CN107083197A - Surface protection film and the optical component for being fitted with the surface protection film - Google Patents
Surface protection film and the optical component for being fitted with the surface protection film Download PDFInfo
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- CN107083197A CN107083197A CN201610886407.8A CN201610886407A CN107083197A CN 107083197 A CN107083197 A CN 107083197A CN 201610886407 A CN201610886407 A CN 201610886407A CN 107083197 A CN107083197 A CN 107083197A
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- Prior art keywords
- film
- agent layer
- surface protection
- protection film
- stripping
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- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/30—Polarising elements
- G02B5/3025—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state
- G02B5/3033—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid
- G02B5/3041—Polarisers, i.e. arrangements capable of producing a definite output polarisation state from an unpolarised input state in the form of a thin sheet or foil, e.g. Polaroid comprising multiple thin layers, e.g. multilayer stacks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
- C09J7/401—Adhesives in the form of films or foils characterised by release liners characterised by the release coating composition
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/04—Optical elements characterised by the material of which they are made; Optical coatings for optical elements made of organic materials, e.g. plastics
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
- G02B1/10—Optical coatings produced by application to, or surface treatment of, optical elements
- G02B1/14—Protective coatings, e.g. hard coatings
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/318—Applications of adhesives in processes or use of adhesives in the form of films or foils for the production of liquid crystal displays
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
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- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Polarising Elements (AREA)
Abstract
The present invention, which is provided, a kind of to be had irregular optical film to surface and can also be used, adherend is polluted less, rheological parameters' change with time, the surface protection film of excellent antistripping antistatic property with not deterioration and not using its optical component to the low stain of adherend.Surface protection film (10), it is formed by the stripping film (5) with peeling agent layer (4) of being fitted on adhering agent layer (2), stripping film (5) is formed by being laminated peeling agent layer (4) on a face of resin film (3), peeling agent layer (4) contains the remover using dimethyl silicone polymer as main component, the antistatic additive not reacted with the remover, ester plasticizer containing at least more than one ehter bond, antistatic additive composition is the ionic compound that fusing point is less than 30 DEG C, antistatic additive composition is transferred to the surface of adhering agent layer (2) with ester plasticizer from the peeling agent layer (4) of stripping film (5), stripping electrostatic pressure when reduction peels off adhering agent layer (2) from adherend.
Description
Technical field
The present invention relates to it is a kind of fit in polarizer, polarizer, it is (following for optical components such as the eyeglass films of display
Otherwise referred to as optical film) surface surface protection film.More specifically there is provided a kind of few surface of pollution to adherend
Diaphragm, further has the surface protection film of the not excellent antistripping antistatic property of deterioration, and use there is provided a kind of
The optical component of the surface protection film.
Background technology
In the past, in manufacture, transport polarizer, polarizer, the eyeglass film for display, antireflection film, hard coat film, use
When the optical articles such as the optical films such as the transparent and electrically conductive film of touch panel and the display using these films, in the light
Coating surface diaphragm on the surface of film, can prevent the dirt or scar on the surface in subsequent handling.On being used as light
The visual examination of the optical film of product is learned, in order to save the time peeled off surface protection film, pasted again, operation effect is improved
Rate, is also directly carried out in the state of surface protection film to be fitted in optical film sometimes.
Typically, in the preparation section of optical articles, in order to prevent the attachment of scar or dirt, using the one of base material film
Face is provided with the surface protection film of adhering agent layer.Surface protection film is fitted in optical film via the adhering agent layer of micro- adhesion strength
On.The reason for making adhering agent layer be micro- adhesion strength is, is peeled off by the surface protection film used from optical film surface
It during removal, can be easily peeled off, and make the non-cohesive residual (generation for preventing cull) of sticker in the production as adherend
On the optical film of product.
In recent years, in the production process of liquid crystal display panel, although the number of packages of generation is few, but still it there occurs due to that will paste
Stripping electrostatic pressure produced when removing is peeled off together in the surface protection film on optical film, is caused for controlling LCD
The circuit blocks such as the driving IC of the display picture of plate destroyed or liquid crystal molecule the phenomenon that suffers damage of orientation.
In addition, the consumption electric power in order to reduce liquid crystal display panel, the driving voltage step-down of liquid crystal material, with
This, drives IC destruction voltage also in step-down.Nearest, it is desirable to make stripping electrostatic pressure+0.7kV~-0.7kV scope it
It is interior.
In addition, recently as the popularization of 3D displays (three-dimensional display), sometimes in the table of the optical films such as polarizer
Laminating FPR (Film Patterned Retarder) film on face.Peel off the table being fitted on the surface of the optical films such as polarizer
After surface protective film, FPR films of fitting.But, if the surface of the optical film such as polarizer is by viscous used in surface protection film
When agent or antistatic additive pollution, the problem of there is difficult stickup FPR films.It is therefore desirable to the surface protection film pair for the purposes
The pollution of adherend is small.
In addition, in some liquid crystal panel producers, as evaluation method of the surface protection film to the contaminative of adherend, adopting
Using the following method：By temporarily peeling off the surface protection film being fitted on the optical films such as polarizer, the state of bubble is being mixed into
Under fit again, and it is heated under prescribed conditions, peels off surface protection film afterwards and observe the table of adherend
The method in face.In the evaluation method, if even if the surface contamination of adherend is micro, be mixed into bubble part, with
Between the part of the sticker contact of surface protection film, there is also during the difference of the surface contamination of adherend, then the table of adherend
Pollute in the form of the vestige of bubble (otherwise referred to as bubble infiltration) and remain in face.Therefore, as the dirt to adherend surface
The evaluation method of metachromia, the evaluation method is very strict evaluation method.In recent years, it is desirable to even in strict as
The result that is judged of evaluation method in, the surface protection that also there is no problem in terms of to the contaminative on the surface of adherend
Film.
When surface protection film is peeled off from the optical film as adherend, in order to prevent because height peels off electrostatic pressure institute
The generation of the undesirable condition caused, it is thus proposed that it is a kind of be used to lower suppressing peeling off electrostatic pressure, using containing antistatic
The surface protection film of the adhering agent layer of agent.
For example, Patent Document 1 discloses a kind of used by the acrylic of alkyl trimethyl ammonium salt, hydroxyl
The surface protection film for the sticker that thing, PIC are constituted.
In addition, Patent Document 2 discloses a kind of acrylate copolymer institute by ionic liquid and acid number below 1.0
The adhesion agent composition of composition and the pressure-sensitive adhesive sheets for having used the adhesion agent composition.
In addition, Patent Document 3 discloses one kind by acrylate copolymer, polyether polyols, utilize anion
Adhesion agent composition that the alkali metal salt that adsorptivity compound has been handled is constituted and the table for having used the adhesion agent composition
Surface protective film.
In addition, Patent Document 4 discloses one kind by ionic liquid, alkali metal salt, glass transition temperature be 0 DEG C with
Under the adhesion agent composition that is constituted of polymer and used the surface protection film of the adhesion agent composition.
In addition, Patent Document 5 discloses it is a kind of containing liquid ions salt, it is containing polymer, for optical component
The adhesion agent composition and adhesive sheet of surface protective plate.
Prior art literature
Patent document
Patent document 1：JP 2005-131957 publications
Patent document 2：JP 2005-330464 publications
Patent document 3：JP 2005-314476 publications
Patent document 4：JP 2006-152235 publications
Patent document 5：JP 2008-069261 publications
The content of the invention
The technical problem to be solved in the present invention
In above-mentioned patent document 1~5, antistatic additive is added with the inside of adhering agent layer.However, adhering agent layer
Thickness is thicker, or is fitted in that elapsed time after adherend is more long, then relative to the adherend for surface protection film of having fitted, and resists
The amount that electrostatic agent is transferred to adherend from adhering agent layer is more.If the amount for being transferred to the antistatic additive of adherend increases, having can
It can be reduced as the exterior quality of the optical film of adherend, when fitting FPR films, the adherence of FPR films is reduced.
If in order to reduce such antistatic additive shifted from adhering agent layer to adherend through when increase, and reduce viscous
When the thickness of oxidant layer, then other problems can be produced.For example, for the surface such as polarizer through non-glare treated in order to anti-dazzle
When having irregular optical film, there is problems with：Because adhering agent layer is difficult to follow the concavo-convex and mixed of optical film surface
Enter bubble, because the adhesion area between optical film and adhering agent layer is reduced and causes adhesion strength to reduce, surface is protected in use
Cuticula, which is produced, to be floated or comes off.
Accordingly, it would be desirable to it is a kind of for surface have irregular optical film can also be fitted, it is non-to the pollution of adherend
Often less and to the pollution of adherend even if through when the also not increased surface protection film for optical film, furthermore, it is desirable to a kind of
It can lower suppress to peel off the surface protection film for peeling off electrostatic pressure during surface protection film from adherend.
Present inventors have made intensive studies to solve these problems.
In order to adherend pollution less and pollution through when increase it is small, it is necessary to be presumed to pollution adherend reason
Adhering agent layer in antistatic additive composition carry out decrement.But, the antistatic additive composition in adhering agent layer carries out decrement
In the case of, by surface protection film from adherend peel off when stripping electrostatic pressure can increase.Therefore, have studied lower to suppress
Electrostatic pressure is peeled off when surface protection film is peeled off from adherend, without increasing the exhausted of the antistatic additive composition in adhering agent layer
To the method for amount.
Its result is found, by the adhesion agent composition without antistatic additive is coated and dried, being laminated into sticker
After layer, appropriate antistatic additive composition is only assigned on the surface of adhering agent layer, rather than will on a face of base material film
Adhesion agent composition containing antistatic additive is coated and dried, adhering agent layer is formed, so as to lower suppress from as quilt
Stripping electrostatic pressure during surface protection film is peeled off on the optical film of viscous thing, the present invention is completed with this.
The present invention is formed in view of the above circumstances, and its object is to have irregular optics for surface there is provided one kind
Can also be fitted with film, to the pollution of adherend less, to the low stain of adherend even if through when also do not change and have
There is the not surface protection film of the excellent antistripping antistatic property of deterioration and used the optical section of the surface protection film
Part.
Solve the technological means of technical problem
In order to solve the above-mentioned technical problem, inventive concept of the invention is, surface protection film of the invention passes through in base
On one face of material film by the adhesion agent composition without antistatic additive it is coated and dried, stacking adhering agent layer after, adhesion
Appropriate antistatic additive is assigned on the surface of oxidant layer, so as to lower suppress the contaminative to adherend, while lower suppressing
Stripping electrostatic pressure when being peeled off from the optical film as adherend.
In order to solve the above-mentioned technical problem, the present invention provides a kind of surface protection film, and it passes through by with the transparency
Adhering agent layer, and stripping of the laminating with peeling agent layer on the adhering agent layer are formed on one face of the base material film that resin is constituted
Formed from film, it is characterised in that the stripping film is formed by folding peeling agent layer in a surface layer of resin film, wherein, the stripping
Contain remover using dimethyl silicone polymer as main component, the antistatic additive not reacted with the remover from oxidant layer and contain
There is the ester plasticizer of at least more than one ehter bond, the antistatic additive composition is that fusing point is the ionic chemical combination less than 30 DEG C
Thing, the antistatic additive composition is transferred to the sticker with the ester plasticizer from the peeling agent layer of the stripping film
The surface of layer, the stripping electrostatic pressure when adhering agent layer is peeled off from adherend is reduced with this.
In addition, the adhering agent layer is preferably by making the sticker group containing (methyl) acrylate copolymer and crosslinking agent
Compound crosslinking is formed.
In addition, the peeling force when stripping film is peeled off from the adhering agent layer is preferably below 0.2N/50mm.
In addition, the present invention provides a kind of optical component by above-mentioned surface protection film of fitting.
Invention effect
Pollution of the surface protection film to adherend of the present invention is few, to the low stain of adherend even if through when will not also become
Change.Even in addition, the surface protection film of the present invention has irregular optical film on the surface that adherend is AG Polarizers etc.,
It can also be used.In addition, in accordance with the invention it is possible to provide it is a kind of can relatively low suppression when being peeled off from the optical film as adherend
The surface protection film of produced excellent antistripping antistatic property stripping electrostatic pressure, with not deterioration and use
The optical component of the surface protection film.
According to the surface protection film of the present invention, the surface of optical film can be definitely protected, therefore, it is possible to realize production
The raising of rate and the raising of yield rate.
Brief description of the drawings
Fig. 1 is the sectional view for representing the surface protection film concept of the present invention；
The sectional view of states of the Fig. 2 for expression by stripping film from the surface protection film of the present invention after stripping；
Fig. 3 is the sectional view of the one embodiment for representing the optical component of the present invention.
Description of reference numerals
1 ... base material film；2 ... adhering agent layers；3 ... resin films；4 ... peeling agent layers；5 ... stripping films；7 ... antistatic additive and ester
Class plasticizer；8 ... adherends (optical component)；10 ... surface protection films；11 ... peel off the surface protection film of stripping film；20…
It is fitted with the optical component of surface protection film.
Embodiment
Below by way of embodiment, the present invention will be described in detail.
Fig. 1 is the schematic diagram for representing the surface protection film concept of the present invention.The surface protection film 10 is in transparent base material film 1
A face surface on, be formed with adhering agent layer 2.On the surface of the adhering agent layer 2, it is fitted with the surface of resin film 3
It is formed with the stripping film 5 of peeling agent layer 4.
The base material film 1 used in surface protection film 10 as the present invention, using by with the transparency and pliability
The base material film that is constituted of resin.Thereby, it is possible to be used as the shape on the optical component of adherend so that surface protection film to be fitted in
State, carries out the outward appearance detection of optical component.The film being made up of the resin with the transparency as base material film 1, is suitably used
Polyethylene terephthalate, PEN, polyethylene glycol isophthalate, poly terephthalic acid fourth two
The polyester films such as alcohol ester.In addition to polyester film, as long as with required intensity and with optics adaptability, then can also be used by other
The film that resin is constituted.Base material film 1 can be tensionless winkler foundation film or the film through uniaxially or biaxially stretching.In addition it is also possible to will
The axial orientation angles control that the stretching ratio of stretched film or the crystallization of adjoint stretched film are formed specifically is being worth.
The thickness of base material film 1 used in the surface protection film 10 of the present invention, is not particularly limited, but for example preferred
12~100 μm or so of thickness, if 20~50 μm or so of thickness, then be easier to operate to, thus more preferably.
In addition, can be as needed, being set on the face of the opposite side in the face of the formation adhering agent layer 2 of base material film 1 prevents table
Stain-proofing layer, antistatic layer, hard conating of anti-scar of face dirt etc..In addition it is also possible to implement to utilize on the surface of base material film 1
The easily adhesion processing such as the surface that corona discharge is carried out is modified, coating Anchor Agent.
In addition, the adhering agent layer 2 used in the surface protection film 10 of the present invention, as long as it is fitted in the surface of adherend
On, it can be simply peeled away after being finished, and be difficult to pollute the sticker of adherend, then it is not particularly limited, if considering to be fitted in
Durability after on optical film etc., then glue usually using the acrylic compounds for being crosslinked (methyl) acrylate copolymer
Agent.
As (methyl) acrylate copolymer, it can include n-butyl acrylate, 2-ethyl hexyl acrylate, propylene
The main monomers such as the different monooctyl ester of acid, the different nonyl ester of acrylic acid, with acrylonitrile, vinylacetate, methyl methacrylate, ethyl acrylate etc.
Comonomer, acrylic acid, methacrylic acid, hydroxy-ethyl acrylate, hy-droxybutyl, GMA, N-
The functional monomers such as methylol methacrylamide, methoxy polyethylene glycol methacrylate-styrene polymer etc. containing polyoxy alkylidene
The copolymer of monomer copolymerization.(methyl) acrylate copolymer, its main monomer and other monomers can be (methyl)
Acrylate, can also be containing one or more in addition to (methyl) acrylate as the monomer outside main monomer
Monomer.Other monomers beyond main monomer, can be selected from but be not particularly limited to above-mentioned comonomer, functional monomer, contain
There is monomer of polyoxy alkylidene etc..
As the curing agent added in adhering agent layer 2, the crosslinking agent for being crosslinked (methyl) acrylate copolymer can be arranged
Enumerate isocyanate compound, epoxide, melamine compound, metal chelate compound etc..In addition, being used as thickening
Agent, can include rosin, coumarone-indene, terpenes, petroleum-type, phenols etc..
The thickness of adhering agent layer 2 used in the surface protection film 10 of the present invention, is not particularly limited, but preferably 5~
The thickness of 40 μm or so of thickness, more preferably 10~30 μm or so.Further, since when surface protection film is peeled off from adherend
Operability is excellent, so it is preferred that the peel strength (adhesion strength) to adherend surface of surface protection film is 0.03~0.3N/
25mm or so the adhering agent layer 2 with micro- adhesion strength.Further, since from surface protection film 10 peel off stripping film 5 when behaviour
The property made is excellent, therefore peeling force when preferably peeling off stripping film 5 from adhering agent layer 2 is below 0.2N/50mm, more preferably
Below 0.14N/50mm.
In addition, the stripping film 5 used in the surface protection film 10 of the present invention, is that stripping is laminated in the one side of resin film 3
Formed from oxidant layer 4, the peeling agent layer 4 contains the remover, not anti-with the remover using dimethyl silicone polymer as main component
The antistatic additive answered and at least ester plasticizer containing more than one ehter bond.Made in the surface protection film of the present invention
In stripping film, the antistatic additive composition is preferably that fusing point is the ionic compound less than 30 DEG C.
As resin film 3, polymer PET, PA membrane, polyethylene film, polypropylene screen, polyimide film etc. can be included, by
In with excellent transparent and cheap price, therefore particularly preferably polymer PET.Resin film can be tensionless winkler foundation film, can also
It is uniaxially or biaxially stretched film.Furthermore, it is possible to the axial direction formed by the stretching ratio of stretched film, with the crystallization of stretched film
Orientation angles control be specifically worth.
The thickness of resin film 3 is not particularly limited, but such as preferably 12~100 μm or so of thickness, if 16~50 μm
The thickness of left and right, then easily operation, so more preferably.
In addition, can be as needed, implement to be modified using the surface that corona discharge is carried out on the surface of resin film 3, be coated with
The easily adhesion processing such as Anchor Agent.
As the remover using dimethyl silicone polymer as main component for constituting peeling agent layer 4, addition can be included anti-
Answer silicone remover known to type, condensation reaction type, cationic polymerization type, radical polymerization mould assembly etc..Commercially sell
The product of addition reaction-type silicone remover, for example, can include KS-776A, KS-847T, KS-779H, KS-837, KS-
778th, KS-830 (SHIN-ETSU HANTOTAI's chemical industry (strain) manufacture), SRX-211, SRX-345, SRX-357, SD7333, SD7220,
SD7223, LTC-300B, LTC-350G, LTC-310 (Dow Corning Toray Co., Ltd. manufacture) etc..Commercially sell
The product for the condensation reaction type silicone remover sold, for example, can include SRX-290, SYLOFF-23 (Dow Corning
Toray Co., Ltd. manufacture) etc..The product for the cationic polymerization type silicone remover commercially sold, for example, can enumerate
Go out to have TPR-6501, TPR-6500, UV9300, VU9315, UV9430 (Momentive Performance Materials
Company is manufactured), X62-7622 (SHIN-ETSU HANTOTAI's chemical industry (strain) manufacture) etc..The radical polymerization mould assembly silicone commercially sold
The product of class remover has X62-7205 (SHIN-ETSU HANTOTAI's chemical industry (strain) manufacture) etc..
As the antistatic additive for constituting peeling agent layer 4, preferably with respect to the stripping using dimethyl silicone polymer as main component
From agent solution favorable dispersibility and will not hinder using dimethyl silicone polymer as the anti-quiet of the solidification of the remover of main component
Electric agent.In addition, in order to be transferred to the surface of adhering agent layer 2 from peeling agent layer 4, assign the antistatic effect of adhering agent layer 2, preferably not
With the antistatic additive of the remover reaction using dimethyl silicone polymer as main component.Fusing point is less than 30 DEG C of ionic compound
It is highly suitable as such antistatic additive.
It is less than 30 DEG C of ionic compound as fusing point, for the ionic compound with cation and anion, sun
Ion, can include the cyclic amidines such as imidazol ion ion, pyridinium ion, ammonium ion, sulfonium cation, phosphine ion etc..In addition, as cloudy
Ion, can include CnH2n+1COO-、CnF2n+1COO-、NO3 -、CnF2n+1SO3 -、(CnF2n+1SO2)2N-、(CnF2n+1SO2)3C-、
PO4 3-、AlCl4 -、Al2Cl7 -、ClO4 -、BF4 -、PF6 -、AsF6 -、SbF6 -Deng.
Antistatic additive is relative to the addition using dimethyl silicone polymer as the remover of main component, according to antistatic additive
Species or affinity between remover and it is different.The addition of antistatic additive, it is contemplated that surface is peeled off from adherend
The stripping electrostatic pressure expected during diaphragm, contaminative and adhesiveness of adherend etc. are set.
Constitute the ester plasticizer containing at least more than one ehter bond of peeling agent layer 4, the table for improving adhering agent layer 2
The antistatic property in face.As plasticizer contained in peeling agent layer 4, preferred pair is using dimethyl silicone polymer as main component
Stripper solution good dispersion plasticizer.Also, it is preferred that it will not hinder using dimethyl silicone polymer as main component
The plasticizer of the solidification of remover.In addition, plasticizer, which plays auxiliary, makes antistatic additive contained in peeling agent layer 4 from remover
Layer 4 is transferred to the effect on the surface of adhering agent layer 2.Therefore, plasticizer be preferably not with using dimethyl silicone polymer as main component
The material that is reacted of remover.It is suitably at least ester containing more than one ehter bond in molecule as such plasticizer
Class plasticizer.
The ehter bond of at least more than one in ester plasticizer, existing in the molecule, is to improve and antistatic additive
Between compatibility and need.In addition, in the surface protection film of the present invention, when peeling agent layer is in contact with adhering agent layer,
In order that antistatic additive composition is expeditiously transferred on the surface of adhering agent layer from peeling agent layer, plasticizer has been used.This hair
It is suitable to use the plasticizer containing ester group in order to improve the compatibility of peeling agent layer and adhering agent layer in bright.
As the ester plasticizer containing at least more than one ehter bond in molecule, such as -2- of diethylene glycol two can be included
Ethylhexoate, two -2 ethyl hexanoic acid of tetraethylene glycol ester, six two -2 ethyl hexanoic acid of ethylene glycol esters, triethylene glycol diethyl butyric acid
Ester, polyethylene glycol diethyl butyrate, polypropylene glycol ethylhexanoate, triethylene glycol dibenzoate, tetraethylene glycol hexichol
Formic acid esters, polyethylene glycol dibenzoate, dibenzonate or polyethylene glycol -2 ethyl hexanoic acid benzoic ether etc..
It can be selected from these ester plasticizer groups a kind of or mix two or more used.Here, ethylhexoate is also claimed
Make ethylhexoate (ethylhexanoate), ethylhexoate (ethylhexoate), ethylhexoate (ethyl hexane
Acid ester) etc..Benzoic ether (benzoate) then refers to benzoate.
Ester plasticizer is relative to the addition using dimethyl silicone polymer as the remover of main component, because of plasticizer
Species, the affinity between remover and it is different, but be contemplated that from adherend peel off surface protection film when desired stripping
Contaminative, adhesiveness from electrostatic pressure, to adherend etc. are set.
To the mixing between the remover and antistatic additive and ester plasticizer using dimethyl silicone polymer as main component
Method, without special restriction.Any one following method can be used：To the remover using dimethyl silicone polymer as main component
It is middle add and mix antistatic additive and ester plasticizer after, the method added and mix remover solidification catalyst；Use
After organic solvent beforehand dilution is using dimethyl silicone polymer as the remover of main component, adds and mix antistatic additive and ester
The method of class plasticizer and remover solidification catalyst；Remover using dimethyl silicone polymer as main component is advance
It is diluted in after organic solvent, adds and mixed catalyst, then adds and mix antistatic additive and the method for ester plasticizer etc..
In addition, as needed, the auxiliary of the adhesion such as silane coupler improver or the compound containing polyoxy alkylidene etc. can be added
Help the material of antistatic effect.
Using dimethyl silicone polymer as the remover of main component and antistatic additive and ester plasticizer mixed proportion simultaneously
Be not particularly limited, but relative to 100 parts of the solid constituent using dimethyl silicone polymer as the remover of main component, with solid into
The summation for dividing meter antistatic additive and ester plasticizer is preferably 5~100 parts or so of ratio.Relative to dimethyl silicone polymer
For 100 parts of the solid constituent of the remover of main component, if the summation of antistatic additive and ester plasticizer be converted into solid into
When the addition divided is less than 5 parts of ratio, then antistatic additive and ester plasticizer are reduced to the transfer amount on adhering agent layer surface, difficult
To play the anti-static function for assigning sticker.In addition, relative to using dimethyl silicone polymer as the remover of main component
100 parts of solid constituent, if the addition for being converted into solid constituent of the summation of antistatic additive and ester plasticizer is more than 100 parts
During ratio, then antistatic additive and ester plasticizer are also transferred simultaneously with the remover using dimethyl silicone polymer as main component
Onto the surface of adhering agent layer, it is thus possible to the adhesiveness of sticker can be reduced.
The method and laminating stripping film 5 of adhering agent layer 2 are formed on the base material film 1 of the surface protection film 10 of the present invention
Method, can be carried out, be not particularly limited by known method.Specifically, following methods can be included：(1) in base
The resin combination for forming adhering agent layer 2 is coated with the one side of material film 1, it is dried, is formed after adhering agent layer, laminating
The method of stripping film 5；(2) resin combination for forming adhering agent layer 2 is coated with the surface of stripping film 5 and it is done
It is dry, formed after adhering agent layer, method of base material film 1 etc. of fitting uses any of which method.
In addition, the method that adhering agent layer 2 is formed on the surface of base material film 1 can be known method.Specifically, may be used
With using known in reverse coating, scraper type coating, gravure coating, the coating of slit type extrusion pressing type, Meyer rod coating, airblade coating etc.
Coating method.
In addition, similarly, forming peeling agent layer 4 on resin film 3, carried out using known method.Specifically,
Coating method known to gravure coating, Meyer rod coating, airblade coating etc. can be used.
Surface protection film 10 of the invention with said structure, peels off sticker from the optical film as adherend
Surface potential during layer is preferably+0.7kV~-0.7kV.Further, surface potential is more preferably+0.5kV~-0.5kV, special
It is not preferably+0.1kV~-0.1kV.The surface potential can pass through the antistatic additive contained by adding and subtracting in peeling agent layer and esters
Species, addition of plasticizer etc. are adjusted.
The sectional view of states of the Fig. 2 for expression by stripping film from the surface protection film of the present invention after stripping.
By peeling off stripping film 5 on the surface protection film 10 shown in Fig. 1, make institute in the peeling agent layer 4 of stripping film 5
The sticker of surface protection film 10 is arrived in the part transfer (attachment) of the antistatic additive and ester plasticizer (reference 7) contained
The surface of layer 2.Therefore, in fig. 2, turn on the surface for the adhering agent layer 2 for peeling off the surface protection film 11 of the state of stripping film
The antistatic additive and ester plasticizer of print, are illustrated with the spot of reference 7.By make antistatic additive and ester plasticizer into
Points 7 are transferred to the surfaces of adhering agent layer 2 from stripping film 5, compared with the adhering agent layer 2 before transfer, by adhering agent layer 2 from being glued
Stripping electrostatic pressure reduction when being peeled off on thing.In addition, stripping electrostatic pressure when adhering agent layer is peeled off from adherend, Ke Yitong
Known method is crossed to be measured.For example, after surface protection film is fitted on the adherends such as polarizer, being peeled off using high speed
Testing machine (TESTER SANGYO CO .LTD. manufacture) peels off surface protection film with 40m per minute peeling rate, makes simultaneously
Determine the surface potential on adherend surface with every 10ms with surface potential meter (KEYENCE CORPORATION are manufactured), and by this
When surface potential absolute value maximum be used as peel off electrostatic pressure (kV).
In the surface protection film of the present invention, when by the surface protection film 11 of the state for peeling off stripping film shown in Fig. 2
When being fitted on adherend, the antistatic additive and ester plasticizer and the table of adherend being transferred on the surface of the adhering agent layer 2
Face is contacted.Thus, it is possible to stripping electrostatic pressure when lower suppressing again to peel off surface protection film from adherend.
Fig. 3 is the sectional view for the embodiment for representing the optical component of the present invention.
Stripping film 5 is peeled off from the surface protection film 10 of the present invention, to expose the state of adhering agent layer 2, via adhesion
Oxidant layer 2 is fitted on the optical component 8 as adherend.
That is, Fig. 3 represents a kind of optical component 20 of the surface protection film 11 for the present invention that fitted., can as optical component
Include polarizer, polarizer, eyeglass film, the polarizer for being also used as polarizer, the light such as polarizer for being also used as eyeglass film
Film.Above-mentioned optical component can be used as the liquid crystal display devices such as liquid crystal display panel, the optical system of various metrical instrument classes
The component parts of device etc..In addition, as optical component, can also include antireflection film, hard coat film, for touch panel
The optical films such as transparent and electrically conductive film.
According to the present invention optical component, using surface protection film 11 from the optical component (optical film) as adherend
When upper stripping is removed, fully relatively low it can suppress to peel off electrostatic pressure.Therefore, it is not required to worry and damages driving IC, TFT element, grid
The circuit blocks such as line drive circuit, can improve the production efficiency in the manufacturing processes such as liquid crystal display panel, keep production process
Reliability.
Embodiment
Next the present invention is further described according to embodiment.
(embodiment 1)
(making of surface protection film)
By the addition reaction-type silicone of 5 parts by weight, (Dow Corning Toray Co., Ltd.s manufacture, trade name：
SRX-345), 7.5 parts by weight are used as the fusing point to be double (the fluoroform sulphurs of three normal-butyl first ammoniums of 27.5 DEG C of ionic compound
Acyl) imines (3M companies manufacture, FC-4400) 10% the ethyl acetate solution, -2- ethyl hexyls of tetraethylene glycol two of 0.75 parts by weight
Acid esters, the toluene of 95 parts by weight and ethyl acetate are 1:Platinum catalyst (the Dow Corning of 1 mixed solvent, 0.05 parts by weight
Toray Co., Ltd.s manufacture, trade name：SRX-212) mix, be stirred mixing, prepare the stripping for forming embodiment 1
From the coating of oxidant layer.It is used for shape using Meyer rod coating on the surface for the polyethylene terephthalate film that thickness is 38 μm
Into the coating of the peeling agent layer of embodiment 1, it is 0.2 μm to make dried thickness, is carried out using 120 DEG C of heated air circulation type baking ovens
Dry 1 minute, obtain the stripping film of embodiment 1.On the other hand, relative to the 2-EHA by 90 parts by weight, 7 weights
Methoxy poly (ethylene glycol) (400) methacrylate, the copolymer of the acrylic acid 2- hydroxyl ethyl esters of 3 parts by weight of amount part are constituted
The parts by weight of 30% ethyl acetate solution 100 of sticker polymer, stir and mix the Isocyanates curing agent of 1.5 parts by weight
(TOSOH CORPORATION are manufactured, trade name：CORONATE (registration mark) HX), prepare the sticker combination of embodiment 1
Thing.In addition, CORONATE (registration mark) HX is the curing agent of HDI classes (hexamethylene diisocyanate class).
So that dried thickness is 20 μm on the surface for the polyethylene terephthalate film that thickness is 38 μm
After the adhesion agent composition of mode coating Examples 1, it is dried 2 minutes using 100 DEG C of heated-air circulation oven, forms adhesion
Oxidant layer.Afterwards, on the surface of the adhering agent layer, the embodiment 1 for above-mentioned preparation of being fitted via peeling agent layer (silicone-treated face)
Stripping film.The adhesive film of gained is incubated 5 days in the environment of 40 DEG C, solidifies adhering agent layer, obtains the surface of embodiment 1
Diaphragm.
(comparative example 1)
By the addition reaction-type silicone of 5 parts by weight, (Dow Corning Toray Co., Ltd.s manufacture, trade name：
SRX-345), the toluene and ethyl acetate of 95 parts by weight are 1:Platinum catalyst (the Dow of 1 mixed solvent, 0.05 parts by weight
Corning Toray Co., Ltd.s manufacture, trade name：SRX-212) mix, be stirred mixing, prepare for forming ratio
Compared with the coating of the peeling agent layer of example 1.On surface of the thickness for 38 μm of polyethylene terephthalate film, Meyer rod is used
The coating of peeling agent layer for forming comparative example 1 is coated with by dried thickness in the way of 0.2 μm, 120 DEG C are used
Heated-air circulation oven is dried 1 minute, obtains the stripping film of comparative example 1.On the other hand, relative to the implementation of 100 parts by weight
The sticker polymer solution (solid constituent is 30% ethyl acetate solution) of example 1, adds and mixes 3 parts by weight as fusing point
For double (trifluoro methylsulfonyl) imines of three normal-butyl first ammoniums of 27.5 DEG C of ionic compounds (3M companies manufacture, FC-4400)
Isocyanates curing agent (the TOSOH CORPORATION manufactures, trade name of 10% ethyl acetate solution, 1.5 parts by weight：
CORONATE (registration mark) HX), prepare the adhesion agent composition of comparative example 1.
On surface of the thickness for 38 μm of polyethylene terephthalate film, so that dried thickness is 20 μm
Mode is coated with after the adhesion agent composition of comparative example 1, is dried 2 minutes using 100 DEG C of heated-air circulation oven, forms adhesion
Oxidant layer.Afterwards, fitted on the surface of the adhering agent layer above-mentioned preparation comparative example 1 stripping film peeling agent layer (at silicone
Reason face).The adhesive film of gained is incubated 5 days in the environment of 40 DEG C, solidifies adhering agent layer, the surface for obtaining comparative example 1 is protected
Cuticula.
(comparative example 2)
Except the three normal-butyl first ammoniums double (three not added in adhering agent layer as fusing point for 27.5 DEG C of ionic compound
Fluorine methylsulfonyl) outside imines, in the same manner as comparative example 1, obtain the surface protection film of comparative example 2.
(comparative example 3)
In addition to tetraethylene glycol two -2 ethyl hexanoic acid ester as ester plasticizer is not added in peeling agent layer, with reality
Apply example 1 similarly, obtain the surface protection film of comparative example 3.
(embodiment 2)
Except the adhesion agent composition of alternate embodiment 1, the acrylic acid by 58 parts by weight relative to 100 parts by weight is used
The sticker that the copolymer of the acrylic acid 2- hydroxyl ethyl esters of 2- ethylhexyl esters, the butyl acrylate of 38 parts by weight and 4 parts by weight is constituted
30% ethyl acetate solution of polymer, adds and mixes the Isocyanates curing agent (TOSOH of 1.2 parts by weight
CORPORATION is manufactured, trade name：CORONATE (registration mark) HX) adhesion agent composition outside, with embodiment
1 similarly, obtains the surface protection film of embodiment 2.
(embodiment 3)
Except the adhesion agent composition of alternate embodiment 1, the acrylic acid by 96 parts by weight relative to 100 parts by weight is used
30% ethyl acetate of the sticker polymer that 2- ethylhexyl esters, the copolymer of the acrylic acid 2- hydroxyl ethyl esters of 4 parts by weight are constituted is molten
Liquid, adds and mixes Isocyanates curing agent (the TOSOH CORPORATION manufactures, trade name of 1.2 parts by weight：
CORONATE (registration mark) HX) adhesion be outside composition, similarly to Example 1, to obtain the surface of embodiment 3
Diaphragm.
The method and result of following presentation evaluation test.
<The assay method of the peeling force of stripping film>
It is width 50mm, long 150mm by the sample shear of surface protection film.Under 23 DEG C × 50%RH experimental enviroment, make
Intensity when peeling off stripping film was determined along 180 ° of direction with the peeling rate of 300mm/ minutes with cupping machine, and made with this
For the peeling force (N/50mm) of stripping film.
<The assay method of the adhesion strength of surface protection film>
The low reflection processing polarizer (AG-LR polarizers) of anti-dazzle is fitted in glass with double-sided adhesive tape using make-up machine
On the surface of glass plate.Then fit and be cut into after wide 25mm surface protection film on the surface of polarizer, 23 DEG C ×
Preserved one day under 50%RH experimental enviroment.Afterwards using cupping machine with the peeling rate of 300mm/ minutes, along 180 °
Direction determines intensity when peeling off surface protection film, and in this, as peeling force (N/25mm).
<The assay method of the stripping electrostatic pressure of surface protection film>
The low reflection processing polarizer (AG-LR polarizers) of anti-dazzle is fitted in glass with double-sided adhesive tape using make-up machine
On the surface of glass plate.Then fit and be cut into after wide 25mm surface protection film on the surface of polarizer, 23 DEG C ×
Preserved one day under 50%RH experimental enviroment.Afterwards using high speed electronic stripping tester (TESTER SANGYO CO .LTD. manufacture)
Surface protection film is peeled off with 40m per minute peeling rate, while using surface potential meter (KEYENCE CORPORATION systems
Make) determine the surface potential on the polarizer surface per 10ms, and using the maximum of the absolute value of surface potential now as
Peel off electrostatic pressure (kV).
<The determination method of the surface contamination of surface protection film>
The low reflection processing polarizer (AG-LR polarizers) of anti-dazzle is fitted in glass with double-sided adhesive tape using make-up machine
On the surface of glass plate.Then fit and be cut into after wide 25mm surface protection film on the surface of polarizer, 23 DEG C ×
Preserved 3 days and 30 days under 50%RH experimental enviroment.Surface protection film is peeled off afterwards, visually whether is deposited on observation polarizer surface
In pollution.As the criterion of surface contamination, the situation of pollution-free transfer on polarizer is evaluated as (zero), confirmed partially
The situation of the transfer for having pollution on piece of shaking is evaluated as (×).
On obtained embodiment 1~3 and the surface protection film of comparative example 1~3, its measurement result is as shown in table 1~2.
" 2EHA " is that 2-ethyl hexyl acrylate, " #400G " are that methoxy poly (ethylene glycol) (400) methacrylate, " HEA " are propylene
Sour 2- hydroxyl ethyl esters, " BA " are that butyl acrylate, " FC4400 " are three normal-butyl first ammoniums double (trifluoro methylsulfonyl) imines, " plasticizer "
For tetraethylene glycol two -2 ethyl hexanoic acid ester.In table 1,2, using the total amount of sticker polymer (solid constituent) as about 100 weight
Part mode, the composition of adhering agent layer is represented with parts by weight.Therefore, in the adhering agent layer of comparative example 1, sticker polymer (Gu
Body composition) with FC4400 part by weight it is 30 parts by weight：The parts by weight of 0.3 parts by weight=100：1.0 parts by weight.
[table 1]
[table 2]
Measurement result according to table 1 and table 2, can obtain drawing a conclusion.
The surface protection film of embodiments of the invention 1~3 has the adhesion strength of appropriateness, and adherend surface is not polluted,
And by surface protection film from adherend peel off when stripping electrostatic force down.
On the other hand, in adhering agent layer the comparative example 1 containing antistatic additive surface protection film, by surface protection film from
Stripping electrostatic when being peeled off on adherend is forced down, and well, but the pollution to adherend after stripping increases.
In addition, being free of antistatic additive in both the adhering agent layer of surface protection film and the peeling agent layer of stripping film
In the surface protection film of comparative example 2, the contaminative to adherend is good, but when surface protection film is peeled off from adherend
Electrostatic pressure is peeled off to increase.
That is, the surface protection film of the comparative example 1 containing antistatic additive and in table in the adhering agent layer of surface protection film
In the surface protection film for the comparative example 2 that antistatic additive is free of in the adhering agent layer of surface protective film and the peeling agent layer of stripping film,
It is difficult to take into account reduction stripping electrostatic pressure and the contaminative to adherend.
On the other hand, after in the peeling agent layer for make stripping film containing antistatic additive and ester plasticizer, only in adhesion
On the surface of oxidant layer transferred with peeling agent layer antistatic additive and ester plasticizer embodiment 1~3 surface protection film in, by
In by adding a small amount of ester plasticizer, just have stripping electrostatic pressure significantly reduces effect, therefore, without the dirt to adherend
Dye, antistripping antistatic property is also good.
In addition, antistatic additive is comprised only in peeling agent layer and without ester plasticizer comparative example 3 surface protection film
In, without the pollution to adherend, antistripping antistatic property is also good.If however, with peeling agent layer containing antistatic additive with
The surface protection film of the embodiment 1~3 of ester plasticizer is compared, then peels off electrostatic pressure and increase.
Industrial applicibility
The surface protection film of the present invention is in the optical film such as polarizer, polarizer, eyeglass film and other various light
In the production process of department of the Chinese Academy of Sciences's part, the surface of the optical component etc. can be fitted in protect surface.In addition, the surface of the present invention is protected
Cuticula electrostatic pressure amount produced when lower can suppress to peel off surface protection film from adherend, and antistripping electrostatic
The rheological parameters' change with time of performance and few to the pollution of adherend, can improve the yield rate of production process, exploitation value industrially
Value is big.
Claims (4)
1. a kind of surface protection film, it is viscous by being formed on a face of the base material film being made up of the resin with the transparency
Oxidant layer, and stripping film of the laminating with peeling agent layer is formed on the adhering agent layer, it is characterised in that
The stripping film is formed by folding peeling agent layer in a surface layer of resin film, wherein, the peeling agent layer contains with poly- two
Methylsiloxane is the remover of main component, the antistatic additive not reacted with the remover and contains at least more than one ether
The ester plasticizer of key,
The antistatic additive composition is the ionic compound that fusing point is less than 30 DEG C, and the antistatic additive composition increases with the esters
Modeling agent is transferred to the surface of the adhering agent layer from the peeling agent layer of the stripping film,
Stripping electrostatic pressure when reduction peels off the adhering agent layer from adherend.
2. surface protection film according to claim 1, it is characterised in that the adhering agent layer is by making containing (methyl) third
The adhesion agent composition crosslinking of olefin(e) acid ester copolymer and crosslinking agent is formed.
3. surface protection film according to claim 1 or 2, it is characterised in that by the stripping film from the adhering agent layer
Peeling force during upper stripping is below 0.2N/50mm.
4. a kind of optical component, it is formed by the surface protection film described in any one in claims 1 to 3 of fitting.
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| JP2016-027291 | 2016-02-16 | ||
| JP2016027291A JP6392798B2 (en) | 2016-02-16 | 2016-02-16 | Surface protective film and optical component on which it is bonded |
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| CN107083197B CN107083197B (en) | 2021-06-15 |
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| KR102119601B1 (en) * | 2018-09-12 | 2020-06-08 | 주식회사 폴리팀 | Masterbatch for manufacturing bio copolyester plastic or using antistatic-coating material |
| CN110452632A (en) * | 2019-09-24 | 2019-11-15 | 上海精珅新材料有限公司 | A kind of OLED display screen lower support film production method and products thereof |
| CN113292946A (en) * | 2021-06-15 | 2021-08-24 | 枣庄佳宏包装材料有限公司 | Cellulose biodegradable adhesive tape |
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| CN107083197B (en) | 2021-06-15 |
| TW201805157A (en) | 2018-02-16 |
| JP6392798B2 (en) | 2018-09-19 |
| TWI726923B (en) | 2021-05-11 |
| KR101927085B1 (en) | 2018-12-10 |
| KR20180067481A (en) | 2018-06-20 |
| KR20170096569A (en) | 2017-08-24 |
| JP2017144609A (en) | 2017-08-24 |
| KR101867850B1 (en) | 2018-06-15 |
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