WO2003020501A2 - Corps stratifie multicouches soudees par faisceau electronique et son procede d production - Google Patents

Corps stratifie multicouches soudees par faisceau electronique et son procede d production Download PDF

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Publication number
WO2003020501A2
WO2003020501A2 PCT/US2002/019950 US0219950W WO03020501A2 WO 2003020501 A2 WO2003020501 A2 WO 2003020501A2 US 0219950 W US0219950 W US 0219950W WO 03020501 A2 WO03020501 A2 WO 03020501A2
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WO
WIPO (PCT)
Prior art keywords
laminated body
resin
multilayer
electron beam
multilayer laminated
Prior art date
Application number
PCT/US2002/019950
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English (en)
Other versions
WO2003020501A3 (fr
Inventor
Tatsuo Fukushi
Keizo Yamanaka
Original Assignee
3M Innovative Properties Company
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 3M Innovative Properties Company filed Critical 3M Innovative Properties Company
Priority to US10/483,874 priority Critical patent/US20040185258A1/en
Priority to AU2002345835A priority patent/AU2002345835A1/en
Priority to EP02744579A priority patent/EP1417092A2/fr
Publication of WO2003020501A2 publication Critical patent/WO2003020501A2/fr
Publication of WO2003020501A3 publication Critical patent/WO2003020501A3/fr

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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
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/16—Layered products comprising a layer of synthetic resin specially treated, e.g. irradiated
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
    • B29C65/1403—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the type of electromagnetic or particle radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
    • B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
    • B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
    • B29C65/1403—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the type of electromagnetic or particle radiation
    • B29C65/1425—Microwave radiation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/01—General aspects dealing with the joint area or with the area to be joined
    • B29C66/05—Particular design of joint configurations
    • B29C66/10—Particular design of joint configurations particular design of the joint cross-sections
    • B29C66/11—Joint cross-sections comprising a single joint-segment, i.e. one of the parts to be joined comprising a single joint-segment in the joint cross-section
    • B29C66/112—Single lapped joints
    • B29C66/1122—Single lap to lap joints, i.e. overlap joints
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
    • B29C66/40—General aspects of joining substantially flat articles, e.g. plates, sheets or web-like materials; Making flat seams in tubular or hollow articles; Joining single elements to substantially flat surfaces
    • B29C66/41—Joining substantially flat articles ; Making flat seams in tubular or hollow articles
    • B29C66/45—Joining of substantially the whole surface of the articles
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    • B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
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    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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    • B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
    • B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
    • B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
    • B29C35/0866—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using particle radiation
    • B29C2035/0877—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using particle radiation using electron radiation, e.g. beta-rays
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
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    • B29C66/00—General aspects of processes or apparatus for joining preformed parts
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    • B29C66/71—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the composition of the plastics material of the parts to be joined
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/7392—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoplastic
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    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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    • B29C66/7394—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material characterised by the intensive physical properties of the material of the parts to be joined, by the optical properties of the material of the parts to be joined, by the extensive physical properties of the parts to be joined, by the state of the material of the parts to be joined or by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of the parts to be joined being a thermoplastic or a thermoset characterised by the material of at least one of the parts being a thermoset
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Definitions

  • the present invention relates to a multilayer laminated body comprising three or more laminated resin sheets and to a process for its production, and more- specifically it relates to a multilayer laminated body wherein the layers are bonded together by electron beam radiation and to a process for its production, the multilayer laminated body being useful as a multilayer optical sheet.
  • Prior Art Optical interference filters which reflect light at high efficiency due to their multilayer structures of resin films with different refractive indexes are known. Prior research on reflection of light from multilayered resin films may be found in Alfrey et al . , Polymer Engineering and Science, Vol.9, No.6, pp.400-404, 1964, Radford et al . , Polymer Engineering and Science, Vol .13 , No .3 , pp.216-221, etc .
  • laminated bodies of approximately 500 layers prepared by alternating lamination of resins with different refractive indexes (polyesters, polycarbonates, acrylic polymers, etc.), having layer thicknesses selected for 1/4 wavelength, can exhibit an average reflectivity of about 99% in the total visible light range.
  • the orientation of the resin films of the laminated body can be utilized to achieve a polarizer structure.
  • the thickness of each layer (resin film) in such multilayer structures may be, for example, approximately a few hundred nanometers .
  • Such multilayer optical sheets are produced by multilayer melt extrusion of the necessary number of layers of two types of thermoplastic resins with different refractive indexes, and rapid drawing thereof (for example, U.S. Patent No. 3,773,882, No. 3,195,865, etc.).
  • molten resins are collected in a feed block from two, three or more extruders, forming therein a flow of a multilayer structure with the resins alternately repeating, for example, a multilayer structure of 2 layers (ABABAB ... ) or 3 layers (ABCABC...), and after extrusion thereof with an ordinary single manifold flat film die while simultaneously adjusting the die width, the exiting multilayer sheet is rapidly drawn to produce a multilayer optical sheet.
  • Fluorine-containing materials or polyolefin-based materials are sometimes preferred for use as resin films for constitution of multilayer optical sheets. These materials have low surface energy and low adhesion with other resins, and do not form adhesion in multilayer njesin films during production by extrusion and stretching. Consequently, it has been essentially impossible to avoid peeling between the resin films or bulging in the multilayer ' optical sheet caused by changes in environmental humidity or temperature during use of multilayer optical sheets or mechanical action during handling. When such a multilayer optical sheet is actually incorporated into a device, a device construction is adopted which minimizes peeling between the three or more layers of resin films. However, the possibility of peeling between resin films due to the conditions of use still remains. It has therefore been desirable to provide sufficient bonding between resin films of such multilayer resin sheets.
  • Toray Co. has disclosed a class of inventions using fluorine-containing resin films as base materials, and notable among them is Japanese Unexamined Patent Publication HEI No. 10-58617 which discloses a mending sheet having an antifouling layer on one side of a fluorine resin film and an adhesive layer on the other side.
  • the adhesion between the fluorine resin film and the antifouling and adhesive layers is promoted by surface treatment or primary coat treatment.
  • An ultraviolet absorbing layer is provided between the fluorine resin film and the adhesive layer, and addition of a crosslinking agent to the ultraviolet absorbing layer allows crosslinking by heat, ultraviolet radiation or electron beam radiation.
  • the adhesion between the fluorine resin film and the ultraviolet absorbing layer is promoted by surface treatment or primary coat treatment .
  • Japanese Unexamined Patent Publication HEI No. 4-146129 describes a fluorine-containing resin film which has a printing layer formed by an ink resin composition on the surface of a metal whereby thermal bonding forms a resin-coated metal, for which reason the ink resin composition is composed of an energy beam-curing resin.
  • the printing layer is only partially printed on the fluorine-containing resin film, and the fluorine-containing resin film is thermally bonded to the metal surface.
  • the fluorine-containing resin film is thermally bonded to the metal base material and there is no adhesion between the resin films of the multilayer sheet.
  • Japanese Unexamined Patent Publication HEI No. 5- 8353 proposes using radiation crosslinking to introduce a crosslinked structure into a resin tube having a polyamide resin outer layer and a fluorine-containing resin inner layer, as a resin tube suitable for vehicle fuel tubing and the like.
  • This is a double-extruded resin product, and thus differs from the present invention which is a multilayer laminated sheet prepared by lamination of a plurality of resin films.
  • the present invention provides the following.
  • a multilayer laminated body comprising three or more layers, preferably five or more layers, more preferably ten or more layers and especially 40 or more layers of laminated resin sheets made of at least two different materials, the multilayer laminated body being characterized by having chemical bonding formed between the layers of resin sheets by electron beam radiation.
  • the multilayer laminated body of the invention is a laminated body comprising three or more layers, preferably ten or more layers and especially 40 or more layers of laminated resin sheets made of at least two different materials.
  • the multilayer laminated body of the invention wherein the constitutive resin sheets are made of at least two different materials, provides multiple layers of these resin sheets of different materials to exhibit a composite function that cannot be achieved by single resin sheets.
  • the resins of different materials are typically resins with different optical properties, and especially refractive index, which are laminated into a multilayer optical sheet, but this is not necessarily limited to optical properties.
  • resin sheets with different physical permeability may be laminated to fabricate a multilayer laminated body exhibiting multiple functions.
  • the multilayer laminated body of the invention is a laminated body prepared by laminating three or more layers, preferably ten or more layers and especially 40 or more layers of resin sheets.
  • a multilayer optical sheet usually 40 or more layers, and even from 100 to 400 layers, of resin sheets are laminated to form a reflective sheet or the like but, depending on the function, the multilayer laminated body may have three or more layers or approximately ten layers .
  • Electron beam radiation of such a multilayer laminated body to form chemical bonding between the resin sheets constituting the multilayer laminated body has been unknown in the prior art .
  • the thickness of the resin sheets constituting the multilayer laminated body of the invention may be set to ⁇ /4 for the optical thickness of each adjacent high refractive index layer and low refractive index layer, for an interference effect.
  • the optical thickness of the film is adjustable by about 40-200 nm, considering the incident angle, to obtain satisfactory reflection.
  • a similar construction may be used to fabricate a multilayer laminated body which selectively transmits only a specific wavelength range while substantially blocking other wavelength ranges, for use as an optical filter.
  • the present invention may be effectively applied in cases where each resin sheet of the multilayer laminated body is of a material with no adhesion to adjacent resin sheets, or in cases where, for example, each resin sheet is of a material with adhesion with the other resin sheets but sufficient adhesion cannot be achieved between each of the resin sheets during production of the multilayer laminated body due to restrictions inherent in the production process for the multilayer laminated body. That is, the invention may be applied for all laminated bodies prepared by laminating three or more layers, preferably ten or more layers and especially 40 or more layers of resin sheets made of at least two different types of materials, irrespective of the materials of the resin sheets.
  • the present invention is particularly effective in cases where some of the resin sheets constituting the multilayer laminated body are of materials with no adhesion with the other resin sheets, since it represents an indispensable technique.
  • low adhesion resins there may be mentioned fluorine- containing materials, silicone-based materials, polyolefin- based materials and the like.
  • the low adhesion resins are resins having a low surface energy, generally not more than 45 mJ/m 2 , further typically not more than 40 mJ/m 2 or not more than 35 mJ/m 2 .
  • Fluorine-based materials (specifically, fluorine- containing materials and fluorinated materials) to be used as resin sheets for the multilayer laminated body of the invention include, for example, fluorocarbon simple monomers, copolymers and their (mutual) blends or blends with non- fluorine-based materials.
  • Useful fluorine-containing diolefins also exist, for example, perfluorodiallyl ether and perfluoro-1, 3- butanediene. These fluorine-containing monomers may also be copolymerized with fluorine-free terminal unsaturated monoolefin comonomers such as ethylene or propylene. The content of the fluorine-containing monomer is preferably at least 50 wt% of the total monomers in the polymer mixture.
  • the fluorine-containing monomer may be- copolymerized with an iodine- or bromine-containing curing site monomer to prepare a peroxide-curable polymer.
  • Suitable curing site monomers include terminal unsaturated monoolefins of 2-4 carbons, for example, bromodifluoroethylene, bromotrifluoroethylene, iodotrifluoroethylene and 4-bromo-3 , 3 , 4, 4-tetrafluorobutene- 1.
  • fluorocarbon simple monomers, copolymers or mixtures and crosslinked mixtures with other polymers may be used.
  • Fluorine-containing materials constituting fluorine- containing material sheets have excellent chemical resistance, heat resistance, mechanical properties and electrical properties due to the presence of fluorine, and the fluorine content should therefore be at least 10 wt%, more preferably at least 30 wt% and even more preferably at least 40 wt%.
  • the fluorine content may also be 50 wt% or higher, and up to a maximum of 76 wt%.
  • a fluorine-based material sheet is preferably crosslinkable by electron beam radiation. Electron beam-disintegrating materials will require special considerations in regard to the accelerating voltage and linear density of the electron beam, and the irradiation time.
  • polytetrafluoroethylene is a polymer which disintegrates by electron beam radiation, and it is not suitable for the invention.
  • polytetrafluoroethylene may still be suitable if it is modified polytetrafluoroethylene with enhanced disintegration resistance.
  • electron beam- disintegrating materials combined with non-electron beam- disintegrating materials or crosslinking materials can avoid impairment of the film by electron beam radiation, and such materials can be used under these irradiation conditions.
  • Fluorine-containing materials may, if necessary, contain various types of additives such as coloring agents (pigments and dyes) , fillers, ultraviolet absorbers and the like.
  • the present invention may also be applied to multilayer laminated bodies comprising, for example, silicone-based materials and polyolefin-based materials, as well as acrylate-based, urethane-based, polyester-based, polycarbonate-based and polystyrene-based resins.
  • Production of multilayer laminated body The multilayer laminated body of the invention may be prepared by stacking, i.e. laminating, the constitutive resin sheets after their individual fabrication.
  • co-extrusion is preferably used as the production method for a multilayer laminated body of multiple alternating layers of different types of resin sheets.
  • Chill-roll casting, or other methods, may also be employed.
  • multilayer laminated bodies As an example, there is disclosed in WO95/17303 a multilayer laminated film comprising a plurality of alternating separate resin layers such as a crystalline naphthalene dicarboxylic acid polyester layer and a layer of a different resin such as polyester or polycarbonate, wherein the thickness of each layer is less than 0.5 ⁇ m, the refractive index of one resin in one direction is 1.9 while that in the other direction is 1.64, and the multilayer laminated film thereby exhibits a birefringence effect which is useful for polarization.
  • a multilayer laminated film comprising a plurality of alternating separate resin layers such as a crystalline naphthalene dicarboxylic acid polyester layer and a layer of a different resin such as polyester or polycarbonate, wherein the thickness of each layer is less than 0.5 ⁇ m, the refractive index of one resin in one direction is 1.9 while that in the other direction is 1.64, and the multilayer laminated film thereby exhibits a bi
  • optical sheets comprising multilayer laminated films examples include reflective sheets, non-reflective sheets and polarizing sheets.
  • the multilayer laminated body of the invention is characterized by using electron beam radiation to form chemical bonding between the resin sheets constituting the multilayer laminated body.
  • electron beam radiation to form chemical bonding between the resin sheets constituting the multilayer laminated body.
  • the multilayer laminated body of the invention is characterized by having a structure which is based on .the technique of electron beam radiation.
  • the electron beam is irradiated to all of the interfaces of the resin sheets in which it is desired to form bonding for the multilayer ⁇ laminated body.
  • the electron beam does not necessarily have to be irradiated on the entire surface of the multilayer laminated body (each resin sheet) , and for example, it may be irradiated in any type of pattern, such as selectively irradiated at the edge sections, irradiated in a lattice fashion or in one or more lines around the edge sections, or irradiated in an island or intermittent fashion.
  • the bonding when one of the resin sheets is a material with low adhesion such as a fluorine-containing material, the bonding may be formed between the resin sheets by electron beam radiation after laying an adhesion-promoting layer between each of the resin sheets .
  • the irradiation conditions for the electron beam need only be sufficient to generate radicals on the multilayered resin sheet surfaces and they will depend on the types and thicknesses of the resin sheets, but the irradiation will generally be conducted at least 10 keV of an acceleration electric field, and at least 10 kGy of a dose. It is preferably 50-200 keV of an acceleration electric field, and 30-1000 kGy of a dose.
  • the size of the chemical bonding formed between the resin sheets by the invention can be evaluated by an adhesion/peel test of the resin sheets of the resulting multilayer laminated body. Instances of a specific method are described in the examples.
  • the multilayered films of the multilayer laminated body are not only " mechanically attached by the chemical bonding formed in the multilayer laminated body, but the edge regions are also bonded into a hermetically sealed structure, so that moisture and the like from the surrounding atmosphere cannot penetrate into the multilayer laminated body.
  • a 15 cm-square polyurethane (Morthane L429.71, product of Morton International) sheet with a thickness of approximately 0.2 mm was fabricated using a hot press (Mini Test Press 10, product of Toyo Seiki Kogyo) at 180 °C, with a 0.2 mm thickness guide.
  • the thus fabricated sample was irradiated with a 20 Mrad electron beam at an accelerating voltage of 250 kV at room temperature with nitrogen replacement (oxygen concentration: approximately _ 200 ppm).
  • the electron beam apparatus used was a System 7824 Electron Curtain by Energy Science, Inc., and the line speed was 2 m/min.
  • Example 2 the obtained sample was cut into three test strips of 25 mm width to test the adhesive properties of the irradiated sample by ASTM D-1876, known as the T-peel test.
  • a Tenso eter 10 (product of Monsanto Co.) was used for measurement of the peel strength with a crosshead speed of 300 nm/min, and the average values are shown in Table 1.
  • Example 2
  • Example 3 The same procedure was repeated for Example 2, except that a 0.05 mm-thick film of THV500G (product of Dyneon Co.) was used instead of the THV200 film of Example 1. The test results are shown in Table 1.
  • Example 3 a 0.05 mm-thick film of THV500G (product of Dyneon Co.) was used instead of the THV200 film of Example 1. The test results are shown in Table 1.
  • Example 4 The same procedure was repeated for Example 3, except that a 0.1 mm-thick film of ethylene-tetrafluoroethylene copolymer (ETFE) (ET-6235J, product of Dyneon Co.) was used instead of the THV200 film of Example 1. The test results are shown in Table 1.
  • EFE ethylene-tetrafluoroethylene copolymer
  • Example 5 The same procedure was repeated for Example 5, except that a 0.2 ram-thick film of ethylene-propylene-diene monomer copolymer (EPDM) (EP-24, product of Japan Synthetic Rubber Co. Ltd.) was used instead of the urethane film of Example 2 The test results are shown in Table 1.
  • EVA ethylene-vinyl acetate copolymer
  • EPDM ethylene-propylene-diene monomer copolymer
  • Example 6 The same procedure was repeated for Example 6, except that 1 mm-thick nylon-6 fibers (680 denier) were used as the base material instead of the urethane film of Example 2. The test results are shown in Table 1. Comparative Examples 1-6
  • FKM fluorine rubber
  • FE-5830Q product of Dyneon Co.
  • FE-5830Q product of Dyneon Co.
  • the values for the component contents are all parts by weight with respect to 100 parts by weight (phr) of the fluorine rubber.
  • a 15 cm-square sheet with an approximate thickness of 1 mm was fabricated by pressing at 170 °C for 10 minutes, and then secondary vulcanization was carried out at 230 °C for 24 hours.
  • Example 7 The same procedure was repeated for Example 8, except that a 0.1 mm-thick film of ethylene-tetrafluoroethylene copolymer (ETFE) (ET-6235J, product of Dyneon Co.) was used instead of the THV500 film of Example 7.
  • EFE ethylene-tetrafluoroethylene copolymer
  • Example 9 The same procedure was repeated for Example 9, except that a 0.025 mm-thick film of polyethylene naphthalate (PEN) (Teonex film Q01, product of Teijin Co., Ltd.) was used instead of the urethane film of Example 1, and the crosshead speed in the peel test was 10 mm/min.
  • PEN polyethylene naphthalate
  • Table 4 The test results are shown in Table 4.
  • Example 9 The corresponding procedure for Example 9 was repeated for Comparative Example 9, but without electron beam radiation. The test results are shown in Table 4. Table 4
  • Example 13 After using a T-die and a 50 mm single-screw extruder (product of Research Laboratory of Plastics Technology Co., Ltd.) for extrusion of THV200 to a thickness of 0.05 mm onto a PET film (A) with a thickness of 0 " .05 mm and passage through a nip roll, a PET film (B) of the same 0.05 mm thickness was further laminated onto the THV200 side with a nip roll, and both sides were cut for a laminated film width of 300 mm to fabricate a three-layer film.
  • a PET film (B) of the same 0.05 mm thickness was further laminated onto the THV200 side with a nip roll, and both sides were cut for a laminated film width of 300 mm to fabricate a three-layer film.
  • the laminated film sample fabricated in this manner was cut into a 15 cm square and continuously irradiated with an electron beam at 20 Mrad with an accelerating voltage of 250 KV, in the same manner as Example 1, after which a test strip was prepared from the irradiated sample in the same manner as Example 1 to test the adhesive performance of the irradiated sample.
  • Table 5 shows the adhesive forces at "interface A” (PET film A-THV200) and at "interface B" (THV200-PET film B) measured for each sample from the direction of electron beam radiation, in order to determine the adhesive force between each of the layers, and the average values are listed in Table 5. Comparative Example 10
  • Example 14 demonstrates that electron beam radiation in a multilayer film reaches to the interface on the opposite side to improve adhesion.
  • An A4 size was cut out from a multilayer film (DFEF by 3M Co., over 40 layers, 100 ⁇ m thickness), and the entire surface of the multilayer film was irradiated with ari electron beam under different conditions.
  • the electron beam radiation conditions were an accelerating voltage of 200 kV, a dose of 5-15 Mrads (non-irradiated, 5 Mrads, 15 Mrads) and a nitrogen atmosphere (oxygen concentration: approximately 50 ppm) .
  • a strip was cut out with a width of 25 mm and a length of 30- cm, adhesive tape was attached to both sides at one end, and the tape was used for forced interlayer peeling of the multilayer film to approximately 5 cm to prepare a "grip section" with an approximate length of 5 cm.
  • the multilayer film strip was then placed on a tensile tester and the "grip section” was stretched while measuring the T-die peel strength. The peel rate was 300 mm.
  • the relationship between the electron beam radiation conditions and the peel strength was as follows . The values were the same at all sections of all interlayers of the multilayer film.
  • the DFEF multilayer film by 3M Co. is a type of film which is built into liquid crystal monitors and the like to increase screen brightness through reutilization of light by polarization and reflection.
  • electron beam radiation of the multilayer film allowed peeling between the films of the multilayer film to be eliminated without reducing the optical properties, thus increasing the handleability.

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  • Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Electromagnetism (AREA)
  • Mechanical Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Plasma & Fusion (AREA)
  • Thermal Sciences (AREA)
  • Laminated Bodies (AREA)

Abstract

La présente invention concerne un procédé permettant de procurer une liaison suffisante entre des feuilles de résine de feuilles multicouches au moyen d'un procédé simplifié. La solution consiste en la réalisation d'un corps stratifié comprenant au moins trois couches stratifiées de feuilles de résine constituées d'au moins deux matériaux différents, le corps stratifié multicouches étant caractérisé en ce qu'il présente une liaison chimique formée entre lesdites au moins trois couches par rayonnement de faisceau d'électrons. Les couches du film multicouches peuvent être au nombre de quelques centaines ou plus.
PCT/US2002/019950 2001-08-13 2002-06-24 Corps stratifie multicouches soudees par faisceau electronique et son procede d production WO2003020501A2 (fr)

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US10/483,874 US20040185258A1 (en) 2001-08-13 2002-06-24 Electron beam-bonded multilayer laminated body and process for its production
AU2002345835A AU2002345835A1 (en) 2001-08-13 2002-06-24 Electron beam-bonded multilayer laminated body and process for its production
EP02744579A EP1417092A2 (fr) 2001-08-13 2002-06-24 Corps stratifie multicouches soudees par faisceau electronique et son procede d production

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JP2001245709A JP2003062946A (ja) 2001-08-13 2001-08-13 電子線照射で結合された多層積層体及びその製造方法

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Cited By (2)

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WO2008124233A1 (fr) * 2007-04-05 2008-10-16 3M Innovative Properties Company Procédé de fabrication de films à base de polymères fluorés fonctionnalisés
US10801649B2 (en) 2017-09-28 2020-10-13 Saint-Gobain Performance Plastics Corporation Fuel tubings and methods for making and using same

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CN106079686A (zh) * 2008-12-30 2016-11-09 3M创新有限公司 含氟聚合物多层光学膜
JP5885068B2 (ja) * 2010-12-27 2016-03-15 大日本印刷株式会社 積層体およびその製造方法
JP2012158056A (ja) * 2011-01-31 2012-08-23 Dainippon Printing Co Ltd 積層体およびその製造方法
JP5699640B2 (ja) * 2011-01-31 2015-04-15 大日本印刷株式会社 積層体およびその製造方法
JP5699638B2 (ja) * 2011-01-31 2015-04-15 大日本印刷株式会社 積層体およびその製造方法
JP5699639B2 (ja) * 2011-01-31 2015-04-15 大日本印刷株式会社 積層体およびその製造方法
JP5699641B2 (ja) * 2011-01-31 2015-04-15 大日本印刷株式会社 積層体およびその製造方法
JP2012158054A (ja) * 2011-01-31 2012-08-23 Dainippon Printing Co Ltd 積層体およびその製造方法
JP5835643B2 (ja) * 2011-06-09 2015-12-24 大日本印刷株式会社 積層体およびその製造方法
JP5948747B2 (ja) * 2011-07-08 2016-07-06 大日本印刷株式会社 積層体およびその製造方法
JP6131733B2 (ja) * 2013-06-19 2017-05-24 大日本印刷株式会社 光学フィルムの製造方法および光学フィルム

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EP0810087A2 (fr) * 1996-05-28 1997-12-03 Kureha Kagaku Kogyo Kabushiki Kaisha Feuille multicouche thermorétractable
WO1997046384A1 (fr) * 1996-06-07 1997-12-11 Cryovac Inc. Film retrecissable avec bonne adhesion de l'encre
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WO2001002508A1 (fr) * 1999-07-02 2001-01-11 3M Innovative Properties Company Feuille autocollante et son procede de production

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WO1995017303A1 (fr) * 1993-12-21 1995-06-29 Minnesota Mining And Manufacturing Company Film optique multicouche
EP0810087A2 (fr) * 1996-05-28 1997-12-03 Kureha Kagaku Kogyo Kabushiki Kaisha Feuille multicouche thermorétractable
WO1997046384A1 (fr) * 1996-06-07 1997-12-11 Cryovac Inc. Film retrecissable avec bonne adhesion de l'encre
WO2001002508A1 (fr) * 1999-07-02 2001-01-11 3M Innovative Properties Company Feuille autocollante et son procede de production

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2008124233A1 (fr) * 2007-04-05 2008-10-16 3M Innovative Properties Company Procédé de fabrication de films à base de polymères fluorés fonctionnalisés
US10801649B2 (en) 2017-09-28 2020-10-13 Saint-Gobain Performance Plastics Corporation Fuel tubings and methods for making and using same

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