KR101666350B1 - Insulation Film including fluorocarbon thin film and Method of Manufacturing The Same - Google Patents
Insulation Film including fluorocarbon thin film and Method of Manufacturing The Same Download PDFInfo
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- KR101666350B1 KR101666350B1 KR1020150123340A KR20150123340A KR101666350B1 KR 101666350 B1 KR101666350 B1 KR 101666350B1 KR 1020150123340 A KR1020150123340 A KR 1020150123340A KR 20150123340 A KR20150123340 A KR 20150123340A KR 101666350 B1 KR101666350 B1 KR 101666350B1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
- C08L101/12—Compositions of unspecified macromolecular compounds characterised by physical features, e.g. anisotropy, viscosity or electrical conductivity
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
- C09D127/12—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
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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
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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
- C23C14/562—Apparatus specially adapted for continuous coating; Arrangements for maintaining the vacuum, e.g. vacuum locks for coating elongated substrates
Abstract
The present invention relates to a heat shielding film comprising a fluorocarbon thin film which can maximize the characteristic of shielding a near infrared ray wavelength region which is a heat ray region but also maintains the visibility of the visible ray region and is excellent in environmental resistance, will be.
Description
The present invention relates to a thermal barrier film comprising a fluorocarbon thin film and a method of manufacturing the same, and more particularly, to a thermal barrier film comprising a fluorocarbon thin film having excellent heat insulating effect by effectively blocking a near infrared wavelength region, Thin film, and a method for manufacturing the same.
Currently, various projects have been established to establish policy measures to simultaneously solve the two opposing objectives of measures to prevent environmental pollution caused by the use of fossil fuels and energy conservation measures due to the fineness of fossil fuels. In particular, A building or a vehicle that provides a pleasant and comfortable environment with reduced life energy by proper control, has been used as a functional film thermal barrier film as a means of controlling such thermal energy.
On the other hand, sunlight, which is thermal energy that is supplied infinitely in nature, is composed of visible light, ultraviolet light, and infrared light, and the visible light is a wavelength related to human vision, ultraviolet light is also called chemical light, . In addition, because most of the radiant heat emitted by the sun or the object is composed of infrared rays, the infrared rays are called heat rays. As mentioned in KS L 2016 (film for window glass), the energy distribution value for solar wavelength is in the range of 380 to 780 nm in the wavelength range due to thermal energy in the solar wavelength, Although the infrared region of 780 to 2200 nm occupies more than 95% and the wavelength of the solar light region is shielded by using a short-circuit film, it is impossible to control the visible light, which is a limitation of the conventional transparent heat- Which is the limit.
In other words, all of the heat shielding materials used in the conventional transparent heat shielding film are absorbed by the absorption of heat energy which is actually absorbed from the outside, and the problem of the temperature rise of the substrate and the heat energy absorbed are re- It is difficult to obtain a high heat shielding effect, and in the case of a product with high heat shielding efficiency, it is difficult to obtain visibility due to occurrence of cloudiness phenomenon.
Patent patents relating to heat short films developed to control the sunlight as described above are as follows: Patent Document 1 discloses a method in which one of polyurethane, epoxy or modified acrylic paint is selected on top of a PET film to form a pretreatment film A silver reflection film in which a silver film is formed on a surface of the silver reflection film and a method of manufacturing the silver reflection film are known. However, in the method of manufacturing a silver reflection film, a pretreatment application layer is formed on a substrate and a silver film is formed thereon. Is not a transparent film showing a visible transmittance like a film used for construction and a vehicle because it has the same shape as a mirror having a complete visual field shielding effect, and has a problem that a manufacturing cost and a productivity are deteriorated due to a complicated manufacturing process in which several layers are formed. Patent Document 2 discloses a method in which a film coated with a dye and an adhesive layer is laminated on a metal vapor-deposited base film using a laminating method and then adhered with an adhesive to prevent detachment of dye or desorption of deposited metal, However, it requires expensive equipment for depositing metal on the substrate, and has a disadvantage that the production rate is low and the defect rate is high. In addition, since the manufacturing process is complicated and the total thickness of the final film is high, when the user installs in a place such as a window, it is difficult to construct due to bubbles, foreign matter, layer separation, edge curling, Patent Document 3 discloses a heat ray shielding film having a high light transmittance in the visible light region and a low light transmittance in the near infrared region. However, in order to improve the heat ray shielding performance, the heat ray shielding component must be added in a large amount, The light transmittance of the region is lowered. That is, if the addition amount of the heat shielding component is reduced, the transmittance in the visible light region is increased but the heat shielding property is lowered. Therefore, it has been difficult to satisfy both the heat ray shielding property and the visible light transmittance simultaneously. Furthermore, when the heat ray shielding component is used in excess, it also has drawbacks such as a decrease in the physical properties, particularly impact resistance and toughness, of the transparent resin as a base material.
In order to solve the problems of the prior arts as described above, the Applicant has found that by improving the optical characteristics of the heat shield film and improving the heat resistance of the heat shield film by arranging the heat shield film in a thin thickness by a dry process and disposing the thin film containing fluorocarbon in the outermost layer The present invention provides a thermal barrier film comprising a transparent fluorocarbon thin film capable of effectively protecting the surface of a film exposed to the external environment and a method for manufacturing the same.
An object of the present invention is to provide a heat shielding film which is optically transparent and has excellent surface lubrication characteristics while greatly improving the transmittance in the visible light region by disposing a superhydrophobic and highly insulating fluorocarbon thin film in the outermost layer.
It is another object of the present invention to provide a method of manufacturing a thin film magnetic head capable of simplifying a manufacturing process by allowing all processes to be sputtered with a low energy and realizing a roll-to-roll process capable of manufacturing a large- The present invention also provides a method of manufacturing a heat shielding film comprising the fluorocarbon thin film, which can be applied immediately without any modification cost.
In addition, the present invention provides conductivity to a fluorocarbon thin film including a fluorine-based polymer having a disadvantage that electrical energy can not be easily applied as a typical insulator, thereby improving the problems in the RF sputtering process, Provided is a method for manufacturing a heat shielding film comprising a fluorocarbon thin film which can stably be sputtered even in a DC power supply system.
The heat shielding film according to the present invention comprises a heat ray blocking layer composed mainly of silver (Ag), copper (Cu) or nickel (Ni), and an optical compensation layer comprising a heat end element, Layer, it is possible to selectively block the region of the near infrared ray wavelength in the heat ray region and to provide a transparent heat ray shielding film with improved visible light transmittance. In addition, all layers can be formed by high deposition Deposition is possible.
The fluorocarbon protective layer according to an embodiment of the present invention includes a fluorinated polymer and a performing dopant that imparts conductivity.
In the present invention, the functionalizing agent may include one or two or more functionalizing agents selected from conductive particles, conductive polymers and metal components. Due to the functionalizing agent imparting such conductivity, not only the RF but also the MF And DC can be deposited by sputtering a fluorocarbon thin film, and a high temperature deposition rate and dielectric breakdown can be prevented, so that a heat short film including a fluorocarbon thin film of high quality can be formed.
The fluorocarbon protective layer according to an embodiment of the present invention may include any one or two or more functionalizing agents selected from conductive particles, conductive polymers, metal components, etc., and may be a metal organic compound, a metal oxide, a metal carbonaceous material, And further includes at least one metallic compound selected from carbonates, metal bicarbonates, metal nitrides, metal fluorides, and the like, and further the surface characteristics of the fluorocarbon protective layer can be controlled.
Further, the present invention can easily adjust the thicknesses of the optical compensation layer, the heat ray blocking layer and the fluorocarbon protective layer through sputtering using a more industrially useful power supply method such as MF or DC, And MF or DC sputtering is possible in all of the processes for forming each layer, so that the process can be continuously performed in a single equipment by applying the roll-to-roll process, thereby remarkably improving the productivity.
According to an embodiment of the present invention, there is provided a method of manufacturing a thermal barrier film, including: a first step of coating an optical compensation layer including an element having a thermal end on one surface of an adherend; A second step of coating a heat ray blocking layer comprising silver (Ag), copper (Cu), or nickel (Ni) as a main component on one surface of the optical compensation layer; And coating the surface of the heat ray blocking layer with a fluorocarbon protective layer. Here, the coating of step 1 to step 3 is performed by MF or DC sputtering.
The method for manufacturing a thermal barrier film according to an embodiment of the present invention may further include repeating the steps 1 and 2 sequentially two or more times before performing the step 3 so that the area of the near infrared ray wavelength At 90% or more, and at the same time prevents diffused reflection, thereby minimizing the glare and ensuring a clear and bright field of view for the visible light region.
The present invention provides a roll-to-roll type sputtering deposition system capable of continuously performing MF or DC sputtering for all the steps of forming the optical compensation layer, the heat ray blocking layer, and the fluorocarbon protective layer.
The roll-to-roll type sputtering deposition system according to an embodiment of the present invention includes an unwinder chamber for loading an adherend, a main chamber for depositing a thin film on one surface of the substrate, And a winder chamber for regenerating the deposited thin film. At this time, the main chamber may have three MF dual sputtering cathodes and one single DC sputtering cathode.
The heat shielding film according to the present invention has an advantage of being excellent in the wavelength blocking property in the near infrared region and at the same time maintaining the visibility of the visible light region and maintaining transparency due to high transmittance in the visible light region. Further, by introducing the fluorocarbon thin film into the outermost layer, the optical characteristics of the heat shield film can be maximized, and water repellency, antifouling properties and the like can be remarkably improved.
Furthermore, the heat shielding film according to the present invention can easily adjust the thickness of the thin film through sputtering, and can form a thinner thin film. Thus, it can be applied to automobile window film, Or a transparent heat shielding glass can be provided.
In addition, the method for manufacturing a thermal barrier film according to the present invention can be applied to a roll-to-roll process capable of sputtering using a commercially available MF or DC power source method, which can deposit all thin films, And the cost reduction is possible.
FIG. 1 is a schematic configuration diagram of a roll-to-roll type sputtering deposition system according to the present invention.
The heat short film including the fluorocarbon thin film according to the present invention and the method for producing the same will be described below. However, unless otherwise defined in the technical terms and scientific terms used herein, And the description of known functions and configurations which may unnecessarily obscure the gist of the present invention will be omitted in the following description.
The heat shielding film according to the present invention not only maximizes the heat insulating effect of the heat ray shielding layer including the metal having the inherent heat shielding property by arranging the fluorocarbon thin film in the outermost layer but also has excellent water repellent and antifouling effect, The environmental resistance of the exposed short-circuit film can be improved.
The heat shield film according to an embodiment of the present invention may include an optical compensation layer including an adherend, a heat ray blocking layer composed mainly of silver (Ag), copper (Cu), or nickel (Ni) Fluorine protective layer. The heat shielding film can form a heat shielding layer mainly composed of silver (Ag), copper (Cu), or nickel (Ni) having a high heat shielding efficiency to realize a high heat shielding effect. The protection layer can maximize the heat ray blocking rate to 90% or more.
In general, in the case of a film using a metal having a thermal efficiency, the content of the metal is increased to increase the thermal efficiency, thereby causing a clouding phenomenon and the like. Thus, the applicant of the present invention has found that the heat insulating properties can be remarkably improved by minimizing the content of the main component contained in the heat ray blocking layer and vapor-depositing the optical compensation layer and the fluorocarbon protective layer having heat insulating property and transparency thereto Thus completing the present invention.
The heat blocking layer according to an exemplary embodiment of the present invention may include aluminum (Al), tungsten (W), gold (Au), tin (Sn), zinc (Zn) (Ni), NiO, ITO, IZO, IZTO, AZO, IAZO, GZO (IZO), and the like. , IGO, IGZO, IGTO, ATO, IATO, IWO, CIO, MIO, SnO 2 , ZnO, ZnAlO x , In 2 O 3 , TiTaO 2 , TiNbO 2 , TiO 2 , RuO 2 , IrO 2 , Nb 2 O 5 , Ta 2 O 5, ZnO, SiO 2, SiN, Si 3 N 4 And Al 2 O 3 And the like, but the present invention is not limited thereto. At this time, from the viewpoint of improving the optical characteristics of the thermal barrier film and eliminating diffuse reflection, it is possible to select from TiO 2 , SiO 2 , SiN, Si 3 N 4 and Al 2 O 3 It is preferable to include at least one additional element.
The fluorocarbon protective layer according to an embodiment of the present invention includes a fluorinated polymer and a functionalizing agent having conductivity.
Generally, in the case of a fluorine-based polymer, in order to sputter it with hydrophobic characteristics and insulation properties, a high-frequency energy of RF (Radio Frequency) must be applied. Accordingly, the fluorine- The deformation is necessarily generated on the joint portion of the target, and defects in the target have to be generated. For this reason, the sputtered fluorine-based polymer is not uniformly deposited on the surface of the adherend, and the deposition efficiency is very poor.
Thus, as described above, the fluorocarbon protective layer according to the present invention includes a functionalizing agent having conductivity to impart conductivity to the target, so that not only high-frequency energy of RF (radio-frequency) but also lower- range frequency) and direct current (DC) deposition of fluorocarbon thin films.
As described above, each of the heat ray blocking layer, the optical compensation layer and the fluorocarbon protective layer of the thermal barrier film according to the present invention can be deposited using a sputtering method, and can be applied to a roll-to-roll process. Since the heat short film can be produced by the continuous process, the productivity can be remarkably improved. Particularly, the fluorocarbon protective layer of the thermal barrier film according to the present invention can be easily deposited by the function of the functionalizing agent by using industrially useful MF or DC, and the deposition efficiency can be remarkably increased.
That is, since the fluorocarbon protective layer of the thermal barrier film according to an embodiment of the present invention imparts conductivity to the fluorine-based polymer, it is surprisingly possible to perform sputtering even in a power supply system of low voltage such as MF or DC, And a high deposition rate can be realized.
The functionalizing agent may be contained in an amount of 0.01 to 2000 parts by weight based on 100 parts by weight of the fluorinated polymer and is preferably 0.5 to 1500 parts by weight in view of being able to deposit a high quality fluorocarbon thin film by preventing a higher deposition rate and dielectric breakdown. And more preferably 1 to 1000 parts by weight.
The functionalizing agent contained in the fluorocarbon protective layer according to an embodiment of the present invention is not limited as long as it is a conductive material, but may be any one or more selected from conductive particles, conductive polymers, and metal components. Here, the conductive particles include, but are not limited to, carbon nanotubes (carbon nanotubes), carbon nanofibers, Carbon black, graphene, graphite, carbon fiber, or a mixture thereof, and may also include other organic conductive particles. In this case, when the organic conductive particles, which are one example of the conductive particles, are used, it is preferable because the conductive particles can be imparted while maintaining the fluorocarbon component. Non-limiting examples of the conductive polymer include polyaniline, polyacetylene, Polytetrafluoroethylene, polythiophene, polypyrrole, polyfluorene, polypyrene, polyazulene, polynaphthalene, polyphenylene, polyphenylene vinylene polyolefins such as polyphenylene vinylene, polycarbazole, polyindole, polyazaphine, polyethylene, polyethylene vinylene, polyphenylene sulfide, polyfuran, polyfuran, polyselenophene, polytellurophene, polysulfur nitride, And the like, but the present invention is not limited thereto. The non-limiting examples of the metal component include copper (Cu), aluminum (Al), silver (Ag), gold (Au), tungsten (W), silicon (Si), magnesium (Mg) ), Molybdenum (Mo), vanadium (V), niobium (Nb), titanium (Ti), platinum (Pt), chromium (Cr), tantalum (Al), silver (Ag), gold (Au), tungsten (W), magnesium (Mg), nickel (Ni) or the like in view of having good adhesion with the metal electrode And mixtures thereof, more preferably copper (Cu), aluminum (Al), silver (Ag), gold (Au) or a mixture thereof.
The fluorocarbon protective layer according to an embodiment of the present invention may further include at least one metal compound selected from metal organic compounds, metal oxides, metal carbon materials, metal hydroxides, metal carbonates, metal bicarbonates, metal nitrides and metal fluorides , It is additionally possible to control the surface properties of the hydrocarbon protective layer. In this case, a static example ruthless of the metal compound is SiO 2, Al 2 O 3, ITO, IGZO, ZnO, In 2 O 3, SnO 2, TiO 2, AZO, ATO, SrTiO 3, CeO 2, MgO, NiO , CaO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , MgF 2 , CuF 2 , Si 3 N 4 , CuN, Nb 2 O 5 , V 2 O 5 and AlN, SiO 2 , Al 2 O 3 , ITO, Nb 2 O 5 , V 2 O 5 And the like.
In the case of the heat shielding film according to the present invention, by forming the fluorocarbon protective layer at the outermost angle of the film, it is possible to remarkably improve the optical characteristics while maintaining the super hydrophobic property and the high transparency, Excellent chemical resistance and lubricity.
Hereinafter, a method of manufacturing a heat shielding film of the present invention will be described.
According to an embodiment of the present invention, the thermal barrier film includes a first step of coating an optical compensation layer including a thermal end element on one side of an adherend; A second step of coating a heat ray blocking layer comprising silver (Ag), copper (Cu) or nickel (Ni) as a main component on one surface of the optical compensation layer; And coating the surface of the heat ray blocking layer with a fluorocarbon protective layer.
At this time, the fluorocarbon protective layer of the thermal barrier film can improve the conductivity and strength of the produced fluorocarbon protective layer by controlling the kind and content of the conductive particles, the conductive polymer, and the metal component as the functionalizing agent. In addition, the inclusion of a functionalizing agent having conductivity has an advantage that a fluorocarbon protective layer can be formed at a low cost by enabling sputtering at a lower voltage due to improved conductivity. Unlike a conventional process in which a high-frequency power source is required for sputtering a fluorine-based polymer, the present invention uses a fluorine-based polymer to which conductivity is imparted, ), The sputtering can be performed smoothly, and the effect of the sputtering is remarkably high.
That is, the coating of the first to third steps according to an embodiment of the present invention can be carried out by industrially useful MF or DC sputtering, and it is possible to implement a roll-to-roll process capable of large-area coating in a very short time, Since the roll-to-roll equipment can be directly applied to the target without replacement cost, it can be advantageously commercialized, and the process can be simplified and manufacturing cost can be reduced.
Further, in the production of the heat shielding film according to the present invention, the nano-sized thin film can be used as a sputtering process, and the thickness of the thin film can be precisely controlled. Accordingly, since the contact angle, visible light transmittance, heat transmittance and the like of the heat short film can be freely adjusted, it is possible to apply the heat short film having excellent energy saving effect by applying it to the appropriate place.
The adherend according to an exemplary embodiment of the present invention may be formed of a material such as silicon, glass, plastic, polypropylene (PP), polyethylene (PE), polycarbonate (PC), polyethylene terephthalate (PET), polyimide (PI), a cyclic olefin copolymer (COC), a cyclic olefin polymer (COC), triacetyl cellulose (TAC), polyethylene naphthalene (PEN), polyurethane PU), polyacrylate, polyester, polymethylene pentene (PMP), polymethyl methacrylate (PMMA), polymethacrylate (PMA), polystyrene polystyrene, PS), styrene-acrylonitrile copolymer (SAN), acrylonitrile-butylene-styrene copolymer (ABS), polyvinyl chloride vinyl chloride (EVA), ethylene-vinyl alcohol copolymer (EVOH), polyvinyl alcohol (PVA), polyarylate, PAR, an acryl-styrene-acrylonitrile copolymer, an ethylene-butylene copolymer, an ethylene-octene copolymer, an ethylene-propylene copolymer ethylene-propylene copolymer, ethylene-propylene-diene monomer copolymer (EPDM), polyamide, polyphenylene oxide (PPO), polybuthylene terephthalate terephthalate (PBT), polytrimethylene terephthalate (PTT), polyoxymethylene (POM), polyphthalamide (PPA), polysulfone (PSf) Polyether sulfone (PES), polyphenylene sulfide (PPS), liquid crystalline polymer (LCP), polyether imide (PEI), polyamide imide (PAI) Polyether ketone (PEEK), polyether ketone (PEKK), polyether ketone ketone ketone (PEKK), polyether ketone ketone ketone (PAEK), polybenzimidazole (PBI), polyvinyl butyral (PVB), polypropylene carbonate (PBT), and polyether ketone (PEKEKK) PPC), polylactic acid (PLA), polyhydroxy alkanoates (PHAs), alkyd resins, phenol resins, epoxy resins, ceramics, quartz, etc. Selected And may be used in films or glass such as polypropylene (PP), polyethylene (PE), polycarbonate (PC), and polyethylene terephthalate (PET)
The fluorocarbon protective layer of the thermal barrier film according to an embodiment of the present invention may include one or more functionalizing agents selected from conductive particles, conductive polymers, metal components, and the like.
Here, the conductive particles include, but are not limited to, carbon nanotubes (carbon nanotubes), carbon nanofibers, Carbon black, graphene, graphite, carbon fiber, or a mixture thereof, and may also include other organic conductive particles. Non-limiting examples of the conductive polymer include Polyaniline, polyacetylene, polythiophene, polypyrrole, polyfluorene, polypyrene, polyazulene, polynaphthalene, and the like. Polyphenylene, polyphenylene vinylene, polycarbazole, polyindole, polyazaphine, polyethylene, polyethylene vinylene, and the like. Polyphenylene sulfide, polyfuran, polyselenophene, polytellurophene, polysulfur nitride, polyether sulfone, polyether sulfone, And the like, but the present invention is not limited thereto. The non-limiting examples of the metal component include copper (Cu), aluminum (Al), silver (Ag), gold (Au), tungsten (W), silicon (Si), magnesium (Mg) ), Molybdenum (Mo), vanadium (V), niobium (Nb), titanium (Ti), platinum (Pt), chromium (Cr), tantalum (Al), silver (Ag), gold (Au), tungsten (W), magnesium (Mg), nickel (Ni) or the like in view of having good adhesion with the metal electrode And mixtures thereof, more preferably copper (Cu), aluminum (Al), silver (Ag), gold (Au) or a mixture thereof.
The functionalizing agent is not particularly limited as long as it has sufficient compatibility with the fluorine-based polymer powder and a homogeneous composition, but preferably has an average particle size in the range of 10 nm to 1000 μm, preferably 10 nm to 100 μm But is not limited thereto.
The fluorocarbon protective layer according to an embodiment of the present invention may further include at least one metal compound selected from metal organic compounds, metal oxides, metal carbon materials, metal hydroxides, metal carbonates, metal bicarbonates, metal nitrides and metal fluorides , It is additionally possible to control the surface properties of the hydrocarbon protective layer. In this case, a static example ruthless of the metal compound is SiO 2, Al 2 O 3, ITO, IGZO, ZnO, In 2 O 3, SnO 2, TiO 2, AZO, ATO, SrTiO 3, CeO 2, MgO, NiO , CaO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , MgF 2 , CuF 2 , Si 3 N 4 , CuN, Nb 2 O 5 , V 2 O 5 and AlN, SiO 2 , Al 2 O 3 , ITO, Nb 2 O 5 , V 2 O 5 And the like.
In the method of manufacturing a heat shielding film according to an embodiment of the present invention, the step of coating the optical compensation layer and the step of coating the heat ray blocking layer may be repeated one or more times in order or randomly And can be repeatedly performed two or more times in order to realize a lower heat transmittance and an excellent visible light transmittance, and then the fluorocarbon protective layer is disposed at the outermost periphery.
The optical compensation layer, the heat ray blocking layer and the fluorocarbon protective layer according to an embodiment of the present invention can be manufactured in the range of 1 to 1000 nm, respectively. In the case of the heat ray blocking layer, the wavelength in the range of 780 to 2200 nm It is preferable that the optical compensation layer is formed in a range of 5 to 15 nm from the viewpoint of improving the adiabatic characteristic by selectively blocking and not decreasing the cyanicity and the optical compensation layer is preferably formed to improve the adiabatic property and to increase the hardness of the heat shield film It is preferably formed in the range of 20 to 100 nm. The fluorocarbon protective layer is preferably formed in the range of 10 to 100 nm in order to maximize the antifouling and waterproof characteristics and to optimize the optical characteristics and strength characteristics of the thermal short film, but the present invention is not limited thereto.
In addition, the present invention can provide a roll-to-roll type sputtering deposition system in which all steps of forming an optical compensation layer, a heat ray blocking layer, and a fluorocarbon protective layer included in the thermal short film can be continuously performed, The sputtering can be performed by MF or DC sputtering.
The roll-to-roll type sputtering deposition system according to an embodiment of the present invention includes an unwinder chamber for loading an adherend, a main chamber for depositing a thin film on one surface of the substrate, And a winder chamber for regenerating the deposited thin film. In this case, the main chamber is provided with three MF dual sputtering cathodes and one single DC sputtering cathode simultaneously, and a process for manufacturing a short-circuiting film can be performed by continuously performing each of MF and DC sputtering, Not only can there be cost savings.
Hereinafter, the present invention will be described in more detail with reference to the following examples. However, these embodiments are provided to aid understanding of the present invention, and the scope of the present invention is not limited thereto in any sense.
(Example 1)
A heat short film was produced using a roll-to-roll sputter (ULVAC, SPW-060) device on a PET film (SKC, SH-40,
The vapor deposition target for each layer of the heat shield film was made into a rectangular plate. A carbon nano tube (CNT) was coated on an Si target (length 950 mm, width 127 mm, thickness 6 mm), Ag target (length 950 mm, width 127 mm, thickness 6 mm), PTFE 95 wt% A fluoropolymer composite target (length 950 mm, width 127 mm, thickness 6 mm) containing 5 wt% was attached to the electrode surface of each copper backing plate. Two Si targets were placed in MF dual sputtering cathode 1 (cathode 1) in the process chamber section and two fluorinated polymer composite targets were placed in MF dual sputtering cathode 2 (cathode 2). Then, one Ag target was placed in the DC single sputtering cathode 3 (cathode 3). Thereafter, the PET film was loaded on an unwinder, the inside of the roll-to-roll sputter apparatus was made to be in a low vacuum state by using a rotary pump and a booster pump, and then a high vacuum (2 10 -4 Pa ). The degree of vacuum inside of the roll-to-roll sputtering apparatus 2 × 10 -4 Pa or less and when the argon (Ar) gas to each of the cathode and the MF DC power were injected at a flow rate of 400 sccm to 1.0 W / cm 2, pre- sputtering. Then, the temperature of the main roll was lowered to 10 캜, and the PET film was transported at a speed of 1 m / min to deposit a thin film for a heat short film. A SiNx thin film (optical compensation layer) was deposited through the cathode 1. At this time, the SiNx thin film was deposited to a thickness of 40 nm at a partial pressure (10 mtorr) of N 2 gas (N 2 gas) at an MF power of 8 W / cm 2 . An Ag thin film (heat ray blocking layer) was deposited on one side of the SiNx thin film at a DC power of 0.6 W / cm 2 through the cathode 3 to a thickness of 12 nm. A fluorocarbon thin film (fluorocarbon protective layer) was deposited on one surface of the Ag thin film at a MF power of 2.0 W / cm 2 through the cathode 2 to a thickness of 20 nm to form a three- And completed the production of the train short film.
Visible light transmittance (Tmax) and infrared transmittance (measured at a wavelength of 1000 nm) were measured in order to confirm the physical properties of the completed heat short film, and the results are shown in Table 1.
1. Contact angle measurement
The water contact angle of the completed short heat film was measured using a contact angle meter (
2. Measured maximum transmittance (Tmax) of visible light
The transmittance of visible light (550 nm) was measured by irradiating light to the finished heat short film using a spectrophotometer (U-410, Hitachi).
3. Measurement of infrared transmittance (measurement wavelength 1000 nm)
The finished heat shield film was measured three times with a UV-Vis spectrometer at a wavelength of 1,000 nm, and its average value was measured to determine the infrared transmittance (%).
(Example 2)
In Example 1, a heat shielding film was produced in the same manner except for the following conditions. A SiNx thin film (optical compensation layer) was deposited to a thickness of 30 nm with an N 2 gas (N 2 gas) partial pressure (10 mtorr) at an MF power of 6.5 W / cm 2 through the cathode 1. An Ag thin film (heat ray blocking layer) was deposited on one surface of the SiNx thin film at a DC power of 0.4 W / cm 2 through the cathode 3 to a thickness of 8 nm. Thereafter, the SiNx thin film and the Ag thin film were sequentially and repeatedly performed in the same manner under the same conditions. A fluorocarbon thin film (fluorocarbon protective layer) was deposited on one surface of the Ag thin film at a MF power of 3.5 W / cm 2 through the cathode 2 to a thickness of 50 nm to form a five- And completed the production of the train short film.
Visible light transmittance (Tmax) and ultraviolet transmittance (measured at a wavelength of 1000 nm) were measured in order to confirm the physical properties of the finished heat short film. The results are shown in Table 1.
(Comparative Example 1)
In Example 1, a heat shielding film was produced in the same manner except for the following conditions. An Si target (length 950 mm, width 127 mm, thickness 6 mm) and an Ag target (length 950 mm, width 127 mm, thickness 6 mm) were attached to the respective copper backing plate electrode surfaces, The target was provided with two Si targets on MF sputtering cathode 1 (cathode 1) and one Ag target on DC sputtering cathode 3 (cathode 3) in the process chamber. An SiN thin film (optical compensation layer) was deposited to a thickness of 40 nm at a partial pressure (10 mtorr) of N 2 gas (N 2 gas) at an MF power of 8 W / cm 2 through the cathode 1. An Ag thin film (heat ray blocking layer) was deposited to a thickness of 12 nm on the surface of the SiN thin film at a DC power of 0.6 W / cm 2 through the cathode 3 to form a two- And completed the heat short film production.
Visible light transmittance (Tmax) and ultraviolet transmittance (measured at a wavelength of 1000 nm) were measured in order to confirm the physical properties of the finished heat short film. The results are shown in Table 1.
As shown in Table 1, in the case of the heat shielding film according to the present invention, it can be seen that by arranging the fluorocarbon thin film at the outermost periphery, the visible light transmittance can be further improved, , The contact angle is high, and water repellency and antifouling property due to moisture and contaminants can be remarkably improved.
In addition, the heat shielding film according to the present invention has an excellent infrared ray blocking rate, greatly enhancing the heat insulating performance and maximizing the energy saving and cooling / heating efficiency, and is expected to be applicable to various industrial fields.
(100), an unwinder chamber (101), an ion plasma trestment (102), a heater (103), a subwinder (suv UW), an unwinder A
Claims (14)
Wherein the conductive particles are at least one selected from the group consisting of carbon nanotubes, carbon nanofibers, carbon black, graphene, graphite, and carbon fibers.
The conductive polymer may be at least one selected from the group consisting of polyaniline, polyacetylene, polythiophene, polypyrrole, polyfluorene, polypyrene, polyazulene, polynaphthalene ), Polyphenylene, polyphenylene vinylene, polycarbazole, polyindole, polyazaphine, polyethylene, polyethylene vinylene (hereinafter referred to as " Wherein the heat shrinkage film is at least one selected from the group consisting of polyphenylene sulfide, polyfuran, polyselenophene, polytellurophene and polysulfur nitride.
Wherein the metal component is at least one selected from Cu, Al, Ag, Au, W, Si, Mg, Ni, Mo, V, Nb, Ti, Pt, Cr and Ta.
IO, OZO, IGO, IGTO, IGO, IGTO, ATO, IATO, IWO, CIO, MIO, MgO, SnO 2 , ZnO, ZnAlO x , In 2 O 3 , TiTaO 2 , TiNbO 2 , TiO 2 , RuO 2 , IrO 2 , Nb 2 O 5 , Ta 2 O 5 , ZnO, SiO 2 , SiN, Si 3 N 4 and Al 2 O 3 Wherein the heat shrink film comprises at least one heat shrink film.
Wherein the fluorocarbon protective layer further comprises at least one metal compound selected from metal organic substances, metal oxides, metal carbon materials, metal hydroxides, metal carbonates, metal bicarbonates, metal nitrides and metal fluorides.
Wherein the metal compound is selected from the group consisting of SiO 2 , Al 2 O 3 , ITO, IGZO, ZnO, In 2 O 3 , SnO 2 , TiO 2 , AZO, ATO, SrTiO 3 , CeO 2 , MgO, NiO, CaO, ZrO 2 , Y 2 O 3 , Al 2 O 3 , MgF 2 , CuF 2 , Si 3 N 4 , CuN, Nb 2 O 5 , V 2 O 5 and AlN.
A second step of coating a heat ray blocking layer containing silver (Ag), copper (Cu), or nickel (Ni) on one surface of the optical compensation layer; And
A third step of coating a fluorocarbon protective layer by MF or DC sputtering using a fluorinated polymer composite target comprising a fluorinated polymer, conductive particles, conductive polymer and at least one functionalizing agent selected from metal components on one surface of the heat ray blocking layer; Wherein the heat-shrinkable film has a thickness of 10 mm or less.
Wherein the step (b) is carried out by repeating the step (1) and the step (2) in sequence two or more times before performing the step (3).
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| KR1020150123340A KR101666350B1 (en) | 2015-09-01 | 2015-09-01 | Insulation Film including fluorocarbon thin film and Method of Manufacturing The Same |
| PCT/KR2016/009772 WO2017039342A1 (en) | 2015-09-01 | 2016-09-01 | Barrier film comprising fluorocarbon thin film and method for manufacturing same |
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| KR1020150123340A KR101666350B1 (en) | 2015-09-01 | 2015-09-01 | Insulation Film including fluorocarbon thin film and Method of Manufacturing The Same |
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| KR101843364B1 (en) * | 2016-11-22 | 2018-03-29 | 한국화학연구원 | Transparent conductive film of water-repellency and plate heater comprising the same |
| CN111689784A (en) * | 2020-05-18 | 2020-09-22 | 珠海格力节能环保制冷技术研究中心有限公司 | Thermal-insulated material of making an uproar, thermal-insulated structure of making an uproar and compressor including it of making an uproar that falls |
| CN111909574A (en) * | 2019-05-10 | 2020-11-10 | 南亚塑胶工业股份有限公司 | Energy-saving film structure |
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