embodiment in, pre-treatment gas using argon gas and oxygen mixed gas, Pre-treatment chamber 202 is evacuated to 1 × 10-4Mbar~9 × 10-3mbar。
In the present embodiment, before processing before carrying out, winding film coating machine starts the heat riser of plated film drum 200, plus hot dip The temperature of film drum 200, specifically, the heat riser of plated film drum 200 is infrared heat riser, and by base material 11 be heated to 20 DEG C~ 250 DEG C, in a kind of preferably embodiment, base material 11 is heated to 80 DEG C~150 DEG C by plated film drum 200.Heated substrate 11, is beneficial to Base material 11 carries out pre-treatment, is coated with dielectric layer, is coated with the operations such as conductive layer, can improve ITO conducting films and be coated with effect.
Step 4, base material 11 enter dielectric layer coating chamber 204, in the acrylic of base material 11 by the way of magnetron sputtering Dielectric layer is coated with resin bed.
Dielectric layer is coated on acryl resin layer by the way of magnetron sputtering, and the material of dielectric layer can be inorganic Thing, such as MgF2、CaF2、SiO2Deng, or organic matter of the refractive index between 1.3~1.65, such as acryl resin, Polyurethane resin, melmac etc., also or above-mentioned organic matter and the inorganic matter mixture.
In the present embodiment, dielectric layer material uses SiO2, dielectric layer coating chamber 204 and conductive layer coating chamber 206 it Between need to keep larger isolation, to ensure that the oxygen in dielectric layer coating chamber 204 does not interfere with the formation of ITO conductive layer, tool Body, dielectric layer coating chamber 204 is more than 200 with the isolation of conductive layer coating chamber 206.In a kind of preferred embodiment, it is situated between Matter layer coating chamber 204 is evacuated to 9 × 10-4Mbar~9 × 10-3Mbar, target material surface to the distance on the surface of base material 11 is 30mm~50mm, working gas using argon gas and oxygen mixed gas, the magnetism intensity of magnetic control sputtering cathode be 100G~ 1500G.Acryl resin layer surface is first coated with dielectric layer and is coated with conductive layer again, and the ITO conductive film impedances of preparation are low, electric conductivity Can be preferably.
Step 5, base material 11 enter conductive layer coating chamber 206, the plating guidance on dielectric layer by the way of magnetron sputtering Electric layer.
In conductive layer coating chamber 206, adopt the mode of magnetron sputtering be coated with dielectric layer base material 11 on be coated with ITO Conductive film, the target for using for being coated with ITO conductive films is In2O3-SnO2Ceramic target or In-Sn metal targets.This reality In applying example, the use In of ITO conductive films is coated with2O3-SnO2Ceramic target, wherein SnO2Quality account for In2O3-SnO2Ceramic target The 0.3%~20% of material amount, in a kind of preferably embodiment, SnO2Quality account for In2O3-SnO2Ceramic target quality 8%~10%.Working gas used in this step adopts purity for the argon gas of 5N and the mixed gas of oxygen, equal beneficial to being formed Even conductive film layer.Also, the sputtering voltage that magnetron sputtering is adopted is for 400V~500V, conducting film coating chamber vacuum is 9 ×10-4Mbar~9 × 10-3Mbar, the temperature of base material 11 is 80 DEG C~150 DEG C.Magnetic control sputtering cathode adopts magnetism intensity for 200G ~1000G, wherein, 500G~800G best results.The ITO conductive film crystal properties of the conductive layer that this method is coated with technique Good, impedance is low, and electric conductivity is preferable.
Pre-treatment removes the steam on the surface of base material 11, is conducive to ITO to crystallize, and improves the crystallinity of ITO conductive membrane layers; The surface of base material 11 is first coated with dielectric layer and is coated with conductive layer again, and the ITO conductive films transmitance of preparation is high, and impedance is low, conductive Preferably, the impedance of ITO conductive membrane layers is about 100 Ω/ to performance, the impedance of the ITO conductive membrane layers prepared than prior art Little about 50 Ω/.
In the present embodiment, base material 11 selects the plastic material of polyester resin, such as polyethylene terephthalate (Polyethylene terephthalate, PET) plastics or cyclenes hydrocarbon type copolymer (COC) plastics, the modeling of polyester resin Material has the good transparency, heat resistance and mechanical property.Preferably, the thickness of base material 11 selects 2mm~100mm.
Pre-treatment removes the steam of acryl resin layer surface, is conducive to ITO to crystallize, and improves ITO conductive membrane layers Crystallinity;Acryl resin layer surface on base material 11 is first coated with dielectric layer and is coated with conductive layer again, and the ITO conductive films of preparation are saturating Cross rate high, and impedance is low, and preferably, the impedance of ITO conductive membrane layers is about 100 Ω/ to electric conductivity, prepares than prior art ITO conductive membrane layers the little about 50 Ω/ of impedance.
Above disclosed is only several preferred embodiments of the invention, can not limit the power of the present invention with this certainly Sharp scope, one of ordinary skill in the art will appreciate that all or part of flow process of above-described embodiment is realized, and according to present invention power Profit requires made equivalent variations, still falls within the covered scope of invention.

Claims (13)

1. a kind of preparation method of transparent conductive film, it is characterised in that include:
By base material loaded in winding film coating machine, and will vacuumize inside the winding film coating machine;
The base material enters pre-treatment chamber, and by the pretreating device of the pre-treatment within the chamber gas glow discharge is produced Plasma, to remove the steam of the substrate surface;
Dielectric layer and conductive layer are plated successively on the surface of the base material.
2. the preparation method of transparent conductive film according to claim 1, it is characterised in that described " base material is entered Pre-treatment chamber, makes gas glow discharge produce plasma by the pretreating device of the pre-treatment within the chamber, to remove The steam of the substrate surface " step includes:The pretreating device produces plasma using oxygen and argon gas glow discharge Remove the steam of the substrate surface.
3. the preparation method of transparent conductive film according to claim 2, it is characterised in that the pre-treatment chamber it is true Reciprocal of duty cycle is 1 × 10-4Mbar~9 × 10-3mbar。
4. the preparation method of transparent conductive film according to claim 3, it is characterised in that it is described " by base material loaded in In winding film coating machine, and will vacuumize inside the winding film coating machine " before, methods described also includes:In the substrate surface Coating acryl resin layer.
5. the preparation method of transparent conductive film according to claim 1, it is characterised in that the dielectric layer is titanium dioxide Silicon materials.
6. the preparation method of transparent conductive film according to claim 1, it is characterised in that the conductive layer is used In2O3-SnO2Ceramic target is made in the way of magnetron sputtering, and SnO2Quality account for In2O3-SnO2Ceramic target quality 0.3%~20%.
7. the preparation method of transparent conductive film according to claim 6, it is characterised in that the In2O3-SnO2Ceramics In target, SnO2Quality account for In2O3-SnO2The 8%~10% of ceramic target quality.
8. the preparation method of transparent conductive film according to claim 1, it is characterised in that the conductive layer uses In- Sn metal targets are made in the way of magnetron sputtering.
9. the preparation method of transparent conductive film according to claim 1, it is characterised in that described " base material is entered Pre-treatment chamber, makes gas glow discharge produce plasma by the pretreating device of the pre-treatment within the chamber, to remove Before the steam of the substrate surface ", methods described also includes:Start the infrared intensification dress of the plated film drum of the winding film coating machine Put, the base material is heated to 20 DEG C -250 DEG C, with the effect for improving pre-treatment, be coated with dielectric layer, be coated with conductive layer.
10. the preparation method of transparent conductive film according to claim 1, it is characterised in that use when being coated with conductive layer Sputtering voltage be 400V~500V.
The preparation method of 11. transparent conductive films according to claim 1, it is characterised in that magnetic control when being coated with conductive layer Sputter cathode adopts magnetism intensity for 200G~1000G.
12. a kind of transparent conductive films, it is characterised in that the transparent conductive film includes the base material being cascading, is situated between Matter layer and conductive layer, the base material for polyester resin plastic material, the dielectric layer is inorganic matter or refractive index 1.3~ Organic matter between 1.65, for preventing the sodium ion on the base material from spreading into the liquid crystal cell of display device, the conduction Layer is tin indium oxide.
13. transparent conductive films according to right wants 12, it is characterised in that the transparent conductive film also includes acrylic Resin bed, the acryl resin layer is located between the base material and the dielectric layer, for reducing the thick of the substrate surface Rugosity.
CN201611021226.5A 2016-11-15 2016-11-15 Preparation method of transparent conducting thin film and transparent conducting thin film Pending CN106637126A (en)

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CN111020522A (en) * 2019-12-09 2020-04-17 王殿儒 Composite type substrate continuous coating system based on gas discharge type high-power electron gun
CN111020522B (en) * 2019-12-09 2022-05-27 王殿儒 Composite type substrate continuous coating system based on gas discharge type high-power electron gun
CN111733384A (en) * 2020-06-19 2020-10-02 豪威星科薄膜视窗(深圳)有限公司 Coating process for capacitive touch screen
CN114823990A (en) * 2022-04-29 2022-07-29 苏州迈为科技股份有限公司 Heterojunction battery efficiency improving method
WO2024031956A1 (en) * 2022-08-09 2024-02-15 通威太阳能(成都)有限公司 Tco coating method, tco coating device, and solar cell and preparation method therefor

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