CN103108533A - Electromagnetic wave shielding material for fpc - Google Patents
Electromagnetic wave shielding material for fpc Download PDFInfo
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- CN103108533A CN103108533A CN2012104553921A CN201210455392A CN103108533A CN 103108533 A CN103108533 A CN 103108533A CN 2012104553921 A CN2012104553921 A CN 2012104553921A CN 201210455392 A CN201210455392 A CN 201210455392A CN 103108533 A CN103108533 A CN 103108533A
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- Prior art keywords
- electromagnetic shielding
- fpc
- film
- shielding material
- conductive paste
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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
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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
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/281—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyimides
-
- 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
- B32B27/28—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42
- B32B27/285—Layered products comprising a layer of synthetic resin comprising synthetic resins not wholly covered by any one of the sub-groups B32B27/30 - B32B27/42 comprising polyethers
-
- 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
- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
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- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Electromagnetism (AREA)
- Engineering & Computer Science (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides an electromagnetic wave shielding material (10) for FPC, wherein the peeling phenomenon due to water vapor generated during the intense heating process is avoided. Meanwhile, the electromagnetic wave shielding material is in the form of a soft film and is excellent in electromagnetic wave shielding performance and bending property even after being subjected to severe bending treatment repeatedly. According to the technical scheme of the invention, one surface of a supporting film (6) is orderly laminated with a substrate (1) composed of a resin film coated with a dielectric medium, a film adhesive layer (2), a conductive paste layer (3) and a conductive adhesive layer (4). The water vapor transmission rate of the substrate is larger than 500g/m2 per day.
Description
Technical field
The present invention relates to a kind of FPC electromagnetic shielding material, it covers the flexible printed circuit substrate (Flexible Printed Circuits is hereinafter referred to as FPC) that repeatedly is subject to flexure operation, is used for electromagnetic wave shielding.
Background technology
In the Portable power handset devices such as mobile phone, for being dwindled, the overall dimension of casing controls with the carrying that is easy to carry about with one, and electronic unit is integrated on tellite.In addition, a plurality of by tellite is divided in order to dwindle the overall dimension of casing, and use has flexual FPC on the connection distribution between divided tellite, can fold tellite, and it is slided.
In addition, in recent years, cause e-machine to carry out malfunction for the impact of the electromagnetic interference that mutually receives between the electromagnetic interference that prevents from being subject to receiving from the outside or inner electronic unit, use electromagnetic shielding material to cover important electronic unit and FPC.
Since previous, as the electromagnetic shielding material that uses for the purpose of this kind electromagnetic shielding, use is provided with the material of bond layer on the surface of the metal forming of rolled copper foil, soft aluminium foil etc.Come overlay masking object (for example, with reference to patent documentation 1,2) by the electromagnetic shielding material that is consisted of by this metal forming.
Particularly, in order to cover important electronic unit to prevent electromagnetic wave, utilize metal forming or metallic plate to make the closed box shape and cover.In addition, to prevent electromagnetic wave, on the single face of metal forming, bond layer is set for the distribution that covers crooked FPC, fits by this bond layer.
In recent years, as the e-machine that carries at one's side, mobile phone is universal rapidly.Mobile phone is preferably, and can dwindle whole size when being accommodated in pocket etc. not using as far as possible, the size of integral body can be become large in use.Need to seek the improvement with mobile phone miniaturization/thinning and operability.As the method that solves these problems, employing is divided into two parts with mobile phone and folds the mode that opens and closes or slide the body structure of the mode of switching.
In addition, mobile phone being divided into during two parts fold the mode that opens and closes or slide any body structure of mode of switching, need to carry out continually the switching (operation that starts, stops) of operation screen.The switching number of times of operation screen carries out with the frequency of tens of times/days or hundreds of times/days.
That is to say, be used in the FPC of mobile phone and cover FPC that FPC carries out electromagnetic shielding and compare with existing portable e-machine with electromagnetic shielding material with the frequency more than very and repeatedly be subject to flexure operation.Therefore, the FPC that realizes the electromagnetic shielding effect of FPC is subject to harsh alternate stress with electromagnetic shielding material.In case be unable to bear this alternate stress, final, consist of FPC and can be subject to rupturing, peeling off equivalent damage with the shielding material of the base material of electromagnetic shielding material and metal forming etc.Its result worries that FPC descends or disappears with the electromagnetic shielding function of electromagnetic shielding material.
Therefore, also known being useful on dealt with the electromagnetic shielding material (for example, with reference to patent documentation 3) that is subject to this flexure operation repeatedly.
In addition, has after the FPC that carries out electromagnetic shielding by covering FPC covers with electromagnetic shielding material the situation of carrying out reflow soldering on the base material of the FPC of the electronic circuit component that is used for loading mobile phone.In the situation that have this heating process, due to heating tempestuously, produce residual solvent, degassed, steam etc. from consisting of FPC with the bond layer of the base material of electromagnetic shielding material, film, conductive paste layer, conductive adhesive layer etc.But because metal foil layer or base film layer become barrier layer for gases, therefore between this barrier layer for gases, due to the expansion of degassed grade, the power generation effect of peeling off has the problem of splitting.
Therefore, for discharging the degassed purpose that produces, motion is offered pin hole (for example, with reference to patent documentation 4,5) at metal film layer.
The prior art document
Patent documentation
Patent documentation 1: Japan opens clear 56-084221 communique in fact
Patent documentation 2: the JP 61-222299 of Japan communique
Patent documentation 3: the Unexamined Patent 7-122883 of Japan communique
Patent documentation 4: the JP 2010-239141 of Japan communique
Patent documentation 5: No. 4647924 communique of Japan's patent
Summary of the invention
(problem that invention will solve)
As above-mentioned patent documentation 1,2 disclosed, arrange on the surface of the metal formings such as rolled copper foil, soft aluminium foil in the electromagnetic shielding material of bond layer, in the situation that the number of times of flexure operation is few, the time that be used is shorter, the shielding properties fault-free.But, reach 5 years to 10 years, the number of times of flexure operation between in use and become in many situation, there is the problem of the durability deficiency of flexural property.This existing electromagnetic shielding material do not have the FPC that is used in nearest mobile phone necessary with electromagnetic shielding material, in the bend test more than 1,000,000 times qualified flexural property.
In addition, patent documentation 3 discloses a kind of electromagnetic shielding material, the metallic film of metal evaporation etc. is set, thereon stacked conductive adhesive on flexible membrane's single face.According to record, this electromagnetic shielding material can be covered in the wire type that is subject to alternating bending and use.Embodiment according to patent documentation 3, be on the single face of polyester film of 12 μ m, the coated film that thickness is the conductive coating paint that adds silver powder of 0.5 μ m to be set at thickness, arranging thereon and making the conductive adhesive heat drying and the thickness that are mixed with polyesters bonding agent and nickel by powder is the conductive adhesive layer of 30 μ m.In addition, according to record, carrying out 500,000 times will be along external diameter
The periphery of axle (mandrel) revert to the action of straight line after the angular bend of 180 ° and be the bend test of 1 circulation, result is not damage.
But, in nearest mobile phone, because the overall dimension with casing diminishes, with the thickness that 0.1mm unit cuts down casing, seek slim as much as possible.The FPC with bending property that can use on this slim casing needs outstanding bending property with electromagnetic shielding material.For example, even seeking to carry out will be along external diameter more than 1,000,000 times
The periphery of axle (mandrel) revert to the action of straight line after the angular bend of 180 ° and be the also not damage of bend test of 1 circulation.Compared with prior art, need a kind of FPC electromagnetic shielding material that can overcome the bend test of carrying out under exacting terms.
In addition, the electromagnetic shielding material put down in writing of the embodiment of patent documentation 3 is that on the resin film of 12 μ m, stacked thickness is that coated film and the thickness of the conductive coating paint of 0.5 μ m is the conductive adhesive layer of 30 μ m at thickness.The thickness of this electromagnetic shielding material integral body has surpassed 40 μ m.
As mentioned above, for the overall dimension attenuation as much as possible with the casing of mobile phone, so require FPC to be as thin as below 30 μ m with the integral thickness of electromagnetic shielding material.That is, compare with electromagnetic shielding material with FPC of the prior art, seek whole thickness thinner and stand the solid FPC electromagnetic shielding material of severeer bend test.
In addition, in order to allow bond layer with conductivity, being used in FPC need to suitable volume ground interpolation electroconductive powder (metal microparticle or carbon particulate) with the conductive adhesive of electromagnetic shielding material.But if make the interpolation quantitative change of electroconductive powder many, the bonding force of pressure-sensitive bond layer can descend so.
In addition, the FPC on mobile phone is with in electromagnetic shielding material etc., because repeatedly carry out flexure operation, so the bonding interface on each layer between base material and conductive paste layer and conductive paste layer and FPC partly is stripped from interlayer.Worry is at this local conductive paste layer fracture that is stripped from, and As time goes on the electromagnetic shielding performance can descend.
In addition, also to stand the bending operation that repeatedly carries out of e-machine length of life (for example bend test of 1,000,000 times) in order to make base material itself, so need outstanding flexural property.
In addition, the electromagnetic shielding material of putting down in writing in patent documentation 4 and 5 embodiment, stacked pin hole with aperture 1 μ m is offered into 100 ~ 150/cm
2Thickness be the rolled copper foil of 6 μ m as metal film layer, the FPC in mobile phone is with in electromagnetic shielding material etc., because repeatedly carry out bending operation, so worry that this metal film layer can rupture and shielding properties descends due to bending operation.
The object of the present invention is to provide a kind of FPC electromagnetic shielding material, it is in the situation that as thisly in reflow soldering heat after electromagnetic shielding material is covered in distributing board etc., can be because the moisture in the residual solvent of each layer or degassed, film is peeled off because heating tempestuously the steam that produces, for being rich in the slim of flexibility, even and repeatedly carry out harsh flexure operation electromagnetic shielding performance and also can not descend, flexural property is outstanding.
(technical scheme of technical solution problem)
In order to stand harsh flexure operation, that stands conductive paste burns till and covers the such heating process of reflow soldering after distributing board, uses the base material that is made of the higher heat-resistant resin film of moisture-vapor transmission in the present invention.Technological thought of the present invention is, in the present invention, is manufactured at least the duplexer that stacks gradually bond layer, conductive paste layer, conductive adhesive layer on the base material that is made of dielectric thin resin film.
In addition, in the present invention, the base material that is made of the heat-resistant resin film is considered flexibility and thermal endurance and is used applied dielectric thin resin film.Thus, the FPC that removed supporter film and stripping film can be as thin as below 25 μ m with the integral thickness of electromagnetic shielding material.
In addition, in the present invention, in order to increase the power of connecting airtight as the film resin film of the polyimide film of base material and conductive paste, between base material and conductive paste layer, bond layer is set.
Therefore, in order to address the above problem, the invention provides a kind of FPC electromagnetic shielding material, stack gradually the base material, the bond layer of film, conductive paste layer, the conductive adhesive layer that are made of applied dielectric thin resin film on the single face of supporter film, the moisture-vapor transmission of described base material is 500g/m
2More than it.
In addition, the polyimide film that described base material forms by using solvent-soluble polyimide consists of, and thickness is preferably 1 ~ 9 μ m.
In addition, described base material is made of polyimide film, and thickness is preferably 1 ~ 9 μ m.
In addition, the bond layer of described film is by making crosslinked formation of polyester resin constituent with epoxy radicals, and thickness is preferably 0.05 ~ 1 μ m.
In addition, described bond layer preferably further contains light absorbing material, and more than one of the black pigment of more than one of the group that free carbon black, graphite, nigrosine, cyanines are black by selecting, titanium is black for described light absorbing material, black iron oxide, chromium oxide, manganese oxide consist of or colored pigment consist of.
In addition, described conductive paste layer is, after coating contained the Nano silver grain of averaged particles footpath 1 ~ 120nm and conductive paste that the resin glue constituent forms, heating and being crimped on by the final thickness after convered structure was 0.1 ~ 2 μ m.
In addition, the specific insulation after the conductive paste of the described conductive paste layer of formation burns till is preferably 1.5 * 10
-5Below Ω cm.
In addition, the invention provides a kind of mobile phone, in this mobile phone, parts that above-mentioned FPC uses as electromagnetic shielding with electromagnetic shielding material and using.
In addition, the invention provides a kind of e-machine, in this e-machine, parts that above-mentioned FPC uses as electromagnetic shielding with electromagnetic shielding material and using.
(effect of invention)
Above-mentioned FPC of the present invention by using the thin resin film (thickness is 1 ~ 9 μ m) that is made of the polyimide film with high heat resistance, obtains standing the outstanding flexural property of harsh flexure operation with electromagnetic shielding material.
Thus, the FPC that removed supporter film and stripping film can be suppressed at below 25 μ m with the integral thickness of electromagnetic shielding material, can the thinning mobile phone and the integral thickness of e-machine.
In addition, the present invention can provide a kind of FPC electromagnetic shielding material, by using the base material that is consisted of by the higher thin resin film of moisture-vapor transmission, therefore in the heating process of the reflow soldering operation after covering the printed circuit wiring substrate etc., can be due to the moisture in the residual solvent of each layer or degassed, film because not heating tempestuously the steam that produces, and each interlayer produces and peels off.
In addition, by using the thin resin film (thickness is 1 ~ 9 μ m) and conductive paste layer that is consisted of by polyimide film, can suppress thickness, and, can access the electromagnetic wave shielding performance energy.
By mix black pigment or the light absorbing material that consists of of colored pigment by more than one in bond layer, the single face side of electromagnetic shielded film can be painted into specific color.
As mentioned above, according to the present invention, a kind of FPC electromagnetic shielding material can be provided, in the heating process of its reflow soldering operation after covering the printed circuit wiring substrate etc., can be due to the moisture in the residual solvent of bond layer or degassed, film because not heating tempestuously the steam that produces, and each interlayer generation is peeled off, is rich in flexibility, for slim, even and repeatedly carry out harsh flexure operation electromagnetic shielding performance and also can not descend, flexural property is outstanding.
Description of drawings
Fig. 1 shows the FPC that the present invention relates to general profile chart of one example of electromagnetic shielding material.
Fig. 2 is the general profile chart that shows the state that uses with removing supporter film and stripping film electromagnetic shielding material from the FPC of Fig. 1.
Symbol description
1 base material
2 bond layers
3 conductive paste layers
4 conductive adhesive layers
6 supporter films
7 stripping films
10,11 FPC electromagnetic shielding materials.
Embodiment
Below, suitable execution mode of the present invention is described.
FPC of the present invention is fitting in as by the FPC of convered structure etc. the time with electromagnetic shielding material, and outer surface is dielectric, the insulation film of need to not fitting on the electromagnetic shielding material outer surface at this FPC.In addition, FPC of the present invention makes whole thickness attenuation with electromagnetic shielding material, improves the bending property to flexure operation.
As shown in Figure 1, FPC of the present invention is flexual for having with the base material 1 of electromagnetic shielding material 10, thickness is the thin resin film of 1 ~ 9 μ m, and this thin resin film is by using moisture-vapor transmission to be 500g/m
2The solvent-soluble polyimide that it the is above and polyimide film that forms consists of.At the stacked supporter film 6 of the one side of base material 1, stack gradually to make at the another side of base material 1 and connect airtight the bond layer 2 that power improves, the conductive paste layer 3 that contains conductive particle between conductive paste layer 3 and base material 1.Further stack gradually conductive adhesive layer 4, stripping film 7 on conductive paste layer 3.This FPC can use with electromagnetic shielding material 11 as the FPC that has removed supporter film 6 and stripping film 7 with electromagnetic shielding material 10 as shown in Figure 2.
(polyimide film)
Become the thin resin film that the FPC that the present invention relates to consists of with the polyimide film that forms by using solvent-soluble polyimide of electromagnetic shielding material 10,11 base material 1, have high mechanical properties, thermal endurance, insulating properties, solvent resistance as the feature of polyimide resin, until it is also very stable to reach 260 ℃ of its chemical states of degree.
As polyimides, the Thermocurable polyimide that generates by the dehydration condensation that carries out of heating polyamic acid and the solvent-soluble polyimide that dissolves in the solvent of non-dehydrating condensation type are arranged.
The manufacture method of the polyimide film usually is, by make diamines (ジ ア ミ Application) and carboxylic diacid acid anhydride (カ Le ボ Application Suan Er No water thing) reaction in polar solvent, after synthetic polyamic acid as the imines precursor, polyamic acid is heated, perhaps by using catalyst to make its dehydration ring-type, obtain the method for corresponding polyimides.But the temperature of the heat treated in this imidization operation is preferably the temperature range of 200 ℃ ~ 300 ℃.In the situation that heating-up temperature is lower than this temperature, the possibility that can not carry out imidization is arranged, thus not preferred, in the situation that heating-up temperature is higher than said temperature, the danger of the thermal decomposition that produces compound is arranged, so also not preferred.
In order more to improve the pliability of base material, FPC of the present invention uses the electromagnetic shielding material used thickness less than the polyimide film as thin as a wafer of 10 μ m.
In the present invention, can use stacked thinner polyimide film on the single face of the supporter film 6 that uses as the reinforcing material on intensity and the base material that forms or do not use supporter film 6 and any in the base material that only consisted of by thinner polyimide film.
In the situation that the thickness of the polyimide film that uses is approximately thin than 7 μ m, is preferably stacked thinner polyimide film on as the single face of the supporter film 6 of the use of the reinforcing material on intensity and forms.
But, polyimide film itself is for having thermal endurance with 200 ℃ ~ 250 ℃ heat treated of carrying out of heating-up temperature, and supporter film 6 is owing to taking into account price and heat resisting temperature performance, use general heat-resistant resin film, for example polyethylene terephthalate (PET) resin film, therefore can not adopt of the prior art from form the method for polyimides as the polyamic acid of imines precursor.
Solvent-soluble polyimide is, the imidization of its polyimides finishes, and, dissolve in solvent.Therefore, coating by make solvent evaporates under less than the low temperature of 200 ℃, can be carried out film forming by after the coating fluid of dissolution with solvents.FPC of the present invention is the thin resin film of polyimides with the base material 1 that uses in electromagnetic shielding material, the thin resin film of this polyimides is after the coating fluid of the solvent-soluble polyimide of the non-dehydrating condensation type of coating on the single face of supporter film 6, make its drying with temperature less than the heating-up temperature of 200 ℃, use solvent-soluble polyimide and form.By as above operation, can stacked thickness be the polyimide film as thin as a wafer of 1 ~ 9 μ m on the single face of the supporter film 6 that is formed by general heat-resistant resin film.Can be on one side with supporter film 6 along its length direction conveyance, on one side form continuously base material 1, bond layer 2, conductive paste layer 3 etc. on this supporter film 6.Can produce FPC electromagnetic shielding material of the present invention by the production method of volume to volume (roll to roll).
The solvent-soluble polyimide of the non-dehydrating condensation type that uses in the present invention is not particularly limited, and can use the coating fluid of the common solvent-soluble polyimide of selling.The coating fluid of the common solvent-soluble polyimide of selling, specifically can enumerate ソ ル ピ ー 6,6-PI(ソ ル ピ ー industry), Q-IP-0895D(ピ ー ア イ skill grinds), PIQ(Hitachi changes into industry), SPI-200N(Nippon Steel chemistry), リ カ コ ー ト SN-20, the new Japanese physics and chemistry of リ カ コ ー ト PN-20() etc.The method that the coating fluid of solvent-soluble polyimide is coated on supporter film 6 is not particularly limited, and for example, can be coated with by the coating machine of metal mold coating machine, scraper type coating machine, lip formula coating machine etc.
The thickness of the polyimide film that uses in the present invention is preferably 1 ~ 9 μ m.If the thickness of polyimide film is made less than 0.8 μ m, so due to the mechanicalness intensity of the film that is made into a little less than, thereby be difficult technically.In addition, if the thickness of polyimide film surpasses 10 μ m, that just can not obtain having the FPC electromagnetic shielding material 11 of outstanding bending property.
In addition, in the situation that the thickness of the polyimide film that uses is approximately thin than 7 μ m, tension adjustment owing to being wound around rolling is more difficult, therefore is preferably stacked thinner polyimide film on the single face of the supporter film 6 that uses as the reinforcing material on intensity and forms.
The thickness of the base material that only is made of thinner polyimide film in the situation that use supporter film 6 is preferably about 7 ~ 9 μ m.
The moisture-vapor transmission of the polyimide film that uses in the present invention in addition, is preferably 500g/m
2More than it.At moisture-vapor transmission lower than 500g/m
2In it situation, in the such heating process of the reflow soldering after covering FPC, due to from the moisture in degassed, the film of the residual solvent of each layer and bonding agent because heating tempestuously the steam that produces, the possibility that exists each interlayer to peel off.Moisture-vapor transmission does not arrange higher limit especially.As long as use same material on base material, because moisture-vapor transmission and thickness are inversely proportional, so in the situation that the thickness of thinning base material and improve moisture-vapor transmission, the thickness that is preferably above-mentioned base material is the scope of 1 ~ 9 μ m.
(supporter film)
The polyolefin film of the base material of the supporter film 6 that uses in the present invention such as the polyester film that can enumerate PETG, polybutylene terephthalate (PBT), PEN etc., polypropylene and polyethylene etc.
The base material of supporter film 6 is such as PETG etc., when base material has to a certain degree fissility, can not implement lift-off processing on supporter film 6, but the stacked base material 1 that is formed by applied dielectric thin resin film directly.In addition, also can implement on the surface of supporter film 6 purpose and be the lift-off processing that is easy to peel off.
In addition, as the base film that above-mentioned supporter film 6 uses, when not having fissility, after the remover of coating amino-alkyd resin or polysilicone etc., implement lift-off processing by heat drying.Because FPC of the present invention is fitted in FPC with electromagnetic shielding material 10,11, so wish not use in this remover polysilicone.Reason is, if polysilicone is used as remover, have so on the surface of the base material 1 on the surface of contact supporter film 6, the part of polysilicone is moved, further use the inside of electromagnetic shielding material 11 by FPC, the danger of moving to conductivity bond layer 4 from base material 1.Have the lip-deep polysilicone that moves to this conductive adhesive layer 4 and weaken the danger of the bonding force of conductive adhesive layer 4.Be used in the thickness of supporter film 6 of the present invention, because remove the thickness of FPC with the integral body of electromagnetic shielding material 11 when being pasted on FPC and using, so be not particularly limited, be generally the thickness of 12 ~ 150 μ m degree.
(bond layer)
To be used in FPC of the present invention with electromagnetic shielding material 10,11 bond layer 2, to be set up in order improving as the film that is consisted of by polyimide film of base material 1 and the connecting airtight power of conductive paste layer 3.
For bond layer 2, because the firing temperature of stacked conductive paste layer 3 thereon is 150 ~ 250 ℃, so need to use the outstanding bonding agent of thermal endurance.In addition, bond layer 2 need to have for the polyimide film that becomes base material 1 and the outstanding bonding force of conductive paste layer 3.
Adhesive resin constituent as being used for bond layer 2 preferably uses the thermoplastic resins such as mylar, polyurethane resin, (methyl) acrylic resin, polyvinyl resin, polystyrene resin, polyamide.Can be also the thermosetting resins such as epoxy resin, amino resins, polyimide resin, (methyl) acrylic resin in addition.
As the adhesive resin constituent of bond layer 2, be particularly preferably and make the crosslinked adhesive resin constituent of polyester resin constituent with epoxy radicals, or epoxy resin is mixed in the resinoid adhesive resin constituent of polyurethane as curing agent.Therefore, bond layer 2 has hard physical property than the base material 1 that the film by polyimides consists of.Polyester resin constituent with epoxy radicals is not specially limited, and obtains such as the reaction of the polybasic carboxylic acid that has the carboxyl more than 2 in epoxy resin (its unhardened resin) that can be by having the epoxy radicals more than 2 in 1 molecule and 1 molecule etc.Polyester resin constituent crosslinked with epoxy radicals uses the crosslinking agent with the used for epoxy resin of epoxy reaction to carry out.
In addition, bond layer 2 can comprise light absorbing material, and black pigment or the coloring pigment of more than one of the group that free carbon black, graphite, nigrosine, cyanines black (シ ア ニ Application Block ラ ッ Network), titanium are black by selecting for this light absorbing material, black iron oxide, chromium oxide, manganese oxide consist of consist of.
Preferably sneak into the black pigment of carbon black etc. in bond layer 2.The light absorbing material that is made of black pigment or coloring pigment is preferably contained with 0.1 ~ 30 % by weight in bond layer 2.The average grain diameter of the primary particle that black pigment or coloring pigment are preferably observed according to SEM is 0.02 ~ 0.1 μ m degree.
In addition, as black pigment, have silicon dioxide granule etc. is immersed in the dyestuff of black only to make skin section become the situation of black, perhaps the pigmentary resin from black forms, and integral body becomes the situation of black.In addition, black pigment is except the situation of black, also comprise grey, partially black dark brown (?っ ぽ い dark brown) or partially black green (?っ ぽ い Green look) etc. be the particle of the color of approximate black, as long as just can use for being difficult for catoptrical dead color.
The thickness of adhesive linkage 2 is preferably 0.05 ~ 1 μ m degree, if the film thickness of this degree, what just can access conductive paste layer 3 connects airtight power fully.In the situation that the thickness of bond layer 2 is below 0.05 μ m, exist the particulate of light absorbing material to expose, base material 1 and conductive paste layer 3 connect airtight the danger that power descends, in addition, even the thickness of bond layer 2 has surpassed 1 μ m, there is no effect for the increase of the bonding force of the base material 1 that is consisted of by polyimide film or conductive paste layer 3.Therefore, if the thickness of bond layer 2 surpasses 1 μ m, manufacturing cost increases, so not preferred.
(conductive paste layer)
Being used for conductive paste layer 3 of the present invention uses conductive filler is sneaked into conductive paste as the resin combination of binding agent (binder).
As conductive paste, preferably comprise select in the conductive filler group that free conductive metal particulate, carbon nano-tube, carbon nano-fiber consist of more than one and the resin glue constituent.As the conductive metal particulate, can use the metal fine powder end of copper, silver, nickel, aluminium etc., use preferably that electric conductivity is high, micropowder or the nano particle of low-cost copper or silver.In addition, also can use as carbon nano-tube, carbon nano-fiber with carbon nano-particles of conductivity.
Wish that the specific insulation after conductive paste layer 3 burns till is 1.5 * 10
-5Below Ω cm.In addition, wish that surface resistivity after conductive paste layer 3 burns till is 0.2 Ω/below.
Be suppressed at the low temperature of the temperature range of 150 ~ 250 ℃ for the firing temperature with conductive paste, the averaged particles footpath of metal microparticle is preferably the scope of 1 ~ 120nm, the more preferably scope of 1 ~ 100nm.
The FPC that the present invention relates to is with electromagnetic shielding material 10,11 conductive paste layer 3, by containing this metal microparticle, not only can corresponding filming, and occur hot stickyly between particulate, also can realize the raising of conductance simultaneously.The conductive paste that the present invention uses is preferably, and is that the metal microparticle of the scope of 1 ~ 120nm is evenly dispersed in dispersion solvent in order to make averaged particles footpath for example, covers this metal particle sub-surface by molecule organic layer, and the dispersive property in solvent is improved.Finally, in the heating firing process of conductive paste, make metal microparticle Surface Contact each other, can access the conductivity of conductive paste layer 3.
The heating of conductive paste is burnt till and is preferably firing temperature in the boiling spread of molecule organic layer, and reason is, for example makes the molecule organic layer on covering metal atomic surface break away from, evapotranspire and remove by heating at the temperature of 150 ~ 250 ℃ of degree.
As mentioned above, the polyimide film that becomes base material 1 has for being the thermal endurance of the heat treated under 200 ℃ ~ 250 ℃ in heating-up temperature.But, in the situation that use supporter film 6, consider the thermal endurance of supporter film 6, being preferably the firing temperature that makes as much as possible conductive paste is low temperature.
The firing temperature of conductive paste is preferably 150 ~ 180 ℃.Firing temperature by making conductive paste in this temperature range, thereby can suppress because heat makes the deteriorated problem that causes bad order of supporter film 6.
In conductive paste, as mix the resin glue constituent that uses with conductive filler, preferably use the thermoplastic resins such as mylar, (methyl) acrylic resin, polyvinyl resin, polystyrene resin, polyamide.In addition, also can use the thermosetting resins such as epoxy resin, amino resins, polyimide resin, (methyl) acrylic resin.
Conductive paste sneak into the conductive filler of conductive metal particulate, carbon nano-tube, carbon nano-fiber etc. in these resin glue constituents after, adds the organic solvent of ethanol or ether etc. as required, carries out the adjustment of viscosity.In addition, the adjustment of the viscosity of conductive paste is carried out according to the increase and decrease of the addition (mix proportion) of organic solvent.
Burn till conductive paste layer 3 thickness afterwards and be preferably 0.1 ~ 2 μ m degree, be more preferably the thickness of 0.3 ~ 1 μ m degree.If the Thickness Ratio 0.1 μ m that burns till after conductive paste layer 3 is thin, obtain high electromagnetic wave shielding performance difficulty.On the other hand, if the Thickness Ratio 2 μ m that burn till after conductive paste layer 3 are thick, can not with the FPC that removes supporter film 6 and stripping film 7 with the THICKNESS CONTROL of the integral body of electromagnetic shielding material 11 below 25 μ m.
(conductive adhesive layer)
Use in electromagnetic shielding material 10,11 at the FPC that the present invention relates to, be laminated in conductive adhesive on conductive paste layer 3 and use acrylic-based adhesives, polyurethanes bonding agent, epoxies bonding agent, rubber-like bonding agent, silicone bonding agent etc. to sneak into the ionic compound of the particulate of conductivity or quaternary ammonium salt etc., electroconductive polymer etc. in normally used heat-curable adhesive, be not particularly limited.
Conductive adhesive does not use the bonding agent that shows at normal temperatures the pressure-sensitive cementability.Conductive adhesive of the present invention is when pressurizeing the bonding agent that gets, because be difficult to descend for crooked bonding force repeatedly, so preferred by heating.
Coordinate the particulate of the conductivity of conductive adhesive layer 4 to be not particularly limited, can be suitable for the particulate of conductivity commonly known in the art.For example, can enumerate metal microparticle that the metal by carbon black and silver, nickel, copper, aluminium etc. consists of and at the composition metal particulate of other metals of surface coverage of these metal microparticles.Suitable these conductivity of choice for use atomic one or more.
In addition, in above-mentioned conductive adhesive layer 4, if in order to obtain outstanding conductivity, for the mutual contact of the particulate of conductivity and this particle and conductive paste layer and as better by contacting between the FPC of convered structure, and contain the volume conductive material, bonding force descends.On the other hand, if lower the amount of conductive particle in order to improve bonding force, conductive particle and conductive paste layer can appear and as insufficient, the conductivity of being become by the contact between the FPC of the convered structure this opposite problem that descends.Therefore, the use level of conductive particle is generally 0.5 ~ 50 weight portion degree, more preferably 2 ~ 10 weight portions with respect to bonding agent (solid) 100 weight portions.
In addition, as the conductive adhesive that consists of conductive adhesive layer 4 of the present invention, preferably contain the anisotropic conductive adhesive of conductive particle, can use known material.As this anisotropic conductive adhesive, can use as with the thermosetting resin of the insulating properties of epoxy resin etc. as principal component, be dispersed with the bonding agent of conductive particle.
In addition, as the conductive particle that is used in anisotropic conductive adhesive, such as the monomer of the metal microparticle that can make up gold, silver, zinc, tin, scolding tin etc. or more than 2 kinds.In addition, as conductive particle, can use by the resin particle of metal plating.The shape of conductive particle preferably has the shape that fine particle connects into the straight chain shape, perhaps the aciculiform shape.If this shape, when by welded part, FPC being heated pressurized treatments, the conductor wirings that can enter FPC at the low lower conductive particle of exerting pressure.
The contact resistance value of anisotropic conductive adhesive and FPC is preferably 5 Ω/below cm.
The bonding force of conductive adhesive is not particularly limited, and its assay method is as the criterion with the test method of record in JIS Z 0237.For being peeled off (ピ ー Le by the bonding force on convered structure surface at peel angle 180 degree), under the peeling rate 300mm/ condition of dividing, be suitably the scope of 5 ~ 30N/ inch.During less than the 5N/ inch, for example, the electromagnetic shielding material that fits in FPC can peel off from FPC, produces floating section at bonding force.
FPC is heated the bonding condition of pressurization be not particularly limited, preference such as temperature are that 160 ℃, plus-pressure are 2.54MPa, hot pressing 30 minutes.
(stripping film)
As the base material of stripping film 7, such as the polyolefin film of the polyester film that can enumerate PETG, polybutylene terephthalate (PBT), PEN etc., polypropylene or polyethylene etc.After the remover of amino-alkyd resin or polysilicone etc. is coated these base films, implement lift-off processing by heat drying.FPC of the present invention is with electromagnetic shielding material 10,11, owing to fitting in FPC, so wish not use polysilicone in this remover.Reason is, if polysilicone is used as remover, have so on the surface of conductive adhesive layer 4 on the surface of contact stripping film 7, the part of polysilicone is moved, further use the inside of electromagnetic shielding material 11 by FPC, 1 danger of moving from conductive adhesive layer 4 to base material.In addition, has the possibility that the lip-deep polysilicone that moves to this conductive adhesive layer 4 weakens the bonding force of conductive adhesive layer 4.The thickness that is used in stripping film 7 of the present invention so be not particularly limited, is generally the thickness of 12 ~ 150 μ m degree owing to being to remove the thickness of FPC with the integral body of electromagnetic shielding material 11 when fitting in FPC and use.
FPC of the present invention can fit in electromagnetic shielding material 10,11 FPC that repeatedly is subject to flexure operation and use, and suitablely uses with electromagnetic shielding material as the outstanding FPC of bending property.In addition, the parts used as electromagnetic shielding with electromagnetic shielding material of FPC of the present invention can be used in mobile phone or e-machine.
Embodiment
Below, illustrate the present invention according to embodiment.
(embodiment 1)
Be that (Co., Ltd.'s system, article number spin in Japan: E5100) use as supporter film 6 for PETG (PET) film of 50 μ m with thickness.Moisture-vapor transmission on the single face of this supporter film 6 during with thickness 33 μ m is 180g/m
2The coating fluid of it solvent-soluble polyimide carries out the curtain coating coating in the mode that dried thickness becomes 4 μ m, makes its drying, the stacked base material 1 that is made of dielectric thin resin film.On the base material 1 that is formed, use is used to form the coating of bond layer 2, so that the mode that dried thickness is 0.3 μ m is coated with, lamination adhesive layer 2, described coating will be for mixing as the carbon black of the black pigment of light absorbing material and the polyester resin constituent that heat resisting temperature is 260 ~ 280 ℃.On bond layer 2, as conductive filler, the conductive paste that uses silver particles hybrid modulation that averaged particles footpath is about 50nm to become after the mode that becomes 0.3 μ m with dried thickness is coated with, burns till and forms conductive paste layer 3 with 150 ℃ of temperature.On conductive paste 3, thereby the conductive adhesive of epoxies thermosetting resin is coated with formation conductive adhesive layer 4 in the mode that dried thickness becomes 12 ~ 18 μ m, obtains the FPC electromagnetic shielding material of embodiment 1.The value of the specific insulation of the conductive paste layer 3 after mensuration is burnt till is 1.5 * 10
-5Below Ω cm.
(embodiment 2)
Except the coating fluid with solvent-soluble polyimide carries out the curtain coating coating in the mode that dried thickness becomes 6 μ m, make its drying, beyond the stacked base material 1 that is consisted of by dielectric thin resin film, the same manner as in Example 1, obtain the electromagnetic shielding material of embodiment 2.
(embodiment 3)
Except the coating fluid with solvent-soluble polyimide carries out the curtain coating coating in the mode that dried thickness becomes 8 μ m, make its drying, beyond the stacked base material 1 that is consisted of by dielectric thin resin film, the same manner as in Example 1, obtain the electromagnetic shielding material of embodiment 3.
(comparative example 1)
The polyimide film that the Thermocurable polyimide that use is 10 μ m by thickness except not using supporter film 6 consists of is as base material 1, and is the same manner as in Example 1, obtains the FPC electromagnetic shielding material of comparative example 1.
(comparative example 2)
Except the coating fluid with solvent-soluble polyimide carries out the curtain coating coating in the mode that dried thickness becomes 18 μ m, make its drying, beyond the stacked base material 1 that is consisted of by dielectric thin resin film, the same manner as in Example 1, obtain the electromagnetic shielding material of comparative example 2.
(comparative example 3)
Except the coating fluid with solvent-soluble polyimide carries out the curtain coating coating in the mode that dried thickness becomes 24 μ m, make its drying, beyond the stacked base material 1 that is consisted of by dielectric thin resin film, the same manner as in Example 1, obtain the electromagnetic shielding material of comparative example 3.
(the moisture-vapor transmission assay method of base material)
Be that (Co., Ltd.'s system, article number spin in Japan: E5100) use as supporter film 6 for PETG (PET) film of 50 μ m with thickness.Coating fluid with solvent-soluble polyimide on the single face of this supporter film 6 carries out the curtain coating coating in the mode that dried thickness becomes 33 μ m, makes its drying, the stacked base material 1 that is made of dielectric thin resin film.
Peel off the base material 1 that is consisted of by thin resin film from supporter film 6, through measuring according to JIS-K-7129B method " according to the method for trying to achieve of the moisture-vapor transmission of infrared ray sensor method ", be 180g/m
2My god.The thickness of known moisture-vapor transmission and determination object is inversely proportional, embodiment 1,2,3 and the moisture-vapor transmission of comparative example 2,3 solvent-soluble polyimide be that the result during with thickness 33 μ m is the basis, tries to achieve by calculating.
Comparative example 1 has been measured the moisture-vapor transmission of the polyimide film that use as base material 1, that Thermocurable polyimide that be 10 μ m by thickness consists of fully by above-mentioned assay method.
(assay method of the surface resistivity of conductive paste layer 3)
According to the regulation that JIS-K-7194 " utilizes the resistivity test method of the four probe method of Markite ", measure the surface resistivity of conductive paste layer 3 by the resistrivity meter (ロ レ ス タ-GP T600 type) of Mitsubishi Chemical's (strain) manufacturing.
(assay method of bend test)
use epoxies heat-curable adhesive (ス リ ー ボ Application De system, article number: 33A-798), the mode that becomes 12 μ m with dried thickness is adjusted, it is coated on conductive paste layer 3, to be coated with heat-curable adhesive (ス リ ー ボ Application De system, article number: conductive paste layer 3 33A-798) overlaps on the flexible printed circuit substrate that is provided with specimen, and make itself and FPC with conductive adhesive layer 4 side of electromagnetic shielding material relative to, at 160 ℃, 2.54MPa lower hot pressing is after 30 minutes, size severing according to wide 12.7mm * long 160mm obtains test film.
According to IPC specification TM-650 " TEST METHODS MANUAL " (reference 3 " resistance to bend(ing) " of JIS-C-6471), use the test film of severing to carry out the IPC bend test under the imposing a condition of R=1.5mm or R=1.0mm, the resistance value of instrumentation conductive paste layer by the flexure operation repeatedly of conductive layer the resistance value during with the initial stage compare the number of times of the bend test when increasing to 2 times, estimate bending property.
Being judged to be of bend test result, according to bend test, the number of times that the resistance value during with the initial stage is compared the bend test when increasing to 2 times due to the flexure operation repeatedly of conductive layer with the resistance value of conductive paste layer surpasses that the situation of 300,000 times is considered as qualified (zero), the situation below 300,000 times is considered as defective (*).
(assay method of flexibility test)
Use the sample (wide 17mm * long 160mm) that is used for bend test, make the ring rigidity testing machine (ル ー プ ス テ ィ Off ネ ス テ ス タ of manufacturing in (strain) Japan essence mechanism) the upper sample of installing begins to measure, with the sample looped-shaped bending, the load when rolling according to the diametric(al) along this ring is estimated the power of elasticity (コ シ).Particularly, make the ring of periphery 80mm in the mode that will become for the outside of the sample looped-shaped bending of bend test electromagnetic shielding material, begin to apply power with the speed of 3.3mm/ second from the upside of ring, until the distance of the minor axis of sample portion becomes 1.5mm, be determined at the stress of the sample when keeping 5 seconds under this state.
(outward appearance of the electromagnetic shielding material after heat resistant test and heat resistant test)
Make FPC relative to coincidence with polyimide film (East レ デ ュ Port Application System カ プ ト Application 200H) with the conductive adhesive of electromagnetic shielding material, hot pressing is 60 minutes under 160 ℃, 4.5MPa.Test film is cut into 2.5cm * 10cm, and immersion pulled after 10 seconds in the solder furnace of 290 ℃.
The outward appearance of the electromagnetic shielding material after the range estimation heat resistant test observes whether existing distortion and shortening etc. abnormal, and N/R good situations is considered as qualified (zero), situation about noting abnormalities is considered as defective (*).
(result of the test)
About embodiment 1 ~ 3 and comparative example 1 ~ 3, carry out surface resistivity, bend test and the flexibility test of conductive paste layer according to above-mentioned test method, table 1 illustrates the result of the test that obtains.
(table 1)
According to the result after the heat resistant test shown in table 1 as can be known, the moisture-vapor transmission of base material 1 is relevant to outward appearance after heat resistant test.That is, if the enough height of the moisture-vapor transmission of base material 1, so could be owing to producing gasification and cause and peeling off of interlayer can access good outward appearance because heating tempestuously from the moisture in degassed, the film of the residual solvent of each layer, bonding agent.
The thickness of the base material that the polyimide film that the FPC that from these result of the tests as can be known, has outstanding thermal endurance and a bending property needs to form by using solvent-soluble polyimide with electromagnetic shielding material consists of forms the film of 1 ~ 9 μ m.But as the thickness of the polyimide film that is made of Thermocurable polyimide of selling in Japan now, 7.5 μ m are the thickness of thin slab product.With in electromagnetic shielding material, need to use the polyimide film than this thin thickness at FPC of the present invention in base material.Therefore, be only the polyimide film of 1 ~ 9 μ m by use the thickness that obtains by the coating fluid than unfertile land curtain coating coating solvent soluble polyimide in base material, just can access the FPC electromagnetic shielding material of outstanding bending property.
FPC of the present invention can be used in as the electromagnetic shielding parts the various e-machines such as mobile phone, notebook computer, carried terminal with electromagnetic shielding material.
Claims (9)
1. FPC electromagnetic shielding material, stack gradually the base material, the bond layer of film, conductive paste layer, the conductive adhesive layer that are made of applied dielectric thin resin film on the single face of supporter film, the moisture-vapor transmission of described base material is 500g/m
2More than it.
2. FPC electromagnetic shielding material according to claim 1, the polyimide film that described base material forms by using solvent-soluble polyimide consists of, and thickness is 1 ~ 9 μ m.
3. FPC electromagnetic shielding material according to claim 1 and 2, described base material is made of polyimide film, and thickness is 1 ~ 9 μ m.
4. FPC electromagnetic shielding material according to claim 1 and 2, the bond layer of described film is by making crosslinked formation of polyester resin constituent with epoxy radicals, and thickness is 0.05 ~ 1 μ m.
5. FPC electromagnetic shielding material according to claim 1 and 2, described bond layer further contains light absorbing material, and more than one of the black pigment of more than one of the group that free carbon black, graphite, nigrosine, cyanines are black by selecting, titanium is black for described light absorbing material, black iron oxide, chromium oxide, manganese oxide consist of or colored pigment consist of.
6. FPC electromagnetic shielding material according to claim 1 and 2, described conductive paste layer is, after coating contained the Nano silver grain of averaged particles footpath 1 ~ 120nm and conductive paste that the resin glue constituent forms, heating and being crimped on by the final thickness after convered structure was 0.1 ~ 2 μ m.
7. FPC electromagnetic shielding material according to claim 1 and 2, the specific insulation after the conductive paste that consists of described conductive paste layer burns till is 1.5 * 10
-5Below Ω cm.
8. mobile phone, the parts that the described FPC of claim 1 or 2 is used as electromagnetic shielding with electromagnetic shielding material use.
9. e-machine, the parts that the described FPC of claim 1 or 2 is used as electromagnetic shielding with electromagnetic shielding material use.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011248736A JP5726048B2 (en) | 2011-11-14 | 2011-11-14 | Electromagnetic wave shielding material for FPC |
| JP2011-248736 | 2011-11-14 |
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| Publication Number | Publication Date |
|---|---|
| CN103108533A true CN103108533A (en) | 2013-05-15 |
| CN103108533B CN103108533B (en) | 2015-09-16 |
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| CN201210455392.1A Active CN103108533B (en) | 2011-11-14 | 2012-11-13 | FPC electromagnetic shielding material |
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| JP (1) | JP5726048B2 (en) |
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Also Published As
| Publication number | Publication date |
|---|---|
| KR20130054144A (en) | 2013-05-24 |
| JP2013105888A (en) | 2013-05-30 |
| CN103108533B (en) | 2015-09-16 |
| JP5726048B2 (en) | 2015-05-27 |
| KR101359474B1 (en) | 2014-02-06 |
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