CN107615408A - The manufacture method and conducting film of conducting film - Google Patents
The manufacture method and conducting film of conducting film Download PDFInfo
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- CN107615408A CN107615408A CN201680030108.2A CN201680030108A CN107615408A CN 107615408 A CN107615408 A CN 107615408A CN 201680030108 A CN201680030108 A CN 201680030108A CN 107615408 A CN107615408 A CN 107615408A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
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Abstract
The problem of the present invention is the manufacture method and conducting film for providing the conducting film high with the adaptation, environmental resistance and marresistance of substrate.Comprise the steps：The 1st resin bed (S1) is formed on substrate using the 1st resin combination comprising the 1st functional group, it is not absorbed in conductive material to the degree of the inside of layer and the 1st resin bed is dried into (S2), then there is the conductive pattern (S3, S4) of opening portion when being formed and being overlooked on the 1st resin bed, using comprising can with the 2nd resin combination of the 2nd functional group of the 1st functional group's co-curing of above-mentioned 1st resin bed by be coated to conductive pattern it is at least one of in a manner of form the 2nd resin bed, make the 1st resin bed and the 2nd resin bed co-curing (S5).
Description
Technical field
The present invention relates to the manufacture method of conducting film and conducting film.
Background technology
According to the purposes applied into various electronic units, develop, produced various conducting films.For example, electrically conducting transparent
Film is in liquid crystal display (LCD), plasm display panel (PDP), organic electroluminescence type display, solar cell
(PV) and in the various fields such as the transparency electrode of touch panel (TP), antistatic (ESD) film and electromagnetic wave shielding (EMI) film make
With.As these nesa coatings, in the past, the nesa coating that make use of ITO (tin indium oxide) is used, but exist following
The problem of such：The supply stability of indium is low, and manufacturing cost is high, lacks flexibility, and, high temperature is needed during film forming.Therefore, generation
Exploration for ITO nesa coating is actively carried out.Wherein, the nesa coating containing metal nanometer line due to electric conductivity,
Optical characteristics and flexibility are excellent, and using wet process film forming, manufacturing cost is low, and high temperature, etc. is not needed during film forming, because
And the nesa coating as replacement ITO is suitable.
For example, as it is known that comprising nano silver wire, have high conductivity, optical characteristics, flexibility nesa coating (referring to
Patent document 1).In addition, following, Patent Document 2 discloses have the electrically conducting transparent containing metal nanometer line over the transparent substrate
The manufacture method of the nesa coating of layer.
In such nesa coating, the adaptation height of conductive layer and substrate is necessary, in addition, especially for containing
For the nesa coating of metal nanometer line, because the surface area of the unit mass of the metals such as silver is big, easily with various compounds
Reaction, accordingly, there exist be short of the problem of environmental resistance is such.Therefore, because the various medicaments used in process, cleaning solution
Influence of oxygen, moisture in the air influence, being exposed by long-term preserve etc., nanostructure easily corrodes, and electric conductivity is held
Easily decline.In addition, especially in the purposes such as electronic material, in order to prevent the attachment such as microgranular impurity, dust, dust, mix
Enter the surface of substrate, usually carry out physics washing procedure using brush etc., but by the process, also surface can be caused to damage,
This turns into problem.
In order to solve the above problems, a variety of surface stacked guards in the nesa coating comprising nano silver wire have been carried out
Film, the trial to nesa coating imparting environmental resistance and marresistance.(referring to patent document 3~4).
As described previously for nesa coating, it is desirable to the adaptation of conductive layer and substrate, environmental resistance and marresistance
It is high.
Prior art literature
Patent document
Patent document 1:Japanese Unexamined Patent Application Publication 2010-507199 publications
Patent document 2:No. 5609008 publications of Japanese Patent No.
Patent document 3:Japanese Unexamined Patent Publication 2014-191894 publications
Patent document 4:Japanese Unexamined Patent Publication 2013-200943 publications
The content of the invention
Invent problem to be solved
It is an object of the invention to provide the adaptation of conductive layer and substrate, environmental resistance and the high conducting film of marresistance
Manufacture method and conducting film.
Means for solving the problems
In order to reach above-mentioned purpose, an embodiment of the invention is a kind of manufacture method of conducting film, methods described
Including following processes：The process that the 1st resin bed is formed on substrate using the 1st resin combination comprising the 1st functional group, preceding
The process that conductive pattern when overlooking with opening portion is formed on the 1st resin bed is stated, using comprising can be with foregoing 1st resin bed
2nd resin combination of the 2nd functional group of the 1st functional group's co-curing by be coated to aforesaid conductive pattern it is at least one of in a manner of
The process of the 2nd resin bed is formed, and makes the process of foregoing 1st resin bed and the 2nd resin bed co-curing.
Preferably, after becoming inviscid on the surface of foregoing 1st resin bed, above-mentioned conductive pattern is formed.
In addition, above-mentioned 1st functional group includes carboxyl, hydroxyl, epoxy radicals, (methyl) acryloyl group, vinyl, pi-allyl etc.
In subsequent handling have reactivity position, it is preferred that the 1st resin combination include the polyurethane containing carboxyl,
The ring of phenol novolak type epoxy resin, phenoxy resin, the polyurethane containing carboxyl with being less than 1 equivalent in terms of carboxyl benchmark
It is any number of in the mixture of oxygen compound, dially phthalate resin.
It is further preferred, that above-mentioned 2nd resin combination includes the mixing of the polyurethane containing carboxyl and epoxide
Thing, phenol novolak type epoxy resin, phenoxy resin, the polyurethane containing carboxyl with carboxyl benchmark be calculated as 1 equivalent with
On the mixture of epoxide, dially phthalate resin and acrylate monomer mixture in it is any number of.
It is further preferred, that aforesaid substrate, the 1st resin bed, conductive pattern and the 2nd resin bed are transparent.
In addition, the other embodiment of the present invention is a kind of conducting film, it is characterised in that has on substrate and includes the 1st
1st resin bed of functional group, the conductive pattern with opening portion when on the 1st resin bed with vertical view, to be coated to the conduction
At least one of mode of pattern is formed with the 2nd resin bed for including the 2nd functional group, also, in aforesaid conductive pattern openings
The curing reaction part of the 1st functional group and the 2nd functional group of the 2nd resin bed in portion with the 1st resin bed.
Preferably, the total light transmittance of above-mentioned conducting film is more than 70%.
Above-mentioned conductive pattern can include the metal nanometer line with unordered cross-contact portion.
Above-mentioned conductive pattern can include the metal fine pattern regularly or irregularly formed.
The effect of invention
Pass through the present invention, it is possible to provide the good conduction of adaptation, environmental resistance, marresistance and optical characteristics with substrate
Film.
Brief description of the drawings
Fig. 1 is the process chart of the manufacture method for the conducting film that embodiment is related to.
Fig. 2 is the concept map for amplifying conductive pattern portions that embodiment is related to.
Fig. 3 is the figure of the environmental resistance evaluation result for the conducting film for representing embodiment 1 and comparative example 7.
Embodiment
Hereinafter, the embodiment (hereinafter referred to as embodiment) of the present invention is illustrated.
The manufacture method for the conducting film that embodiment is related to is characterised by, including following processes：Using including the 1st function
The process that 1st resin combination of group forms the 1st resin bed on substrate, there is opening when being formed and being overlooked on the 1st resin bed
The process of the conductive pattern in portion, using comprising can be with the 2nd of the 2nd functional group of the 1st functional group's co-curing of above-mentioned 1st resin bed the
Resin combination by be coated to conductive pattern it is at least one of in a manner of form the process of the 2nd resin bed, and make the 1st resin bed with
The process of 2nd resin bed co-curing.
The process chart of the manufacture method of conducting film of the present embodiment is shown in Fig. 1.In Fig. 1, first, in substrate 10
Upper formation the 1st resin bed (priming coat) 12 (S1：1st resin bed formation process).Herein, for the 1st resin bed 12, as long as
It is that can be used with the resin of the excellent adhesion of substrate 10.
The method for implementing above-mentioned S1 (the 1st resin bed formation process) is not particularly limited, and can enumerate such as silk-screen printing, recessed
The contact such as version printing and their hectographic printing, bar coater, die coating machine, gravure coater printing, ink jet printing, spraying, spreading
The off-contact printings such as device (dispenser).
As the base material for forming substrate 10, it is not particularly limited, glass substrate, PET (poly terephthalic acid second two can be used
Alcohol ester) resin film such as film, PEN (PEN) film etc..
In addition, the 1st resin bed 12 is made up of the 1st resin combination comprising the 1st functional group, the 1st functional group is in base
Formed on the surface of plate 10 after the 1st resin bed 12 can be with forming the 2nd resin bed described later the 2nd resin combination in include the
2 functional group's co-curings.
Next, for above-mentioned 1st resin bed 12, it is preferred that on the surface of the substrate 10 by the 1st resin combination
After thing is formed as stratiform, heated at normal temperatures or at appropriate temperature, thus, its solidification or drying is used for described later
The conductive material for forming conductive pattern is not absorbed in the degree (S2 of the inside to the 1st resin bed 12：1st resin combination back tender
Sequence).Solidification or the degree dried can be judged by following manner：According to JIS K 5701, utilize parallel plate viscometer
(spreadometer) result of the experiment carried out is 0mm, becomes the state of no mobility, if solid using being formed at normal temperatures
The resin combination of the resin bed of body, then in conductive pattern formation process described later, conductive material will not be absorbed in the 1st completely
In 12 layers of resin bed, thus preferably.After formation (S1), solidification or dry (S2) in the 1st resin bed 12, in the 1st resin bed 12
It is upper to form the conductive pattern 14 when overlooking with opening portion." conductive pattern " is also included to be paved with the situation that whole planar is formed.Afterwards
Have during vertical view shown in the Fig. 2 (a) stated the conductive pattern 14 of opening portion for example can by will in decentralized medium dispersed metal
The ink (ink) (following, sometimes referred to as " metal nanometer line ink ") that nano wire forms is printed on the 1st resin bed 12 and forms pattern
(S3：Printing process), by the metal nanometer line ink irradiation light or being heated so as to be burnt till (S4：Firing process) and
Obtain.The surface of the conductive pattern comprising metal nanometer line through burning till turns into the shape exposed upwards from the surface of the 1st resin bed 12
State.
So-called herein " opening portion ", refer to that the 2nd resin combination described later is thick as being contacted with the 1st resin combination
The breakthrough part in direction is spent, as shown in Fig. 2 (a), (b), there is gap between metal nanometer line 18 or metal fine 19.Need
Bright, Fig. 2 (a), (b) are the concept maps for partly amplifying conductive pattern 14.
In the case of using metal nanometer line ink, by being printed, so that metal nanometer line 18 is disorderly to have
The mode in cross-contact portion is accumulated on substrate, and in the cross-contact portion, electrical connection (including connects metal nanometer line 18 each other
Tactile situation), electric conductivity (Fig. 2 (a)) is thus presented.In addition, opening portion 20 now passes through the metal nano disorderly accumulated
Line 18 and turn into irregular shape.Even if using the whole facial mask of metal nanometer line ink print, can also obtain having in thickness direction
The conductive pattern of the opening portion 20 of upper insertion.So-called herein " metal nanometer line ", refer to have a diameter of tens of nm~hundreds of nm,
Length is the metal nanometer line of several μm~tens of μm of shape.
In addition, in the example shown in Fig. 2 (b), opening for shape (rectangle) of rule is formd by metal fine 19
Oral area 20.Metal foil or metal nanoparticle described later ink can be used to be formed for metal fine 19.It should be noted that Fig. 2 (b)
Example in, metal fine 19 is arranged in clathrate, has cross part, but for example also can be according to row parallel in a certain direction
Row, the mode without cross part are formed.In addition, also can irregularly configure metal fine 19, it is random to make opening portion 20
Shape.
The printing process implemented in above-mentioned S3 (printing process) is not particularly limited, as long as can be by metal nanometer line ink
The printing process of pattern is printed as, can be used.Such as silk-screen printing, intaglio printing and their hectographic printing, rod can be enumerated
The off-contact printings such as the contact such as painting machine, die coating machine, gravure coater printing, ink jet printing, spraying, dispenser.It is above-mentioned in progress
In the case of contact printing, preferably the 1st resin bed 12 by such as the 1st resin combination by being coated on substrate 10 to be formed
Afterwards, dry to touch state (without tackiness), i.e. state of the surface without sticky (without tackiness) are turned into.Thus, even if printing dress
Put and contacted with the 1st resin bed 12, can also carry out good printing.It should be noted that in order to forming the 2nd resin bed 16
2nd resin combination carry out co-curing when, shorten hardening time, can form the 1st resin bed 12 the 1st resin combination in mix
Close curing accelerator.In the case where the 1st resin combination includes epoxide described later, preferably it is pre-mixed solidification and promotes
Agent.
On the other hand, in the case where carrying out the off-contact printing of ink-jetting style etc, it is not necessary to make the 1st resin bed 12 be
Dry to touch state, it is not absorbed in the degree of the inside of the 1st resin bed 12 completely for conductive material, becomes the surface of conductive material
The state exposed on the surface of the 1st resin bed 12.
It should be noted that the ink as the printing available for conductive pattern 14, is not limited to above-mentioned metal nanometer line ink,
Such as metal nanoparticle ink can be used.But in the case of using metal nanoparticle ink, in order to which electric conductivity is presented, it is necessary into
The state densely contacted each other for conducting particles, opening portion 20 is there's almost no when forming whole facial mask, during vertical view.Therefore,
In order to form the pattern with opening portion 20, it is necessary to form the fine rule figure for example as shown in Fig. 2 (b), with opening portion 20
Case (pattern of metal fine 19).Thread pattern can be regularly formed, and also can irregularly be formed, also can be according to such as network diagramming
The case mode with cross part like that is formed.So-called herein " metal nanoparticle ", refer to have the particle diameter with nm levels it is spherical,
Horn shape, flat [plate] shape etc., the particle of preferably spherical shape.
When the total light transmittance for foring the substrate of the conductive pattern 14 after printing is more than 80%, it can be ensured that for making
The sufficient space that 1st resin bed 12 contacts with the 2nd resin bed 16 described later, thus preferably.
Next, by cover conductive pattern it is at least one of in a manner of form (the S5 of the 2nd resin bed (coating) 16：2nd
Resin bed formation process).The available method same with foregoing S1 (the 1st resin bed formation process) of the process is implemented.It is so-called
" at least a portion ", including whole.For example, in the case of in order to make a part expose as electrode portion with turned on outside,
The part is not coated to.In this case, the state for being coated to a part is turned into.Herein, the 2nd resin bed 16 is by comprising can be with forming
2nd resin combination of the 2nd functional group of the 1st functional group's co-curing included in the 1st resin combination of above-mentioned 1st resin bed 12
Thing is formed.After the 2nd resin bed formation process (S5), the 1st resin bed 12 is made based on above-mentioned 1st functional group and the 2nd functional group
With the co-curing (S6 of the 2nd resin bed 16：Co-curing process (omitting diagram)).That is, the 1st function included in the 1st resin bed 12 is made
With the 2nd functional group included in the 2nd resin bed 16 curing reaction occurs for group.Conductive pattern 14 has opening portion in thickness direction
20, the 2nd resin combination for forming the 2nd resin bed 16 enters the opening portion 20, occurs admittedly with the interface of the 1st resin bed 12
Change reaction.That is, in the opening portion 20 of conductive pattern 14, there is the 1st functional group and the 2nd resin bed 16 of the 1st resin bed 12
The curing reaction part of 2nd functional group.As a result, conductive pattern 14 is clamped by the 1st resin bed 12 with the 2nd resin bed 16
(sandwich), and in the opening portion 20 of conductive pattern 14 it is kept, can obtain has good adaptation with substrate 10
Conductive pattern 14.As the combination of the 1st functional group and the 2nd functional group of the 2nd resin bed 16 of the 1st resin bed 12, example can be enumerated
Such as carboxyl/epoxy, epoxy radicals/carboxyl, hydroxyl/carboxyl, (methyl) acryloyl group/vinyl, vinyl/(methyl) acryloyl
Base, pi-allyl/(methyl) acryloyl group etc., but it is not limited to these.
2nd resin combination of the 1st resin combination with forming the 2nd resin bed 16 as the above-mentioned resin bed 12 of composition the 1st
The combination of thing, according to (the 1st resin bed：2nd resin bed) order, can enumerate：((the 1st functional group is the polyurethane containing carboxyl
Carboxyl)：The mixture (the 2nd functional group is epoxy radicals) of polyurethane and epoxide containing carboxyl), (phenol novolacs
Type epoxy resin (the 1st functional group is epoxy radicals)：Phenol novolak type epoxy resin (the 2nd functional group is epoxy radicals)), (benzene
Epoxide resin (the 1st functional group is epoxy radicals)：Phenoxy resin (the 2nd functional group is epoxy radicals)), (polyurethane containing carboxyl
(the 1st functional group is carboxyl)：Phenoxy resin (the 2nd functional group is epoxy radicals)), (polyurethane containing carboxyl with carboxyl base
Mixture of the quasi- meter less than the epoxide of 1 equivalent (the 1st functional group is carboxyl)：Polyurethane containing carboxyl with carboxyl base
Standard is calculated as the mixture (the 2nd functional group is epoxy radicals) of epoxide more than 1 equivalent), (dially phthalate resin
(the 1st functional group is pi-allyl)：(the 2nd functional group is alkene to the mixture of dially phthalate resin and acrylate monomer
Propyl group and acryloyl group)) etc..
In combinations thereof, contain in the 1st resin combination comprising the polyurethane containing carboxyl, the 2nd resin combination
In the case of the combination of the polyurethane and epoxide of carboxyl, by adding to the 1st resin bed 12 and the 2nd resin bed 16
Heat so that the carboxyl (the 1st functional group) of the polyurethane containing carboxyl included in the 1st resin bed 12 and the 2nd resin bed 16 with
The epoxy radicals (the 2nd functional group) of epoxide is bonded and co-curing occurs.1st resin combination includes the poly- ammonia containing carboxyl
Ester and epoxide, the 2nd resin combination in terms of carboxyl benchmark less than 1 equivalent include the polyurethane containing carboxyl and with carboxylic
Co-curing similarly occurs for the situation that base benchmark is calculated as the combination of epoxide more than 1 equivalent.In addition, in phenol novolac
Type epoxy resin combination each other, in the case of phenoxy resin composition combination with one another, by adding appropriate ring
Oxygen tree fat is with curing agent and is heated so as to which co-curing occur.In this case, the 1st functional group and the 2nd functional group turn into
Epoxy radicals.In addition, include phenoxy resin comprising the polyurethane containing carboxyl, the 2nd resin combination in the 1st resin combination
In the case of combination, by being heated to the 1st resin bed 12 and the 2nd resin bed 16, so as to carboxyl (the 1st functional group) and epoxy
Base (the 2nd functional group) is bonded and co-curing occurs.In addition, include dially phthalate resin (the in the 1st resin combination
1 functional group is pi-allyl), the 2nd resin combination include dially phthalate resin and acrylate monomer (the 2nd function
Group is pi-allyl and acryloyl group) combination in the case of, it is solid altogether to occur so as to carry out addition polymerization by carrying out light irradiation
Change.
Herein, aforesaid substrate 10, the 1st resin bed 12, the resin bed 16 of conductive pattern 14 and the 2nd are preferably transparent.Thus,
It can be applied to the transparent elements such as touch panel.So-called transparent herein, it is more than 80% to refer to total light transmittance.Comprising them
Into the total light transmittance of conducting film of the invention of composition be preferably more than 70%, more preferably more than 75%, further
Preferably more than 80%.
Embodiment
Hereinafter, embodiments of the invention are illustrated.It should be noted that following embodiment is used to will be readily understood that this
Invention, the present invention are not restricted by the embodiments.
In the present embodiment, the molecular weight and acid number of resin and the total light transmittance of conductive pattern and sheet resistance according to
In the following manner determines.
＜ molecular weight ＞
The value to be converted according to polystyrene measured using gel permeation chromatography (hereinafter referred to as GPC).
GPC condition determination is as described below.
Device name：Japan Spectroscopy Corporation HPLC units HSS-2000
Post：Shodex posts LF-804
Mobile phase：Tetrahydrofuran
Flow velocity：1.0mL/min
Detector：Japan Spectroscopy Corporation RI-2031Plus
Temperature：40.0℃
Sample size：The μ L of sample loop 100
Sample solution concentration：It is prepared into about 0.1 mass %
＜ acid numbers ＞
With precision balance precise about 0.2g samples to 100ml conical flasks, ethanol/toluene=1/2 (matter is added thereto
Amount ratio) mixed solvent 10ml dissolved.And then into the container drop of addition 1~3 ethanolic phenolphthalein solution as indicator,
It is sufficiently stirred until sample becomes uniform.It is titrated with 0.1N potassium hydroxide-ethanol solution, by the blush of indicator
Terminal when continuing 30 seconds as neutralization.Using by its result, the acid number using the value that following calculating formulas obtains as resin.
Acid number (mg-KOH/g)=(B × f × 5.611)/S
B：The usage amount (ml) of 0.1N potassium hydroxide-ethanol solution
f：The factor of 0.1N potassium hydroxide-ethanol solution
S：The collection capacity (g) of sample
＜ total light transmittances ＞
It is the conductive pattern formed with the cutting of 50mm square on substrate, uses nephelometer (NDH2000, the electric color work of Japan
Industry system) be measured obtained from value.
＜ sheet resistances ＞
Use resistrivity meter ロ レ ス タ (registration mark) GP MCP-T610 types (Mitsubishi Chemical ア Na リ テ ッ Network systems), profit
It is measured with 4 terminal methods.Mode determination and ESP patterns are used using terminal.
＜ contains the synthesis example ＞ of the polyurethane of carboxyl
[synthesis example 1]
To with agitating device, thermometer, condenser 2L three-necked bottles in, be loaded as the C- of polyol compound
(Co., Ltd.'s Network ラ レ systems, PCDL, raw material glycol mol ratio are 1,9- nonanediols to 1015N:2- methyl isophthalic acids, 8- are pungent
Glycol=15:85, molecular weight 964) 143.6g, 2, the 2- dimethylolpropionic acid (days as the dihydroxy compounds with carboxyl
This chemical conversion Co. Ltd. system) 27.32g and the propylene glycol monomethyl ether (trade name as solvent：Acetic acid methoxy propyl
Ester, ダ イ セ Le Co. Ltd. system) 259g, dissolve above-mentioned 2,2- dimethylolpropionic acids in 90 DEG C.
The temperature of reaction solution is reduced to 70 DEG C, using dropping funel, the デ being added dropwise through 30 minutes as polyisocyanates
ス モ ジ ュ ー Le (registration mark)-W (di-2-ethylhexylphosphine oxide (4- cyclohexyl isocyanates), firmly changes バ イ エ Le ウ レ タ Application strain formulas
Commercial firm's system) 87.5g.After completion of dropwise addition, 120 DEG C are warming up to, carries out reacting for 6 hours in 120 DEG C, isocyanates is confirmed by IR
After basic disappearance, isobutanol 0.5g is added, and then in 120 DEG C react within 6 hours.The weight of the obtained polyurethane containing carboxyl
Average molecular weight is 32300, and the acid number of the resin is 40mgKOH/g.
[synthesis example 2]
Except having used C-1015N (Co., Ltd.'s Network ラ レ systems) 44.8g, 2,2- dimethylolpropionic acid (Japanization strain
Formula commercial firm system) 16.1g and propylene glycol monomethyl ether (ダ イ セ Le Co. Ltd. system) 100.3g, デ as solvent
It is same with synthesis example 1 outside ス モ ジ ュ ー Le (registration mark)-W (firmly changing バ イ エ Le ウ レ タ Application Co. Ltd. system) 40.7g
Operate sample, obtain the polyurethane containing carboxyl.The weight average molecular weight of the obtained polyurethane containing carboxyl is 29200, the tree
The acid number of fat is 60mgKOH/g.
[embodiment 1]
As shown in table 1 like that, in PET (polyethylene terephthalate) substrate (East レ (strain) Le ミ ラ ー processed (registrations
Trade mark) 125T60) on, using bar coater printer's ink, the ink is to coordinate the polyurethane tree containing carboxyl synthesized in synthesis example 1
Fat and キ ュ ア ゾ ー Le (registration mark) 2P4MHZ-PW (2- phenyl -4- methyl -5- hydroxymethyls as curing accelerator
Imidazoles, relative to the mass parts of resin 100, add 1 mass parts) and turn into 30 with the resin component concentration comprising curing accelerator
Quality % mode is diluted with propylene glycol monomethyl ether and forms (equivalent to the 1st resin combination), in 100
DEG C carry out drying in 1 hour, is formed thickness be 10 μm (using ミ Star ト ヨ high-precision digital-display micrometers (digimatic
Micrometer) MDH-25M 293-100, measure arbitrary 5 at obtained from average value) priming coat (equivalent to the 1st resin
Layer).The thickness of priming coat forms priming coat by measure and carries out the dried thickness including substrate and subtract the thickness of substrate
Spend and obtain.
After drying, implement tackiness evaluation based on JIS Z0237.The situation that all balls are not stopped is as without hair
It is viscous, the state table that any ball stops is shown with tacky.
After confirming without tacky (without tackiness), nano silver wire dispersion liquid is made, and (by nano silver wire 0.125g, (line is average
Diameter is about 40nm, and average length is about 10 μm, is the number average by SEM 100 nano silver wires arbitrarily observed) point
Dissipate in ethanol 50g (preparing the mass % dispersion liquids of nano silver wire 0.25)), using dispersion liquid 0.05g, using bar coater, with not
The mode overflowed from priming coat is coated.The coating of nano silver wire dispersion liquid has been carried out well.Coating nano silver wire disperses
After liquid, in 100 DEG C burn till within 1 hour, form the conductive pattern of whole planar.Sheet resistance after burning till is 80 Ω/, Quan Guang
Line transmitance is 89%.
Then, as coating (equivalent to the 2nd resin bed), using bar coater, to cover the substantially entire surface of conductive pattern
Mode printer's ink, in 140 DEG C carry out 1 hour co-curing, the ink is the polyurethane containing carboxyl synthesized in synthesis example 1
In resin 10g and epoxide (Mitsubishi Chemical jER (registration mark) 828) 0.69g, coordinate relative to poly- containing carboxyl
It is 1 mass parts for the mass parts of total amount 100 of urethane resin and epoxide (Mitsubishi Chemical jER (registration mark) 828)
Curing accelerator (four countries be melted into processed キ ュ ア ゾ ー Le (registration mark) 2P4MHZ-PW) and formed (equivalent to the 2nd resin
Composition, propylene glycol monomethyl ether is used in a manner of the resin component concentration comprising curing accelerator turns into 30 mass %
Dilution).Overall thickness untill including priming coat is 20 μm.If relative to the poly- ammonia containing carboxyl synthesized in synthesis example 1
The mass parts of ester resin 100 coordinate the epoxide (Mitsubishi Chemical jER (registration mark) 828) of 6 mass parts, then synthesis example 1
The carboxyl of the polyurethane resin containing carboxyl of middle synthesis and epoxide (Mitsubishi Chemical jER (registration mark) 828)
Epoxy radicals turns into 1 equivalent.For the coating (equivalent to the 2nd resin bed) of embodiment 1, as shown in table 1 like that, make synthesis
The cooperation of the polyurethane resin containing carboxyl synthesized in example 1 and epoxide (Mitsubishi Chemical jER (registration mark) 828)
It is 100 to 7 (being 100/7 described in table 1) than (mass ratio), therefore, turns into following compositions：Relative to what is synthesized in synthesis example 1
For the carboxyl of polyurethane resin containing carboxyl, the epoxy radicals of epoxide (Mitsubishi Chemical jER (registration mark) 828)
Somewhat excessively exist.
For obtained conducting film, following evaluating characteristics are carried out.Show the result in table 1.
(adaptation evaluates (disbonded test))
For cured film, evaluated as adaptation, carry out cross cut test (cross cut test) JIS K5600.Will knot
Fruit is recorded in table 1,2 as " disbonded test ".It should be noted that the numerical value of result of the test is smaller, adaptation (resistance to stripping is represented
From property) higher (being most preferably 0).In table 1, the disbonded test result of embodiment 1 is 0, it is known that adaptation (peel resistance) is high.
(marresistance experiment)
Test, simply judged by paper friction scratch resistance as marresistance.For the paper used, JK is used
ワ イ パ ー, reciprocal 5 times on the cover layer.By visual observation and microscope, confirmation have not damaged, scratch.Using result as " anti-scratch
Wound property is tested " and it is recorded in table 1,2.
◎：By visual observation and microscope does not observe damage, scratch.
○：Do not observe damage by visual observation, but Slight abrasion marks are observed by microscope.
△：Do not observe damage by visual observation, but damage, scratch are observed by microscope.
×：Damage, scratch can be differentiated by visual observation.
(environmental resistance)
As environmental resistance, using Constant Temperature and Humidity Chambers (ETAC TH402A), in 85 DEG C, 85%RH (relative humidity) atmosphere
Lower preservation, changed with the ratio relative to initial surface resistivity to determine the sheet resistance untill after about 1100 hours.Will knot
Fruit is shown in Fig. 3.
(optical characteristics)
As optical characteristics, the conducting film that is obtained using Haze meter NDH 2000 (the electric color system of Japan) measure
HAZE (mist degree) and determination of light transmittance.Table 1,2 is recorded in using result as " optical characteristics ".
○：Total light transmittance is more than 80% and HAZE is less than 20%
×：Total light transmittance is that more than 80% and HAZE is higher than 20%
[embodiment 2~6]
The ink prepared similarly to Example 1 in addition to using being formed except the material being changed to shown in table 1, by same
Thickness is formed, same process forms priming coat, conductive pattern and coating.Carry out adaptation evaluation similarly to Example 1
The experiment of (disbonded test), marresistance, optical characteristics evaluation, show the result in table 1.If in the coating relative to embodiment 2
The mass parts of polyurethane resin 100 containing carboxyl synthesized in the synthesis example 2 used, coordinate epoxide (Mitsubishi Chemical's system
JER (registration mark) 828) 9 mass parts, then the carboxyl and epoxidation of the polyurethane resin containing carboxyl synthesized in synthesis example 2
The epoxy radicals of compound (Mitsubishi Chemical jER (registration mark) 828) turns into 1 equivalent.For embodiment 2 coating (equivalent to
2nd resin bed) for, as shown in table 1 like that, make the polyurethane resin and epoxy compound containing carboxyl synthesized in synthesis example 2
The match ratio (mass ratio) of thing (Mitsubishi Chemical jER (registration mark) 828) is 100 to 10 (they being 100/10 described in table 1), because
This, turns into following compositions：For the carboxyl of the polyurethane resin containing carboxyl synthesized in synthesis example 2, epoxy compound
The epoxy radicals of thing (Mitsubishi Chemical jER (registration mark) 828) is somewhat excessively present.
In addition, for the priming coat (equivalent to the 1st resin bed) of embodiment 6, as shown in table 1 like that, make synthesis example 1
The polyurethane resin containing carboxyl of middle synthesis and the match ratio of epoxide (Mitsubishi Chemical jER (registration mark) 828)
(mass ratio) is 100 to 3 (being 100/3 described in table 1), therefore, turns into following compositions：What is synthesized in synthesis example 1 contains carboxyl
Polyurethane resin carboxyl residual half.It should be noted that the coating (equivalent to the 2nd resin bed) of embodiment 6 and reality
It is same to apply example 1.
[embodiment 7]
The ink prepared similarly to Example 1 in addition to using being formed except the material being changed to shown in table 1, by same
Thickness is formed, same process forms priming coat, conductive pattern and coating.Now, the curing accelerator as coating, generation
For キ ュ ア ゾ ー Le (registration mark) 2P4MHZ-PW (four countries' chemical conversion system), IRGACURE (registration mark) 184 has been used
(BASF AG's system).It should be noted that instead of 140 DEG C of solidifications of 1 hour, small-sized UV irradiation units QRU-2161- is used
Z11-00 (Co., Ltd.'s オ ー Network makes institute), carries out about 40mW/cm2Exposure, thus carries out co-curing.Carry out and embodiment 1
Same adaptation evaluates (disbonded test), marresistance experiment, optical characteristics evaluation, shows the result in table 1.
[comparative example 1]
The material shown in table 2 is changed to form and form priming coat.Priming coat is liquid state, tacky serious, even if sharp
With other print processes such as ink-jet, also fail to carry out the printing of nano silver wire ink.Think that reason is：In other examples middle-molecular-weihydroxyethyl
For more than 10,000, on the other hand, the molecular weight of the resin of comparative example 1 is small, is 4100.
[comparative example 2~5]
The ink prepared similarly to Example 1 in addition to using being formed except the material being changed to shown in table 2, by same
Thickness is formed, same process forms priming coat, conductive pattern and coating.Wherein, comparative example 4 carries out about 40mW/cm2UV
Light exposes, and carries out the processing suitable with co-curing.The adaptation carried out similarly to Example 1 evaluates (disbonded test), scratch resistance
Property experiment, optical characteristics evaluation, show the result in table 2.
In embodiment 1~4, identical resin component is used in priming coat and coating, when carrying out co-curing, is passed through
The chemical bonding of priming coat and coating and it is closely sealed, it is not peeling-off.
In embodiment 5, in the priming coat resin component different from having been used in coating, but due to co-curable
Functional group, thus, there is no the stripping after solidification between priming coat and coating.On the other hand, in comparative example 4,5, the bottom of at
The coating resin different from having used curing mechanism in coating, UV is implemented in comparative example 4 and solidifies, is real in comparative example 5
In the case of having applied heat cure, with coating co-curing does not occur for priming coat, peeling-off between priming coat and coating.
In addition, in embodiment 6, as priming coat, the ratio of half is remained to poly- containing carboxyl with functional group's (carboxyl)
Epoxide (Mitsubishi Chemical jER (registration mark) 828) is added in urethane, under 100 DEG C of drying conditions of 1 hour, into
It is closely sealed also with coating by being chemically bonded by residual functionality for appropriate state as semi-solid preparation, thus, there is no
Stripping between priming coat and coating.On the other hand, for comparative example 2 and 3, for what is used in priming coat and coating
The condition that resin can be fully cured, the time point of priming coat (100 DEG C, drying in 1 hour) is being formd, it is residual with coating reaction
Remaining functional group disappears in priming coat, therefore, peeling-off between priming coat and coating (disbonded test result is 5).
It can be seen from embodiment 1~6 and comparative example 2~5, the superiority of co-curing is carried out.
[table 1]
[table 2]
[comparative example 6]
In addition to being not provided with priming coat, for composition similarly to Example 1.Similarly to Example 1 closely sealed is carried out
Property evaluation (disbonded test), marresistance experiment, optical characteristics evaluation, show the result in table 2.Disbonded test, scratch resistance experiment
Well, but due to base coat, thus when the pet substrate after to silver coating nanowire dispersion heats, full light is saturating
Crossing rate reduces by more than 5%, but is more than 80%.However, HAZE is 2% before heating, but after the heating more than 50%, optics is special
Property is significantly damaged.By heating, oligomer separates out from pet substrate, surface roughness increase, therefore, damages optical characteristics.
[comparative example 7]
To be not provided with coating comparative example.Carried out similarly to Example 1 adaptation evaluation (disbonded test),
Marresistance experiment, optical characteristics evaluation, show the result in table 2.Due in the absence of coating, therefore, being tried by marresistance
Test, damage is produced in metal portion, in addition, the result of environmental resistance similarly to Example 1 as shown in Figure 3 is understood, passing through
After about 700 hours, resistance starts significantly to rise, and environmental resistance is low.
Description of reference numerals
10 substrates, 12 the 1st resin beds, 14 conductive patterns, 16 the 2nd resin beds, 18 metal nanometer lines, 19 metal fines, 20
Opening portion.
Claims (10)
1. a kind of manufacture method of conducting film, it includes following processes：
The process that the 1st resin bed is formed on substrate using the 1st resin combination comprising the 1st functional group,
There is the process of the conductive pattern of opening portion when being formed and being overlooked on foregoing 1st resin bed,
Using comprising can be with the 2nd resin combination of the 2nd functional group of the 1st functional group's co-curing of foregoing 1st resin bed with quilt
The process that at least one of mode of aforesaid conductive pattern forms the 2nd resin bed is covered, and
Make the process of foregoing 1st resin bed and the 2nd resin bed co-curing.
2. the manufacture method of conducting film according to claim 1, wherein, become on the surface of foregoing 1st resin bed without viscous
Property after, formed aforesaid conductive pattern.
3. the manufacture method of conducting film according to claim 1 or 2, wherein, foregoing 1st functional group include carboxyl, hydroxyl,
It is any number of in epoxy radicals, (methyl) acryloyl group, vinyl, pi-allyl.
4. according to the manufacture method of conducting film according to any one of claims 1 to 3, wherein, foregoing 1st resin combination bag
Containing the polyurethane containing carboxyl, phenol novolak type epoxy resin, phenoxy resin, the polyurethane containing carboxyl with carboxyl
Benchmark meter is less than any number of in the mixture of the epoxide of 1 equivalent, dially phthalate resin.
5. according to the manufacture method of conducting film according to any one of claims 1 to 4, wherein, foregoing 2nd resin combination bag
Mixture, phenol novolak type epoxy resin, phenoxy resin containing the polyurethane containing carboxyl and epoxide, contain
The mixture of the polyurethane of carboxyl and the epoxide being calculated as with carboxyl benchmark more than 1 equivalent, dially phthalate tree
It is any number of in the mixture of fat and acrylate monomer.
6. according to the manufacture method of conducting film according to any one of claims 1 to 5, wherein, aforesaid base plate, the 1st resin bed,
Conductive pattern and the 2nd resin bed are transparent.
7. a kind of conducting film, wherein, there is the 1st resin bed for including the 1st functional group on substrate, have on the 1st resin bed
There is the conductive pattern of opening portion when having vertical view, by be coated to the conductive pattern it is at least one of in a manner of formed with including the 2nd
2nd resin bed of functional group, also, the 1st functional group in aforesaid conductive pattern openings portion with foregoing 1st resin bed and the
The curing reaction part of 2nd functional group of 2 resin beds.
8. conducting film according to claim 7, wherein, total light transmittance is more than 70%.
9. the conducting film according to claim 7 or 8, wherein, aforesaid conductive pattern, which includes, has unordered cross-contact portion
Metal nanometer line.
10. the conducting film according to claim 7 or 8, wherein, aforesaid conductive pattern is included and regularly or irregularly formed
Metal fine pattern.
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| JP2015-150490 | 2015-07-30 | ||
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| PCT/JP2016/071920 WO2017018427A1 (en) | 2015-07-30 | 2016-07-26 | Method for producing conductive film, and conductive film |
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| JP (1) | JP6664396B2 (en) |
| KR (1) | KR102000956B1 (en) |
| CN (1) | CN107615408B (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112321868A (en) * | 2019-07-18 | 2021-02-05 | 波音公司 | Removal of surface films and primers from composite substrates by use of co-cured paint films |
| CN113196891A (en) * | 2018-12-27 | 2021-07-30 | 富士胶片株式会社 | Photosensitive transfer material, laminate, touch panel, method for manufacturing substrate with pattern, method for manufacturing circuit substrate, and method for manufacturing touch panel |
| CN113316743A (en) * | 2018-12-27 | 2021-08-27 | 富士胶片株式会社 | Conductive transfer material, method for manufacturing substrate having pattern, method for manufacturing circuit substrate, laminate, and touch panel |
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| JP2019206738A (en) * | 2018-05-30 | 2019-12-05 | Ｄｏｗａエレクトロニクス株式会社 | Silver nanowire ink, transparent conductive film producing method and transparent conductive film |
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| JP2002164247A (en) * | 2000-11-24 | 2002-06-07 | Murata Mfg Co Ltd | Dielectric ceramic composition and layered ceramic capacitor |
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| WO2010064630A1 (en) * | 2008-12-02 | 2010-06-10 | 大日本印刷株式会社 | Electromagnetic wave shielding material, and method for manufacturing same |
| JP2013200943A (en) | 2012-03-23 | 2013-10-03 | Toray Advanced Film Co Ltd | Transparent conductive film and manufacturing method of the same, and touch panel |
| JP2014075215A (en) * | 2012-10-03 | 2014-04-24 | Sekisui Chem Co Ltd | Insulation material, multilayer film, laminate, connection structure, production method of laminate, and production method of connection structure |
| JP2014191894A (en) | 2013-03-26 | 2014-10-06 | Dic Corp | Transparent electroconductive film and touch panel |
| KR20150084689A (en) * | 2014-01-14 | 2015-07-22 | 주식회사 동진쎄미켐 | Transparent conductive electrode and method for producing the same |
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| WO2010082428A1 (en) * | 2009-01-19 | 2010-07-22 | コニカミノルタホールディングス株式会社 | Transparent electrode, method for producing same, and organic electroluminescent element |
| CN104073178A (en) * | 2013-03-29 | 2014-10-01 | 第一毛织株式会社 | Anisotropic conductive film including conductive adhesive layer and semiconductor device connected by the same |
| JP2015131429A (en) * | 2014-01-14 | 2015-07-23 | 東レ株式会社 | Conductive laminate, and touch panel and electronic paper using the same |
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| CN113196891A (en) * | 2018-12-27 | 2021-07-30 | 富士胶片株式会社 | Photosensitive transfer material, laminate, touch panel, method for manufacturing substrate with pattern, method for manufacturing circuit substrate, and method for manufacturing touch panel |
| CN113316743A (en) * | 2018-12-27 | 2021-08-27 | 富士胶片株式会社 | Conductive transfer material, method for manufacturing substrate having pattern, method for manufacturing circuit substrate, laminate, and touch panel |
| CN112321868A (en) * | 2019-07-18 | 2021-02-05 | 波音公司 | Removal of surface films and primers from composite substrates by use of co-cured paint films |
| CN112321868B (en) * | 2019-07-18 | 2023-04-21 | 波音公司 | Removal of surface films and primers from composite substrates by use of co-cured paint films |
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| CN107615408B (en) | 2019-07-02 |
| TWI693160B (en) | 2020-05-11 |
| JP6664396B2 (en) | 2020-03-13 |
| WO2017018427A1 (en) | 2017-02-02 |
| JPWO2017018427A1 (en) | 2018-05-24 |
| TW201718247A (en) | 2017-06-01 |
| KR102000956B1 (en) | 2019-07-17 |
| KR20170133483A (en) | 2017-12-05 |
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