WO2014175023A1 - Procédé de fabrication de film fonctionnel - Google Patents

Procédé de fabrication de film fonctionnel Download PDF

Info

Publication number
WO2014175023A1
WO2014175023A1 PCT/JP2014/059737 JP2014059737W WO2014175023A1 WO 2014175023 A1 WO2014175023 A1 WO 2014175023A1 JP 2014059737 W JP2014059737 W JP 2014059737W WO 2014175023 A1 WO2014175023 A1 WO 2014175023A1
Authority
WO
WIPO (PCT)
Prior art keywords
inorganic layer
heat
functional film
layer
resistant substrate
Prior art date
Application number
PCT/JP2014/059737
Other languages
English (en)
Japanese (ja)
Inventor
健治 属
和喜 田地
Original Assignee
コニカミノルタ株式会社
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by コニカミノルタ株式会社 filed Critical コニカミノルタ株式会社
Publication of WO2014175023A1 publication Critical patent/WO2014175023A1/fr

Links

Images

Classifications

    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate
    • C23C18/1241—Metallic substrates
    • 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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • 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
    • B32B38/00—Ancillary operations in connection with laminating processes
    • B32B38/0036—Heat treatment
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/122—Inorganic polymers, e.g. silanes, polysilazanes, polysiloxanes
    • 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
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/125—Process of deposition of the inorganic material
    • C23C18/1283—Control of temperature, e.g. gradual temperature increase, modulation of temperature
    • 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
    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
    • B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
    • B32B2037/243—Coating
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/30—Properties of the layers or laminate having particular thermal properties
    • B32B2307/306—Resistant to heat
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/40—Properties of the layers or laminate having particular optical properties
    • B32B2307/412—Transparent
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/712—Weather resistant
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/724—Permeability to gases, adsorption
    • B32B2307/7242—Non-permeable
    • 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
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/70—Other properties
    • B32B2307/724—Permeability to gases, adsorption
    • B32B2307/7242—Non-permeable
    • B32B2307/7246—Water vapor barrier
    • 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
    • B32B2309/00—Parameters for the laminating or treatment process; Apparatus details
    • B32B2309/02—Temperature

Definitions

  • the present invention relates to a method for producing a functional film excellent in production efficiency.
  • a functional film is a film in which a constituent layer (functional layer) that expresses various functions is provided on a flexible plastic film, such as a gas barrier film, an antireflection film, an anti-reflection film, and the like.
  • a dazzling film such as a heat ray blocking film, a transparent conductive film, a moisture proof film, an ultraviolet deterioration preventing film, a diffusion film, a weather resistant film, and an antibacterial film.
  • organic EL organic electroluminescence
  • gas barrier film will be described as a representative example of a functional film.
  • the gas barrier layer constituting the gas barrier film generally, a method of forming a silica vapor deposition film using a vacuum vapor deposition apparatus or the like is known. In this vacuum vapor deposition, a large vacuum apparatus or the like is used. In addition, due to restrictions on the equipment to be used, the suitability for continuous production by the roll-to-roll method was poor, and there was a problem in terms of economy and productivity.
  • JP-A-8-269690 discloses a coating solution containing perhydropolysilazane (hereinafter also referred to as PHPS) or organic polysilazane on a polyester film.
  • PHPS perhydropolysilazane
  • a method is disclosed in which PHPS or organic polysilazane is cured and polymerized by plasma treatment to form an inorganic polymer layer made of silicon oxide or the like.
  • the inorganic polymer layer formed by the method disclosed in Japanese Patent Application Laid-Open No. 8-269690 is a layer disposed between the base material and the metal vapor deposition layer, and the adhesion between the metal vapor deposition layer and the base material. In addition, it is a layer for imparting chemical stability to the base material, and its effect as a gas barrier layer is low.
  • Patent Document 1 Also disclosed is a method for converting a thin film (0.05 to 5 ⁇ m) containing PHPS or organic polysilazane as a main component into a dense glass-like layer having transparency and a high barrier property to gas (for example, see Patent Document 1.)
  • the conversion method described in Patent Document 1 is adapted to the substrate used by irradiation with vacuum ultraviolet light (hereinafter also referred to as VUV) having a wavelength of 230 nm or less and UV light having a wavelength of less than 300 nm.
  • VUV vacuum ultraviolet light
  • the gas barrier property of the obtained gas barrier layer is as follows: It is insufficient.
  • the flexible thin film plastic film applied to various electronic devices does not have sufficient gas barrier properties as described above, and when the gas barrier properties are imparted to the plastic film, the gas barrier properties as described above.
  • the plastic film itself has low heat resistance, the gas barrier layer formation is limited by the maximum temperature of the process, and must be kept low. This is a major obstacle in forming the layer. As a result, an electronic device having high reliability using a plastic film has not been realized.
  • a method in which a solution containing, for example, polysilazane or a siloxane polymer is applied on a heat resistant substrate (for example, a glass substrate), an inorganic layer is formed by baking treatment, and then transferred onto a plastic film.
  • a heat resistant substrate for example, a glass substrate
  • an inorganic layer is formed by baking treatment, and then transferred onto a plastic film.
  • Patent Document 2 the man-hours for peeling off the formed inorganic layer and the man-hours for adhering to the other substrate are many, the process is complicated, and the production suitability, particularly continuous production. This is a very poor method.
  • the conditions in the peeling step and the adhesion step are not strictly controlled, it is difficult to stably form the gas barrier layer.
  • the present invention has been made in view of the above problems, and its solution is a functional film excellent in functionality (for example, gas barrier properties), transparency and flatness, without requiring a large facility, It is an easy method to provide a method for producing a functional film that is excellent in economic efficiency and production stability and can be produced at a high production capacity (production speed).
  • the present inventor applied an inorganic layer forming precursor on a heat-resistant substrate to form an inorganic layer forming precursor layer, and then thermally baked the inorganic layer forming precursor layer
  • the function is achieved by closely contacting and transferring the formed inorganic layer to the plastic film surface under the condition that the temperature of the heat-resistant substrate is equal to or higher than a specific temperature.
  • a functional film which is characterized by producing a film, is a functional film excellent in functionality (for example, gas barrier properties), transparency and flatness, without requiring large equipment, and simple. It has been found that the method can provide a method for producing a functional film that is excellent in economic efficiency and production stability and can be produced at a high production capacity (production speed).
  • the heat-resistant base material is an endless heat-resistant base material that is continuously conveyed, and the coating process, the thermal baking process, the cooling process, the adhesion process, and the transfer process are online processes that are performed by continuously conveying the endless heat-resistant base material.
  • a functional film excellent in functionality for example, gas barrier property
  • transparency is not required for large equipment, and is excellent in economic efficiency and production stability by a simple method, and A method for producing a functional film that can be produced at a high production capacity (production speed) can be provided.
  • the transfer is performed within a specific temperature condition range during the cooling process in the process of transferring onto the plastic film in the cooling process of the inorganic layer.
  • the adhesiveness between the inorganic layer and the plastic film can be increased as compared with the method of transferring the inorganic layer to room temperature and transferring it after cooling or transferring it by reheating after cooling. This is because by transferring at a stage where the temperature is high to a certain degree, the surface activity of the inorganic layer can be in close contact with the plastic film, and softening at the temperature at the close contact with the plastic film. It is estimated that the followability with the heat-resistant base material is improved and the transfer can be stably performed.
  • Process flow figure which shows an example of the manufacturing process by the single wafer system which is an example of the manufacturing method of the functional film of this invention Graph showing an example of temperature history pattern in each manufacturing process
  • the process flow figure which shows an example of the on-line manufacturing process by the roll-to-roll system which is an example of the manufacturing method of the functional film of this invention
  • an inorganic layer forming precursor is applied on a heat resistant substrate to form an inorganic layer forming precursor layer, and then the inorganic layer forming precursor layer is thermally baked to form an inorganic layer.
  • a functional film is produced by closely adhering and transferring the formed inorganic layer to the plastic film surface under the condition that the temperature of the heat-resistant substrate is a specific temperature or higher. It is characterized by. This feature is a technical feature common to the inventions according to claims 1 to 7.
  • the highest attainable temperature in the thermal firing step is within a temperature range of 200 to 600 ° C. Is preferable from the viewpoint that can be stably formed.
  • a release layer forming step of forming a release layer on the heat resistant substrate is performed before the coating step of applying the inorganic layer forming precursor on the heat resistant substrate to form the inorganic layer forming precursor layer. It is preferable from the viewpoint that the inorganic layer can be stably transferred to the plastic film surface side when the formed inorganic layer is transferred in close contact with the plastic film surface.
  • having a film cleaning step for cleaning the surface of the transferred inorganic layer provides a higher quality functional film by removing the release layer remaining on the inorganic layer. From the viewpoint of being able to do so.
  • the heat-resistant substrate is an endless heat-resistant substrate that is continuously conveyed, and the coating process, the heat-firing process, and the cooling
  • the process and the transfer process are online processes in which the endless heat-resistant substrate is continuously conveyed.
  • ⁇ is used to mean that the numerical values described before and after it are included as a lower limit value and an upper limit value.
  • a coating step of coating an inorganic layer forming precursor on a heat resistant substrate to form an inorganic layer forming precursor layer (2) a thermal firing step of thermally firing the formed inorganic layer forming precursor layer to form an inorganic layer; (3) a cooling step for cooling the formed inorganic layer; (4) Adhering step between the surface of the heat-resistant substrate having the inorganic layer and the plastic film surface; (5) a transfer step of transferring the inorganic layer to the plastic film surface;
  • the technical feature is that (3) the temperature at which the inorganic layer and the plastic film surface are adhered and transferred in the (4) adhesion step and (5) transfer step after the cooling step.
  • the heat-resistant substrate is cooled and the temperature is lowered to 40 ° C.
  • an adhesive layer application step of forming an adhesive layer on the plastic film (7) Applying an inorganic layer forming precursor on a heat resistant substrate to form an inorganic layer forming precursor layer (1) Forming a release layer that forms a release layer on the heat resistant substrate before the coating step Process, Can be provided as needed.
  • the above steps (1) to (7) may be carried out by a batch method (also referred to as a single wafer method or an offline method).
  • a batch method also referred to as a single wafer method or an offline method.
  • the above steps (1) to (7) are performed in a roll-to-roll system (also referred to as an online system).
  • the method of performing is preferable from the viewpoint of realizing high productivity.
  • FIG. 1 shows a single-wafer manufacturing process flow as an example of a method for manufacturing a functional film of the present invention.
  • process route 1 which is a process for forming an inorganic layer
  • the surface of the heat-resistant substrate 1 is subjected to plasma cleaning 2 or the like in step A to clean the surface of the heat-resistant substrate 1.
  • the release layer 3 is formed on the heat-resistant substrate 1 washed in the process B while the heat-resistant substrate 1 is conveyed by the conveyance roller DR using the coater C1.
  • the formed release layer 3 in the wet state is dried in step C using the drying device 4 while blowing warm air 6 from the heating means 5.
  • Step D a coating liquid for forming an inorganic layer forming precursor layer is applied on the dried release layer 3 using the coater C2, thereby forming the inorganic layer forming precursor layer 7.
  • the formed heat-resistant substrate 1 inorganic layer forming precursor layer 7 is dried with warm air 6 in the drying step of Step E having the same configuration as Step C.
  • the heat-resistant substrate 1 having the dried inorganic layer forming precursor layer 7 is transferred to the thermal firing step which is Step F, and is heated and heated to a predetermined temperature by the thermal firing member 9 using the thermal firing apparatus 8.
  • the inorganic layer forming precursor layer 7 is subjected to a heat baking treatment to be converted into the inorganic layer 10.
  • the heat-resistant base material 1 converted into the inorganic layer 10 by the heat baking treatment is transferred to the cooling step which is the step G, and the cooling member 12 incorporated in the cooling device 11 is blown with the cold air 13 to start cooling.
  • process route 2 in process H.
  • a plastic film 21 constituting a functional film is prepared, and in Step I, an adhesive layer 22 is applied to the surface of the plastic film 21 with a coater C3, and drying is performed in the same manner as in Step C as necessary.
  • the plastic film 21 with the adhesive layer 22 having the adhesive layer 22 already formed on another line may be used.
  • Step G the temperature (T 2 ) until the heat-resistant substrate 1 having the inorganic layer 10 is cooled from the heat firing temperature and the temperature of the heat-resistant substrate 1 decreases to reach 40 ° C.
  • the inorganic layer 10 and the adhesive layer 22 provided on the plastic film 21 produced in the process route 2 are bonded in the process J.
  • the crimping process of the process K it crimps
  • the functional film unit 15 is separated.
  • the separated functional film unit 15 is subjected to a cleaning process on the film surface in Step N to remove an unnecessary release layer, thereby producing the functional film unit 15.
  • a metal substrate excellent in heat resistance is preferable, and for example, nickel, stainless steel (SUS), carbon steel, titanium alloy and the like can be used.
  • the thickness of the heat-resistant substrate is preferably configured within a range of 0.3 to 2.0 mm.
  • cleaning treatment means 2 for the surface of the heat-resistant substrate known cleaning means such as a plasma cleaning method and a dry ice cleaning method can be applied.
  • atmospheric pressure plasma is suitably used as a cleaning treatment condition by the plasma cleaning apparatus.
  • the cleaning conditions include conditions in which a cleaning surface modification treatment is performed using a nitrogen gas containing 1 to 20% by volume of oxygen, a frequency of 100 kHz to 150 MHz, a voltage of 10 V to 10 kV, and an irradiation distance of 5 to 20 mm.
  • the plasma cleaning apparatus for example, an atmospheric pressure plasma surface treatment apparatus AP Plasma manufactured by E-square Co., Ltd. using a dielectric barrier discharge downstream type plasma head can be mentioned.
  • the material constituting the release layer 3 according to the present invention is not particularly limited as long as it is a material having a release function, but polyvinyl pyrrolidones (including vinyl pyrrolidone polymers) are preferably used.
  • polyvinylpyrrolidones include polyvinylpyrrolidone (Mw about 40,000), polyvinylpyrrolidone (Mw about 9,000), polyvinylpyrrolidone (Mw about 16,000), vinylpyrrolidone-vinyl acetate copolymer (copolymerization mole).
  • polyvinyl pyrrolidone examples include a polyvinyl pyrrolidone single polymer.
  • the polyvinyl pyrrolidone preferably has a viscosity average molecular weight of 5000 to 50000.
  • polyvinyl pyrrolidone a commercial item can also be used and specifically, PSFK15 and PVPK30 by BASF Japan are mentioned.
  • the polyvinyl pyrrolidone is dissolved in an appropriate solvent, for example, an organic solvent such as water or alcohol to prepare a release layer forming coating solution.
  • an appropriate solvent for example, an organic solvent such as water or alcohol to prepare a release layer forming coating solution.
  • the coater C1 used in the step B is not particularly limited as long as it is a wet coater.
  • the coating device include a coater, an extrusion type coater, a slide type coater, and an inkjet head.
  • the temperature at the time of application of the release layer forming coating liquid is not particularly limited, and can be carried out by appropriately selecting an optimum temperature.
  • the layer thickness of the release layer 3 is not particularly limited, but the layer thickness after the process C (drying process-1) shown below is within a range of about 0.2 to 10 ⁇ m. Yes, preferably in the range of 0.5 to 5.0 ⁇ m, more preferably in the range of 1.0 to 3.0 ⁇ m.
  • drying apparatus 4 examples include a heating apparatus such as a warm air heating method or a heater heating method (for example, a panel heater, a halogen heater, or the like).
  • a heating apparatus such as a warm air heating method or a heater heating method (for example, a panel heater, a halogen heater, or the like).
  • the heating means 5 constituting the specific drying apparatus 4 includes a heater heating method (for example, a method in which infrared heaters, halogen heaters, panel heaters and the like are installed above and below the heat-resistant substrate 1 and heated by radiant heat), a heat-resistant group As a transport roller (not shown) for transporting the material 1, a method of heating using a heat roller, a hot air heating method (for example, temperature-controlled hot air is blown from the top and bottom of the heat-resistant substrate 1, and a release layer In the present invention, the hot air heating method is preferable because temperature control can be performed with high accuracy.
  • a heater heating method for example, a method in which infrared heaters, halogen heaters, panel heaters and the like are installed above and below the heat-resistant substrate 1 and heated by radiant heat
  • a heat-resistant group As a transport roller (not shown) for transporting the material 1, a method of heating using a heat roller, a hot air heating method (for example, temperature-controlled hot air is blown
  • Step C of FIG. 1 the heat-resistant substrate 1 on which the wet release layer 3 ⁇ / b> A is formed in Step B is transferred to the drying device 4 by the transport roller DR.
  • the drying device 4 is provided with heating means 5 on the upper part (the release layer 3 surface side) and the lower part (the back surface side of the heat resistant base material 1) of the heat resistant base material 1, respectively. Is sprayed to dry the release layer 3.
  • Step D Coating process of coating solution for forming inorganic layer forming precursor layer
  • a coating liquid for forming the inorganic layer forming precursor layer is applied on the release layer 3.
  • a coating liquid for forming an inorganic layer forming precursor layer using a coater C2 is applied on the release layer 3 of the heat-resistant substrate 1 conveyed by a conveyance roller (not shown) or the like from the process C.
  • a conveyance roller not shown
  • the wet inorganic layer forming precursor layer 7A is formed.
  • the inorganic layer forming precursor contained in the inorganic layer forming precursor layer 7 (7A) is a material that is converted into an inorganic layer by heat treatment in the subsequent heat firing step (step F). Materials can be mentioned.
  • Inorganic layer forming precursor examples include, for example, polysilazane, polysiloxane, polysilane, glass frit, glass paste and the like as the SiO 2 precursor.
  • the “polysilazane” used in the present invention is a polymer having a silicon-nitrogen bond in the structure, and has SiO 2 , Si 3 N 4 having a bond such as Si—N, Si—H, or N—H, and an intermediate between them.
  • a polymer made of ceramic precursor inorganic polymer such as a solid solution SiO x N y as a precursor of silicon oxide nitride, for example, a unit represented by the following general formula described in JP-a-8-112879 (1)
  • a compound having a main skeleton is preferred.
  • R 1 , R 2, and R 3 each represent a hydrogen atom, an alkyl group, an alkenyl group, a cycloalkyl group, an aryl group, an alkylsilyl group, an alkylamino group, or an alkoxy group.
  • perhydropolysilazane in which all of R 1 , R 2 and R 3 are hydrogen atoms is particularly preferred from the viewpoint of the denseness as the gas barrier layer to be obtained.
  • organopolysilazane in which a part of the hydrogen atom bonded to Si is substituted with an alkyl group or the like has an alkyl group such as a methyl group, thereby improving the adhesiveness with the release layer 3 which is an underlayer.
  • the ceramic film made of hard and brittle polysilazane can be provided with toughness, and even when the film thickness (average film thickness) is made thicker, the occurrence of cracks can be suppressed. Accordingly, perhydropolysilazane and organopolysilazane may be appropriately selected according to the application, and may be used in combination.
  • Perhydropolysilazane is presumed to have a linear structure and a ring structure centered on 6- and 8-membered rings.
  • the number average molecular weight (Mn) is about 600 to 2000 (polystyrene conversion), and there are liquid or solid substances, and the state varies depending on the molecular weight. These are marketed in a solution state dissolved in an organic solvent, and the commercially available product can be used as it is as a polysilazane-containing coating solution.
  • a silicon alkoxide-added polysilazane obtained by reacting a silicon alkoxide with a polysilazane having a main skeleton composed of a unit represented by the above general formula (1) (for example, Japanese Patent Laid-Open No. Hei. No.
  • glycidol-added polysilazanes obtained by reacting glycidol see, for example, JP-A-6-122852
  • alcohol-added polysilazanes obtained by reacting with alcohol see, for example, JP-A-6-6 240208
  • a metal carboxylate-added polysilazane obtained by reacting a metal carboxylate see, for example, JP-A-6-299118
  • Acetylacetonate complex-added polysilazane (in example, JP-A 6-306329 JP reference.), Fine metal particles of the metal particles added polysilazane obtained by adding (e.g., JP-A-7-196986 JP reference.), And the like.
  • amines or metal catalysts can be added to promote conversion to a silicon oxide compound.
  • Specific examples include Aquamica NAX120-20, NN110, NN310, NN320, NL110A, NL120A, NL150A, NP110, NP140, and SP140 manufactured by AZ Electronic Materials Co., Ltd.
  • an organic solvent for preparing a coating liquid containing polysilazane it is preferable to avoid using an alcohol or water-containing one that easily reacts with polysilazane.
  • hydrocarbon solvents such as aliphatic hydrocarbons, alicyclic hydrocarbons, aromatic hydrocarbons, halogenated hydrocarbon solvents, aliphatic ethers, fats Ethers such as cyclic ethers
  • hydrocarbons such as pentane, hexane, cyclohexane, toluene, xylene, solvesso and turben, halogen hydrocarbons such as methylene chloride and trichloroethane, dibutyl ether and dioxane
  • ethers such as tetrahydrofuran.
  • organic solvents may be selected according to the solubility of polysilazane, the evaporation rate of the solvent, and the like, and a plurality of organic solvents may be mixed.
  • polysiloxane with terminal Si-H An example of a polysiloxane having a methyl group as an organic group and terminated with Si—H is represented by the following general formula (2).
  • the organic group may be other than a methyl group, for example, a phenyl group, or may be different such that each organic group is mixed.
  • polysiloxane with terminal Si-OH An example of a polysiloxane having a methyl group as an organic group and terminated with Si—OH is represented by the following general formula (3).
  • the organic group may be other than a methyl group, for example, a phenyl group, or may be different such that each organic group is mixed.
  • polysiloxane with Si-H in the side chain An example of a polysiloxane having a methyl group as an organic group and Si—H in the side chain is represented by the following general formula (4).
  • the organic group may be other than a methyl group, for example, a phenyl group, or may be different such that each organic group is mixed.
  • n is in the range of 1 to 100, preferably 30 to 100, and more preferably 50 to 100.
  • glass frit and glass paste examples include powder glass manufactured by AGC Electronics (for example, trade names: ASF series, SK-231-300, KF 9173, LS-5-300M, etc.) and glass paste (AP series, etc.). And the like.
  • organic compounds containing the following metal elements can be exemplified.
  • silicon compound examples include silane, tetramethoxysilane, tetraethoxysilane, tetra n-propoxysilane, tetraisopropoxysilane, tetra n-butoxysilane, tetra t-butoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, and diethyl.
  • titanium compounds include titanium methoxide, titanium ethoxide, titanium isopropoxide, titanium tetraisoporooxide, titanium n-butoxide, titanium diisopropoxide (bis-2,4-pentanedionate), titanium.
  • examples thereof include diisopropoxide (bis-2,4-ethylacetoacetate), titanium di-n-butoxide (bis-2,4-pentanedionate), titanium acetylacetonate and butyl titanate dimer.
  • Zirconium compounds include zirconium n-propoxide, zirconium n-butoxide, zirconium t-butoxide, zirconium tri-n-butoxide acetylacetonate, zirconium di-n-butoxide bisacetylacetonate, zirconium acetylacetonate, zirconium acetate and Zirconium hexafluoropentanedioate and the like can be mentioned.
  • aluminum compounds include aluminum ethoxide, aluminum triisopropoxide, aluminum isopropoxide, aluminum n-butoxide, aluminum s-butoxide, aluminum t-butoxide, aluminum acetylacetonate, and triethyldialuminum tri-s-butoxide. Can be mentioned.
  • the same wet coater as described in the step B can be used.
  • the coating thickness can be set appropriately according to the purpose.
  • the coating thickness is about 10 nm to 10 ⁇ m after drying, preferably about 10 nm to 1 ⁇ m.
  • drying apparatus 4 applicable in the process E the same apparatus as the drying apparatus 4 described in the above-mentioned process C can be exemplified.
  • Process F Thermal firing process
  • the inorganic layer forming precursor layer 7 formed in the process E is subjected to a heat baking treatment to be modified into a gas barrier layer composed of the inorganic layer 10, for example, SiO 2 .
  • the thermal baking apparatus 8 is used to apply high-temperature thermal energy to the inorganic layer forming precursor layer 7 formed of, for example, polysilazane or the like, and is composed of SiO 2 or the like.
  • the inorganic layer 10 is formed.
  • a plurality of thermal baking members 9 are provided therein, and the inorganic layer forming precursor layer 7 is heated and converted into the inorganic layer 10 according to a preset temperature history.
  • the plurality of heat-fired members 9 may be disposed on both surfaces of the heat-resistant substrate 1 or may be disposed only on the surface side having the inorganic layer forming precursor layer 7. Also good.
  • the heating temperature by the plurality of heat-fired members 9 can be controlled independently, and each heat-fired member 9 is set to an optimum heating temperature so as to have a heating profile as shown in FIG. .
  • the thermal firing temperature is not particularly limited, but the highest temperature is preferably in the temperature range of 200 to 500 ° C.
  • the thermal baking apparatus is equipped with a thermometer, for example, a non-contact type reflection thermometer, and constantly monitors the temperature of the heat-resistant substrate surface during the thermal baking process. Is a preferred embodiment.
  • the baking apparatus include a roller hearth skin, a discharge plasma baking apparatus, a pulse current baking apparatus, a high-frequency baking apparatus, a near infrared baking apparatus (NIR), and the like.
  • a near-infrared baking apparatus (NIR) is preferable from the viewpoint of processing.
  • an NIR lamp manufactured by Adphos Corporation can be used as the near-infrared baking apparatus.
  • the NIR lamp made by Adphos is a lamp having a wavelength range of 800 to 1500 nm in the near infrared region and a maximum wavelength at 850 nm, and evenly to the inside of the heating object (inorganic layer forming precursor layer 7).
  • the inorganic layer 10 in which the entire film is uniformly converted into the inorganic film can be formed by allowing the heat energy to pass through the inorganic layer forming precursor layer 7 uniformly at high speed.
  • the NIR lamp that is the thermal firing member 9 may be arranged only on one surface side having the inorganic layer forming precursor layer 7.
  • the inorganic layer forming precursor layer 7 before the inorganic layer forming precursor layer 7 is subjected to heat treatment in the thermal baking step, for example, before ultraviolet rays, visible rays, infrared rays, ultrasonic waves, plasma discharges, corona discharges, microwaves, etc. Processing may be performed.
  • the process G is a process of cooling the heat-resistant substrate 1 heated to a high temperature in the process F, which is a previous process.
  • a cooling member 12 is disposed on both sides of the heat-resistant substrate 1, and a cold air 13 or the like is blown to the heat-resistant group having the inorganic layer 10.
  • the material 1 is cooled to a predetermined temperature.
  • bonding is performed at the temperature of 40 degreeC or more of the temperature of a heat-resistant base material. More specifically, the bonding temperature is preferably in the range of 60 to 200 ° C, more preferably in the range of 100 to 150 ° C.
  • the cooling means that can be applied in the cooling step includes a cooling method using a water cooling roller or a chill roller, a cooling method using cold air, and the like, but is not limited thereto.
  • the cooling device is equipped with a thermometer, for example, a non-contact type reflection thermometer, and the temperature of the heat-resistant substrate surface during the cooling process can be constantly monitored.
  • a thermometer for example, a non-contact type reflection thermometer
  • the plastic film 21 on the transfer side is preferably a transparent transparent plastic film.
  • polyesters such as polyethylene terephthalate (PET) and polyethylene naphthalate (PEN), polyethylene, polypropylene, cellophane, cellulose Acetate, cellulose triacetate (TAC), cellulose acetate butyrate, cellulose acetate propionate (CAP), cellulose acetates such as cellulose acetate phthalate, cellulose nitrate or derivatives thereof, polyvinylidene chloride, polyvinyl alcohol, polyethylene vinyl alcohol, Syndiotactic polystyrene, polycarbonate, norbornene resin, polymethylpentene, polyetherketone, polyester Imide, polyethersulfone (PES), polyphenylene sulfide, polysulfones, polyetherimide, polyetherketoneimide, polyamide, fluororesin, nylon, polymethylmethacryl
  • Step I is a step of applying an adhesive layer 22 on the prepared plastic film 21 by a wet coating method. After applying the adhesive layer 22, a drying step as described in the above-described step C may be provided as necessary.
  • the adhesive layer 22 is preferably formed of a resin component, for example, polyester resin, urethane resin, acrylic resin, melamine resin, epoxy resin, polyamide resin, vinyl chloride resin, and vinyl chloride.
  • a single resin such as a vinyl acetate copolymer resin or a mixed resin thereof can be used.
  • an adhesive "MAXIVE (registered trademark)" manufactured by Mitsubishi Gas Chemical Co., Ltd.
  • MAXIVE registered trademark
  • a polyepoxy resin as a main agent
  • a polyamine resin as a curing agent
  • the adhesive layer 22 may be composed of only one layer or may be composed of a plurality of layers.
  • the thickness of the adhesive layer 22 is preferably in the range of 1 to 100 ⁇ m, more preferably in the range of 3 to 50 ⁇ m.
  • the coater used to form the adhesive layer includes a blade coater, knife coater, impregnation coater, die coater, slot die coater, roller coater, gravure coater, bar coater, comma coater, extrusion coater, slide coater, inkjet head, etc. And a wet coating apparatus.
  • the application temperature of the adhesive layer is not particularly limited, and an optimum temperature condition can be appropriately selected within a temperature range of 20 to 50 ° C.
  • Bonding is performed after arranging the inorganic layer 10 provided on the heat-resistant substrate 1 and the adhesive layer 22 formed on the plastic film 21 to face each other.
  • the temperature at which the two are bonded is performed under a temperature condition in which the temperature of the heat-resistant substrate 1 is 40 ° C. or higher. More specifically, as described above, the bonding temperature is preferably in the range of 60 to 200 ° C., and more preferably in the range of 100 to 150 ° C.
  • the adhesiveness of an inorganic layer and a plastic film can be made high by bonding the heat resistant base material 1 and the plastic film 21 on the temperature conditions whose temperature of the heat resistant base material 1 is 40 degreeC or more. I guess. This is because adhesion and transfer at a certain high temperature level allow the inorganic layer 10 to be in close contact with the plastic film 21 with extremely high surface activity, and the plastic film 21 is softened at the temperature at the time of adhesion. By doing so, the followability with the heat-resistant substrate 1 is improved, it is possible to suppress defects such as wrinkles and unevenness at the time of transfer, and it is assumed that transfer can be performed stably.
  • the same effect as described above can be obtained by the method of reheating after cooling, since the reheating process is provided, the production line from the formation of the inorganic layer to the transfer becomes longer, and there is an opportunity for foreign matters to adhere to the surface of the inorganic layer 10. Increase. If such foreign matter adheres to the surface of the inorganic layer, the inorganic layer 10 is crushed by the attached foreign matter during transfer, resulting in a point failure, which is not a preferable method. The method is extremely excellent in obtaining a high-quality functional film.
  • the unit A produced as described above is pressure-conveyed between the nips using the nip rollers 14 and 14 ′ and is pressure-bonded. At this time, the nip rollers 14 and 14 'can be heated as necessary.
  • nip rollers 14 and 14 ' a rubber roller and a metal roller can be combined, or a rubber roller and a rubber roller can be combined.
  • Process M peeling process
  • the unit A subjected to the pressure-bonding process in the process K is peeled off.
  • a force is applied to the upper and lower sides of the unit A, and from the unit A, from the heat-resistant base material 1, the plastic film 21, the adhesive layer 22, the inorganic layer 10, and the release layer 3 (part). Separated into gas barrier film laminates to be constructed.
  • an atmospheric pressure plasma surface treatment apparatus AP Plasma manufactured by E Square Co., Ltd. using the above-described dielectric barrier discharge downstream type plasma head can be mentioned.
  • the first method is a method called a dry cleaning method (dry cleaning method).
  • dry cleaning method dry cleaning method
  • an ion beam cleaning method, a UV ozone cleaning method, a UV excimer irradiation method, a laser cleaning method, and the like can be given. .
  • the second method is a method called a wet cleaning method (wet cleaning method).
  • a wet cleaning method After immersing a substrate having a gas barrier layer in a liquid, for example, jet cleaning, bubbling cleaning, ultrasonic cleaning, running water cleaning, or the like is used. This is a method of cleaning.
  • this wet cleaning method exhibits a certain level of detergency, it requires a drying step after that, and thus has a problem that the processing time becomes long.
  • the third method is a physical peeling method in which a physical force (for example, impact force of an object) is directly applied to the surface of the gas barrier layer for cleaning.
  • a physical force for example, impact force of an object
  • shower cleaning for example, High pressure spray cleaning, ultrasonic shower cleaning, two-fluid nozzle cleaning
  • ice blast cleaning for example, micro ice jet, dry ice scrub cleaning
  • FIG. 2 shows a typical temperature history pattern in the functional film manufacturing process described above.
  • FIG. 2 mainly shows a temperature history pattern of the heat-resistant substrate 1 from the process B (release layer application process) to the process J (bonding process).
  • step B which is a step of forming the release layer 3A in a wet state
  • the heat-resistant substrate 1 has the same temperature as the release layer forming coating solution.
  • step C drying step 1
  • the heat-resistant substrate 1 is heated to a higher temperature by the heat drying step.
  • Step D the coating liquid for forming the inorganic layer forming precursor layer is applied, but the coating may be performed as it is at the temperature of Step C, which is the previous step, or after cooling once after Step C, the inorganic layer is formed. You may apply
  • a heat baking process is performed as the process F.
  • examples of the temperature rising pattern up to a desired thermal firing temperature include a method of increasing the temperature at a constant temperature increase rate and a method of increasing the temperature stepwise in block units.
  • the maximum temperature T max in the process F is in a temperature range of 200 to 600 ° C.
  • the time T for maintaining the maximum temperature T max can be set as appropriate.
  • step E drying step
  • the thermal baking treatment may be directly performed in the step F. good.
  • a cooling process is performed in the process G.
  • the process is not performed until room temperature (T 1 ) and the heat-resistant substrate 1 is still heated, that is, under the temperature condition of 40 ° C. (T 2 ) or more as the heat-resistant substrate 1. Perform the bonding process.
  • FIG. 1 an example of a method for producing a functional film by a single-wafer method is shown.
  • FIG. 3 An on-line manufacturing method based on a roll-to-roll method is more preferable.
  • FIG. 3 is a process flow diagram showing an example of an on-line manufacturing process using a roll-to-roll method, which is an example of a method for manufacturing a functional film of the present invention.
  • each device shown in FIG. 3 has the same configuration as that of each device described in FIG. 1, and description thereof is omitted here, and only the feature points of the process flow are described.
  • an endless heat-resistant substrate 1 (hereinafter also referred to as an endless belt 1A), for example, a stainless steel casting belt, is held by the support roller SR and supported. While a part of the roller SR functions as a driving roller, it is conveyed endlessly.
  • the release layer coating solution is supplied by the coater C1 to release the wet state.
  • drying is performed by the drying device 4 in Step C to form the release layer 3.
  • Step D the coating liquid for forming the inorganic layer forming precursor layer 7A was supplied onto the release layer 3 from the coater C2, and then dried in Step E to form the inorganic layer forming precursor layer 7. Thereafter, a thermal baking treatment is performed in Step F to modify the inorganic layer forming precursor layer 7 to the inorganic layer 10.
  • step G the endless belt 1 heated at a high temperature is cooled, and the temperature of the endless belt 1 is monitored with a surface thermometer installed at the exit of the step G, but the temperature of the endless belt 1 is 40 ° C. or higher. Then, it is unloaded from the cooling device 11.
  • the plastic film 21 is unloaded from the long laminating roller at the original unwinding part (unwinder part) UW, and the adhesive layer coating solution is applied onto the plastic film 21 from the coater C3 in the process I. , And the adhesive layer 22 is formed, followed by drying with the drying device 4.
  • step J After bonding in step J, niping and pressing with support roller SR and back roller BR in step K, 1 unit of heat-resistant substrate and 21 units of plastic film are separated from each other in step M, whereby a heat-resistant substrate is obtained.
  • the inorganic layer and the release layer formed on 1 are transferred onto the adhesive layer of the plastic film 21.
  • the processes J, K and M are performed almost simultaneously.
  • Step N the release layer residue adhering to the outermost surface of the plastic film 21 is removed by a film surface cleaning process. Furthermore, after application of other functional layers in the process P, for example, formation of a protective layer and the like, and drying in the process Q as necessary, the film is wound by a winding part (winder part) W. In addition, you may perform the process P which forms another functional layer in another line.
  • a winding part winder part
  • Embodiment of the manufacturing method of a functional film can be manufactured by the following embodiment, but the present invention is not limited to the manufacturing method exemplified here.
  • Step A Cleaning the surface of the heat-resistant substrate On the surface of the stainless steel casting belt that is continuously transporting the heat-resistant substrate 1, as a plasma cleaning device 2, an atmospheric pressure plasma surface treatment device AP Plasma manufactured by E-Square Co., Ltd. The surface was cleaned by plasma irradiation.
  • a plasma cleaning device 2 an atmospheric pressure plasma surface treatment device AP Plasma manufactured by E-Square Co., Ltd. The surface was cleaned by plasma irradiation.
  • Step B and Step C Mold Release Layer Formation and Drying Next, using a slot die coater (corresponding to C1) on the stainless steel casting belt continuously conveyed in Step B, polyvinyl pyrrolidone (PVP) as a release agent. ) was applied to a dry film thickness of 1.5 ⁇ m and dried in Step C to form a release layer 3.
  • PVP polyvinyl pyrrolidone
  • Step D and Step E Application and Drying of Inorganic Layer Forming Precursor Layer
  • PHPS perhydropolysilazane
  • the film was applied using a slot die coater (corresponding to C2) under the condition that the film thickness after drying was 50 nm, and then dried in Step E.
  • Step F Thermal Firing Step Next, in Step F, an NIR lamp manufactured by Adphos is used as the thermal firing device 8 and heated at 280 ° C. for 1 minute, and then heated at 500 ° C. for 3 minutes as the maximum temperature (T max ). Then, the inorganic layer forming precursor layer 7 was modified to form the inorganic layer 10.
  • an NIR lamp manufactured by Adphos is used as the thermal firing device 8 and heated at 280 ° C. for 1 minute, and then heated at 500 ° C. for 3 minutes as the maximum temperature (T max ). Then, the inorganic layer forming precursor layer 7 was modified to form the inorganic layer 10.
  • Step G Cooling Step Next, in the cooling step, cold air was blown from both sides of the casting belt to cool the heat-resistant substrate 1 to 120 ° C.
  • Step I Formation of Adhesive Layer Separately, in Process Route 2, a polyethylene terephthalate (PET) film having a thickness of 100 ⁇ m as a plastic film 21 and an adhesive for gas barrier dry laminate epoxy resin as an adhesive “MAXIVE (registered trademark)” “Mitsubishi Gas Chemical Co., Ltd.” was applied at a thickness of 10 ⁇ m and dried to form an adhesive layer 22.
  • PET polyethylene terephthalate
  • Steps J, K, M Pasting and Separation Next, the cooling step was passed, and the casting belt having a substrate temperature of 120 ° C. and the PET film were pasted with the inorganic layer and the adhesive layer facing each other. Subsequently, both base materials were separated and the release layer 3 and the inorganic layer 10 on the heat-resistant base material 1 were transferred onto the PET film.
  • Step N Film cleaning step Next, the surface of the transferred PET film is subjected to a plasma cleaning treatment for 1 minute using an atmospheric plasma surface treatment apparatus AP Plasma manufactured by E-Square Co., Ltd., and remains on the surface.
  • the release agent polyvinyl pyrrolidone
  • the release agent was removed, and the gas barrier film unit 15 was produced.
  • Vapor deposition equipment JEE-400 vacuum vapor deposition equipment manufactured by JEOL Ltd. Constant temperature and humidity oven: Yamato Humidic Chamber IG47M ⁇ raw materials> Metal that reacts with water and corrodes: Calcium (granular) Water vapor impermeable metal: Aluminum ( ⁇ 3-5mm, granular) (Preparation of water vapor barrier property evaluation sample) Using a vacuum deposition apparatus (vacuum deposition apparatus JEE-400 manufactured by JEOL Ltd.), metallic calcium was deposited in a size of 12 mm ⁇ 12 mm through the mask on the inorganic layer forming surface of the produced gas barrier film unit. At this time, the deposited film thickness was set to 80 nm.
  • the mask was removed in a vacuum state, and aluminum was vapor-deposited on the entire surface of one side of the sheet to perform temporary sealing.
  • the vacuum state is released, quickly transferred to a dry nitrogen gas atmosphere, and a quartz glass with a thickness of 0.2 mm is bonded to the aluminum deposition surface via an ultraviolet curing resin for sealing (manufactured by Nagase ChemteX).
  • a water vapor barrier property evaluation sample was prepared by irradiating ultraviolet rays to cure and adhere the resin to perform main sealing.
  • the obtained sample was stored under high temperature and high humidity of 60 ° C. and 90% RH, and the state of metallic calcium corroding with respect to the storage time was observed. Observation is performed every hour for up to 6 hours, every 3 hours for up to 24 hours, every 6 hours for up to 48 hours thereafter, and every 12 hours thereafter, a 12 mm x 12 mm metal
  • the area where metallic calcium corroded relative to the calcium deposition area was calculated in%.
  • the time when the area where the metal calcium corrodes becomes 1% is obtained by interpolating from the observation result by a straight line, and the metal calcium vapor deposition area, the amount of water vapor corroding the metal calcium for the area of 1%, and the time required for it. From the relationship, the water vapor transmission rate of each gas barrier film unit was calculated.
  • the water vapor permeability of the produced gas barrier film unit was 2.0 ⁇ 10 ⁇ 4 g / (m 2 ⁇ 24 h).
  • the visible light transmittance was measured using a spectrophotometer V-570 (manufactured by JASCO Corporation). As a result, the transmittance at 590 nm was 92%.
  • the gas barrier film unit produced above was cut into a size of 00 mm ⁇ 100 mm, stored for 24 hours in an environment of 40 ° C. and 90% RH, and then stored for 2 hours in an environment of 40 ° C. and 10% RH. A test was conducted. Next, the gas barrier film unit was moved to an environment of 23 ° C. and 55% RH, placed on a flat quartz plate, and the average value of the height of lifting from the quartz plate surface at the four corners was measured. As a result of evaluating the flatness of the gas barrier film unit, the evaluation rank was “ ⁇ ”.
  • the functional film (gas barrier film unit) produced by the method for producing a functional film of the present invention has gas barrier properties (water vapor barrier properties), transparency and flatness. It was confirmed that it was excellent in performance.
  • the method for producing a functional film of the present invention is a functional film excellent in functionality (for example, gas barrier properties), transparency and flatness, without requiring large equipment, in a simple manner, economically and It has excellent production stability and can be produced at a high production capacity (production speed), and the functional film obtained thereby can be used for packaging products that require the blocking of various gases such as water vapor and oxygen, and for foods. It can be suitably used as a packaging application for preventing alteration of industrial articles and pharmaceuticals, and as an electronic device material such as a liquid crystal display element, a solar cell, and an organic electroluminescence substrate.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Ceramic Engineering (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)
  • Laminated Bodies (AREA)

Abstract

La présente invention vise à proposer un procédé de fabrication de film fonctionnel, permettant de fabriquer un film fonctionnel ayant une excellente fonctionnalité (par exemple, une propriété d'étanchéité au gaz), transparence et planéité comportant un excellent rendement économique et une excellente stabilité de production, et ayant une productivité élevée par un procédé simple sans nécessiter d'installation à grande échelle. Le procédé de fabrication de film fonctionnel est un procédé pour fabriquer un film fonctionnel au moyen d'une étape d'application consistant à appliquer un précurseur formant couche inorganique sur un substrat thermorésistant pour former une couche de précurseur formant couche inorganique, une étape de combustion consistant à brûler la couche de précurseur formant couche inorganique formée pour former une couche inorganique, une étape de refroidissement consistant à refroidir la couche inorganique formée, une étape de fixation étroite consistant à fixer étroitement une surface ayant la couche inorganique du substrat thermorésistant et une surface de film plastique l'une à l'autre, et une étape de transfert consistant à transférer la couche inorganique vers la surface de film plastique après la fixation étroite, le procédé étant caractérisé en ce que l'étape de transfert est réalisée avant que la température du substrat thermorésistant ne chute à 40 °C après l'étape de refroidissement.
PCT/JP2014/059737 2013-04-23 2014-04-02 Procédé de fabrication de film fonctionnel WO2014175023A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
JP2013-089922 2013-04-23
JP2013089922A JP2016128211A (ja) 2013-04-23 2013-04-23 機能性フィルムの製造方法

Publications (1)

Publication Number Publication Date
WO2014175023A1 true WO2014175023A1 (fr) 2014-10-30

Family

ID=51791604

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/JP2014/059737 WO2014175023A1 (fr) 2013-04-23 2014-04-02 Procédé de fabrication de film fonctionnel

Country Status (2)

Country Link
JP (1) JP2016128211A (fr)
WO (1) WO2014175023A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018180963A1 (fr) * 2017-03-30 2018-10-04 リンテック株式会社 Stratifié barrière contre les gaz, corps d'étanchéité, stratifié conducteur, et procédé de production d'un stratifié conducteur

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019003494A1 (fr) * 2017-06-26 2019-01-03 大日本印刷株式会社 Feuille de transfert thermique
KR102034000B1 (ko) * 2018-03-19 2019-10-18 건국대학교 산학협력단 롤투롤 그라비어 방법을 이용한 에칭장치 및 이를 이용한 에칭방법

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1124081A (ja) * 1997-06-27 1999-01-29 Minnesota Mining & Mfg Co <3M> 光学要素および積層体転写シート
JP2006160893A (ja) * 2004-12-08 2006-06-22 Nitto Denko Corp 無機粉体含有樹脂組成物、膜形成材料層、転写シート、誘電体層形成基板の製造方法、及び誘電体層形成基板
JP2007022075A (ja) * 2005-06-14 2007-02-01 Asahi Kasei Corp 層構造体及びその製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH1124081A (ja) * 1997-06-27 1999-01-29 Minnesota Mining & Mfg Co <3M> 光学要素および積層体転写シート
JP2006160893A (ja) * 2004-12-08 2006-06-22 Nitto Denko Corp 無機粉体含有樹脂組成物、膜形成材料層、転写シート、誘電体層形成基板の製造方法、及び誘電体層形成基板
JP2007022075A (ja) * 2005-06-14 2007-02-01 Asahi Kasei Corp 層構造体及びその製造方法

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2018180963A1 (fr) * 2017-03-30 2018-10-04 リンテック株式会社 Stratifié barrière contre les gaz, corps d'étanchéité, stratifié conducteur, et procédé de production d'un stratifié conducteur
JPWO2018180963A1 (ja) * 2017-03-30 2020-02-06 リンテック株式会社 ガスバリア性積層体、封止体、導電性積層体、及び導電性積層体の製造方法
JP7082972B2 (ja) 2017-03-30 2022-06-09 リンテック株式会社 ガスバリア性積層体、封止体、導電性積層体、及び導電性積層体の製造方法

Also Published As

Publication number Publication date
JP2016128211A (ja) 2016-07-14

Similar Documents

Publication Publication Date Title
US9603268B2 (en) Gas barrier film, method of producing a gas barrier film, and electronic device
KR101526083B1 (ko) 가스 배리어성 필름, 가스 배리어성 필름의 제조 방법 및 전자 디바이스
KR101461346B1 (ko) 가스 배리어성 필름, 가스 배리어성 필름의 제조 방법 및 전자 디바이스
JP6638182B2 (ja) 積層フィルムおよびフレキシブル電子デバイス
KR101430892B1 (ko) 가스 배리어성 필름 및 전자 디바이스
JP5716752B2 (ja) ガスバリアフィルムの製造方法、ガスバリアフィルムおよび電子デバイス
EP2851192A1 (fr) Film de barrière vis-à-vis des gaz, procédé de fabrication pour film de barrière vis-à-vis des gaz, et dispositif électronique
KR20140019869A (ko) 가스 배리어성 필름 및 그의 제조 방법
JP5861644B2 (ja) ガスバリア性フィルムの製造方法、及びガスバリア性フィルム
WO2014175023A1 (fr) Procédé de fabrication de film fonctionnel
KR20210000275A (ko) 전자 디바이스의 제조 방법
WO2015105188A1 (fr) Film formant barrière contre les gaz et dispositif électronique le comprenant
JP2015128829A (ja) 転写体及び転写体を用いた機能性フィルムの製造方法
US20150344651A1 (en) Process for manufacturing gas barrier film
JPWO2015108086A1 (ja) ガスバリア性フィルムおよびこれを含む電子デバイス
JP2014213221A (ja) 機能性フィルムの製造方法
JP2015168238A (ja) 複合積層フィルムの製造方法

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 14787618

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 14787618

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: JP