CN110066411A - Kapton with and preparation method thereof - Google Patents
Kapton with and preparation method thereof Download PDFInfo
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- CN110066411A CN110066411A CN201910058635.XA CN201910058635A CN110066411A CN 110066411 A CN110066411 A CN 110066411A CN 201910058635 A CN201910058635 A CN 201910058635A CN 110066411 A CN110066411 A CN 110066411A
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- coating
- kapton
- base material
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- yellowing
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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
- B32B27/283—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 polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D125/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Coating compositions based on derivatives of such polymers
- C09D125/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D165/00—Coating compositions based on macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2425/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2425/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2465/00—Characterised by the use of macromolecular compounds obtained by reactions forming a carbon-to-carbon link in the main chain; Derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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Abstract
The present invention offer surface of polyimide base material is handled, reduce the Kapton of yellowing with and preparation method thereof.The Kapton, comprising: polyimide base material;And coating, it is coated on the polyimide base material, there is the yellowing YI less than 0Coating.The preparation method of the Kapton, comprising: in the step of polyimide base material applying coating forms composition, it is 0 coating forming material below and the solvent for dissolving the coating forming material that coating formation composition, which includes yellowing YI,;And dry coated coating forms composition, forms yellowing YI in polyimide base materialCoatingThe step of coating less than 0.
Description
Technical field
The present invention relates to a kind of Kapton with and preparation method thereof, more specifically, be related to by handle polyamides
The surface of imines substrate, reduce the Kapton of yellowing with and preparation method thereof.
Background technique
Recently, with the increase of the development of mobile device and popularity rate, display industry is had been greatly developed.It is moving
In the manufacture of dynamic equipment, it is stepped up the use of transparent and flexible organic material instead of existing inorganic material, therefore,
In the display of exploitation transparent configuration or the display of bendable deformable form.
As the organic material for replacing inorganic material, since polyimides (Polyimide) thermal characteristics and mechanical property are excellent
Show, therefore, for manufacturing the alignment films of display devices, the backboard of thin film transistor (TFT) (Thin Film Transistor:TFT)
(Backplane) etc..The thermal characteristics and mechanical property of known polyimides are due to passing through the main chain in polyimide polymer
The internal and charge-transfer complexation (charge transfer complex, CT-complex) that occurs between chain and chain and
The tatanic increase of chain increases with this intermolecular binding force.But polyimides usually has the structure of connection benzene, therefore,
Because of π-electronics resonance of these benzene, the energy level inside chain is lower, absorb long wavelength light guide cause polyimides present it is red or
The tendency of yellow.Therefore, in order to expand the purposes of polyimides, the optical characteristics of polyimides is needed to be improved, in particular, on replacing
Portion's cover glass when preparing substrate using polyimide substrate or with polyimides, needs to be improved the optical characteristics of polyimides.This
Outside, the phase difference characteristics of improvement Kapton be there is a perceived need to, to transmission of light of specific band etc..
It is known that in order to improve the optical characteristics of polyimides, using the monomer replaced by the big fluorine of electronegativity (F) or
Person, which uses, has such as-SO2, the monomers of the functional groups such as-O- prepares polyimides, thus, inhibit the covibration and electricity of benzene
Son transfer, improves the optical characteristics (transmission, turbidity, yellowing (Y1, b*) etc.) of polyimides.But these monomers compared to
Existing monomer is low in the presence of not only combined coefficient, moreover, using the polyimides of this monomer because of the free volume between chain and chain
The problem of (free volume) increases, and thermal characteristics and mechanical property are easily reduced.
Summary of the invention
The object of the present invention is to provide a kind of thermal characteristics and mechanical property for keeping polyimides, do not hinder transmission
And turbidity, further, it is possible to improve the optical characteristics of polyimides, more particularly to reduce the polyamides Asia of yellowing (Yellow Index)
Amine film with and preparation method thereof.
Other objects of the present invention are, provide a kind of structure for not changing Kapton, can also reduce yellowing
Kapton with and preparation method thereof.
To reach the purpose, a kind of Kapton of the present invention comprising: polyimide base material;And coating, it applies
The polyimide base material is spread on, there is negative yellowing (b*Coating< 0 or YICoating<0)。
Also, the preparation method of present invention offer Kapton comprising: in polyimide base material applying coating shape
The step of at composition, coating form composition and include yellowing (b*, YI) for 0 coating forming material below and for dissolving
The solvent of the coating forming material;And dry coated coating forms composition, forms yellowing in polyimide base material
(b*, YICoating) coating less than 0 the step of.
Invention effect
Kapton according to the present invention with and preparation method thereof, keep the thermal characteristics of polyimides and mechanical special
Property, does not hinder transmission and turbidity, further, it is possible to improve the optical characteristics of polyimides, more particularly to reduce yellowing (b*,
Yellow Index)。
Detailed description of the invention
Fig. 1 is the sectional view for showing the structure of Kapton of an embodiment according to the present invention.
Specific embodiment
In the following, present invention will be described in detail with reference to the accompanying.
Fig. 1 is the sectional view for showing the structure of Kapton of an embodiment according to the present invention.As shown in Figure 1,
Kapton of the invention, including polyimide base material 10 (substrate) and coating 20, coated under described gather
Imines substrate 10.
The polyimide base material 10 is thermal characteristics and the outstanding substrate prepared by polyimides of mechanical property
(substrate), dianhydride compound and diamine compound or diisocyanate cpd can be polymerize by usual way
Preparation.The dianhydride compound can lift pyromellitic dianhydride, benzophenone tetracarboxylic dianhydride, biphenyltetracarboxylic dianhydride, naphthalene tetracarboxylic acid
Dianhydride etc., however, it is not limited to this.Bis- (the 3- aminobenzenes of 4,4'- diaminodiphenyl ether, 1,3- can be lifted as the diamine compound
Oxygroup) benzene, bis- (3- amino-benzene oxygen) biphenyl of 4,4`-, 1,4- phenylenediamine and 1,3- phenylenediamine etc..The polyimide base material
10, according to polymeric composition for example with 1 to 15 yellowing, can specifically have 2 to 3 yellowing (Yellow Index, YI (b*)),
The more yellowing of the content of aromatic ring more increase in polymeric composition.
The polyimide base material 10 can be different according to the purposes of Kapton, have with a thickness of 50nm extremely
3000 μm, specially 100nm to 1000 μm, more specifically 1 μm to 100 μm of piece or film morphology.For example, polyamides of the invention
Imines film is used as the backboard of display devices thin film transistor (TFT) (Thin FilmTransistor:TFT)
(Backplane) when purposes, the polyimide base material 10 with a thickness of 1 μm to 30 μm, the Kapton is used as
When the cover glass purposes of display devices, the thickness of the polyimide base material 10 can be 10 μm to 500 μm.
The coating 20 is formed at the coating on the surface of the polyimide base material 10, have lower than 0 yellowing (b*,
YICoating).In this way, yellowing (b*Coating,YICoating) lower than the coating 20 of 0 (negative value) pass through the complementary color of coating 20 and polyimide base material 10
While effect keeps the total transmission of Kapton to spend, yellowing (Yellow Index, b*, YI) can reduce.The present invention
In, transmission (Total Transmittance:T.T) and yellowing can use transmission measuring instrument or chromascope measurement.
Also, refractive index (the n of the coating 20Coating) it is smaller than the refractive index (n of polyimide base material 10Polyimides), in this way,
If by the refractive index (n of coating 20Coating) it is kept less than the refractive index (n of polyimide base material 10Polyimides), then do not hinder transmission
(Transmittance) or while the optical characteristics such as turbidity (Haze) yellowing of Kapton entirety can, be reduced
(b*,YI).In the present invention, refractive index can use ellipsometer (Ellipsometer, Ellipsotechnology) measurement.
The coating 20 may include display chromaticity coordinates value L < 99.9, a* < -0.01, b* < 0 organic material and/or inorganic
Material, thus, it is possible to reduce the yellowing of Kapton entirety.The coating 20, which may include, does not hinder Kapton
The organic material and/or inorganic material of whole optical characteristics (transparency etc.) and physical characteristic (intensity, flexibility etc.).Example
Such as, organic pigment (pigment), organic dyestuff can be used alone or as a mixture as the organic material for forming the coating 20
(dye), electric conductive polymer (Conductive polymer) etc..
As the pigments or dyes, BILE PIGMENTS (Bile pigments), the red (Caput of Kapp spy can be lifted
Mortuum), bipseudoindoxyl dye (Indigo dye), phthalocyanine dye (Phthalocyanine dyes), pigment Violet 23 (Pigment
violet 23;Heterocyclic compound dioxazines (dioxazine) series), Tai Er purple (Tyrian purple;Brominated aubergine
Natural dye) etc., however, it is not limited to this.
As the electric conductive polymer, polyphenylene sulfide (Polyphenylene sulfide can be lifted;PPS), poly- furans
(Polyfuran;Pfu), polyisothianaphthene (Poly (isothianaphthene);PITN), poly- Azulene (Polyazulene;Paz),
Polyethylene dioxythiophene (Polyethylenedioxy thiophene;PEDOT), polyethylene dioxythiophene-polystyrolsulfon acid
(Polyethylenedioxythiophene-polystyrenesulfonate;PEDOT-PSS), polythiophene ethylene
(Polythienylenevinylene;) etc. PTV meet YICoating< 0 polymer, but not limited to this.
As the inorganic material for forming the coating 20, inorganic pigment or inorganic dyestuff can be used, it is, for example, possible to use
Navy blue (ultramarine, PB29 or Na8-10Al6Si6O24S2- 4), Persian it is blue (persian blue, Lapis-lazuli,
The aluminium pigments (Aluminum pigments) such as lazurite);It is cobalt blue (cobalt blue, pigment number PB28), sky blue
Cobalt pigments (the Cobalt such as (cerulean blue, pigment number PB35), cobaltous stannate (cobalt (II) stannate)
pigment);Egyptian blue (egyptian blue), Chinese indigo plant (han blue (BaCuSi4O10)), chessy copper (azurite: carbonic acid
Copper hydroxide (cupric carbonate hydroxide, (Cu3(CO3)2(OH)2)) etc. copper pigment (Copper
pigment);The iron pigment (Ironpigment) of Prussian blue (prussian blue, pigment number PB27) etc.;Yttrium indium manganese is blue
Manganese pigment such as (YInMn Blue) (Manganese pigment) etc..
The coating 20 can further comprise siloxanes (siloxane), silicone derivative, siloxane polymer (- Si-
The silicone compounds such as O-Si-).The silicone compounds do not cause to influence on optical characteristics, and play a part of to improve hardness,
As the concrete example of the silicone compounds, triethoxysilane (triethoxysilane), dimethyl diethoxy can be lifted
Silane (diethoxydimethylsilane), 3- aminopropyl triethoxysilane ((3-aminopropyl)
Triethoxysilane), tetramethylsilane (tetramethyl silicate) etc..When using the silicone compounds, phase
For 20 forming material of coating, 100 parts by weight, it preferably can be 1 parts by weight to 15 weights that content, which is 0.1 parts by weight to 30 parts by weight,
Measure part.When the usage amount of the silicone compounds is very few, it is insufficient to there is a problem of that hardness improves, silicone compounds contain
When measuring excessive, exists and the worry of cracking (Crack) occurs on surface.If using the coating 20 comprising the silicone compounds,
Then the hardness of coating 20 can be improved as more than such as 2H (pencil-lead hardness).
The thickness of the coating 20 can be according to the thickness and yellowing of the polyimide base material 10 and difference, thickness are usual
It is 10nm to 1000 μm, specially 50nm to 50 μm, more specifically 50nm to 2 μm, may be, for example, the thickness of about 300nm.It is preferred that
The thickness ratio of ground, coating 20 and polyimide base material 10 can be 1:0.01 to 0.2.Relative to the thickness of polyimide base material 10,
When the thickness of the coating 20 is excessively thin, the effect for reducing the yellowing of Kapton can be insufficient, when the coating 20
When thickness is excessively thick, the optical characteristics or physical characteristic of polyimides can be reduced.
At this point, the coating 20 can be single layer structure, can also have two layers or multilayer structure, in polyimide base material 10
One or both sides may include the coating 20.
By coating 20, the yellowing of polyimide base material 10 and Kapton poor (Δ YI) can for Δ YI (=
YIPolyimide base material-YIKapton) > 0, the yellowing poor (Δ YI) can change according to thickness, coating material of coating 20 etc..
Kapton of the invention includes coating 20, can be shown mist degree (Haze) < 2, total transmission degree (Total
Transmittance characteristic) > 90%.This is that Kapton of the invention by the inclusion of coating 20 not only shows reduction
The effect of yellowing, moreover, there is not the problem of reducing other optical characteristics i.e. mist degree, transmission, even if it can thus be appreciated that comprising
The problem of other optical characteristics in addition to yellowing reduce, will not occur for coating 20.
The hardness of the Kapton can be 1H to 7H, under the physics such as outer friction, impact and chemical shock
It is not susceptible to damage.
Also, mist degree (Haze) value of the polyimide base material 10 and Kapton preferably satisfies following mathematical expression
1。
[mathematical expression 1]
0.2 < (mist degree of Kapton)/(mist degree of polyimide base material) < 30
When being unsatisfactory for the mathematical expression 1, total turbidity of film is got higher, thus in the presence of cannot be by polyimides of the invention
The problem of materials'use of the film as display.
20 preferred display of coating, 1 Ω/ to 1G Ω/ electric conductivity.Electric conductivity, the present invention are shown by coating 20
Kapton can be used as transparent electrode in lower resistive segments (1 Ω/ to 1000 Ω/), the resistance more than it
(1000 Ω/~) have electrification to prevent effect, therefore, prevent film that can be applicable in Kapton of the invention as electrification.
Then, illustrate the preparation method of Kapton according to the present invention.
In order to prepare Kapton according to the present invention, it is included in 10 applying coating of polyimide base material and forms combination
Object and the step of drying.It includes coating forming material and for dissolving the coating forming material that the coating, which forms composition,
Solvent, may also include silicone compounds as needed.The coating forming material is 0 below as yellowing (YI, b*)
The organic material and/or inorganic material for constituting coating 20 as described above can be used in material.The solvent can dissolve coating
Forming material can select the material for not changing the physical property of polyimide base material 10 of lower part with no particular limitation.As described
The example of solvent can lift deionized water (DeIonized Water;DIW);Methanol (Methanol), ethyl alcohol (Ethanol), isopropanol
The alcohol such as (Isoprophyl alcohol), butanol (buthanol), amylalcohol (pentanol);1-Methyl-2-Pyrrolidone (1-
Methyl-2-pyrrolidinone;NMP), 1- ethyl-2-pyrrolidone (1-ethyl-2-pyrrolidinon;NEP),N,
N- dimethylpropionamide (N, N-Dimethylpropionamide;DMPA), N, N- diethylformamide (N, N-
Diethylformamide;DEF), N,N-dimethylformamide (N, N-Dimethylformamide;DMF), acetoacetyl two
Ethamine (Diethylacetamide;DEAC), DMAC N,N' dimethyl acetamide (N, N-Dimethylacetamide;DMAC) etc..?
The coating is formed in composition, the content of the coating forming material be 5ppm to 40 weight percent, preferably 50ppm extremely
5 weight percent, the content of the solvent be the remaining content of coating forming material, for example, 99.9995 weight percent extremely
60 weight percent, preferably 99.995 weight percent are to 95 weight percent.Also, as needed, the coating is formed
Composition can further comprise silicone compounds.Herein, when the content of the coating forming material is excessively lacked, exist to be formed
Coating 20 too long or that required thickness can not be formed the time required to coating 20.When the content of the coating forming material is excessively more
When, there are problems that coating 20 in homogeneous thickness can not be formed.
As the method for coating the coating formation composition, can select with no particular limitation with method known in this field,
It is, for example, possible to use dip-coating (dip), slot coated, silk-screen printing, spin coating, stencilization, spraying, ink jet printing, mayer sticks to apply
(Mayer Bar Coating), roller (roll) apply, spraying, flow (flow) painting, scraper method (doctor blade) and drop coating
(dispensing), hectographic printing, bat printing (pad printing), intaglio printing, flexographic printing (flexography), impress
The methods of (imprinting).In particular, mayer stick, which applies (Mayer Bar Coating), changes into 4,6,10 etc. for Bar#, therefore,
The coating density of complementary color layer increases or the thickness of complementary color layer increases and be reduced the effect of yellowing.The coating forms composition
Drying can be executed by usual ways such as heated-air drying, natural drying, heat dryings.If repeatedly it is described coating and it is dried
The coating 20 can be then formed as 2 layers or more of multilayered structure by journey.
According to the present invention, in the case where not changing the composition of polyimide base material 10, in the table of polyimide base material 10
Face, which forms coating 20, can keep the yellowing that Kapton is reduced while the optics and physical characteristic of Kapton
(Y1,b*).Kapton according to the present invention can be used for the alignment film film of liquid crystal display device, display devices film
Backboard (Backplane), the cover glass of display devices, display device of transistor (Thin Film Transistor:TFT)
The purposes of the multiplicity such as film, colour filter of the substrate of part, the phase-contrast film of liquid crystal display device, illumination and optical applications.
In the following, by specific embodiment, present invention be described in more detail.Following embodiment illustrates the present invention,
The invention is not limited to following embodiments.The measurement method used in following embodiment and comparative example is as follows.
(1) chromascope (visible ultraviolet light spectrophotometer, uv-visible absorption spectroscopy (UV- yellowing (b*, Y1): are used
Vis spectrometer), Cary 4000, Agilent Technologies) measurement.
(2) chromaticity coordinates value (L, a*, b*): with the electric color equipment of Japan, COH-400 measurement.
(3) transmission (total transmission degree: T.T): with transmission measuring instrument (Japan's electricity color equipment, COH-400) measurement (380
To the region 780nm).
(4) ellipsometer (Ellipsometer, Ellipsotechnology, model:SM642, wavelength refractive index (n): are used
Range (Wavelength range): 380nm to 1,000nm, UV option (UVOption): 240nm to 1,000nm) measurement
(5) turbidity (Haze): with the electric color equipment of Japan, COH-400 measurement.
(6) electric conductivity: with 4 surface resistivity testers (4-Point Surface Resistivity Meter)
(EDTM, RC2175) measurement.
(7) hardness: pencil-lead hardometer is used
[comparative example 1 and embodiment 1]The preparation of Kapton
Polyethylene dioxythiophene-polystyrene sulphur of 0.5 parts by weight of dissolution in the deionized water (DIW) of 95.5 parts by weight
Sour (PEDOT-PSS) and prepared coating and formed composition.With turbidity shown in following table 1 (Haze), yellowing (b*, YI)
And transmission (Total Transmittance:T.T) with a thickness of 10 μm of polyimide base material surface, utilize stepping for Bar#4
Your stick applies (Mayer Bar Coating) and has been evenly coated with coating formation composition.Dry coated coating forms combination
Object forms coating and is prepared for Kapton.The turbidity (Haze) of the prepared Kapton of measurement, yellowing (b*,
YI) and transmission (T.T), the difference with the polyimide base material of not formed cated comparative example 1 is illustrated together in table 1.
Also, refractive index (the n of polyimide base material and Kapton according to the embodiment 1 is illustrated in table 2Polyimides、
nCoating), the mist degree (Haze) of coating 20, total transmission degree (Total Transmittance), chromaticity coordinates value (L, a, b) and conduction
Property.
[comparative example 2 and embodiment 2]The preparation of Kapton
In addition to using the polyimide base material with turbidity, yellowing shown in following table 1 and transmission, use Bar#6's
Except mayer stick applies, it is prepared for Kapton in the same manner as in Example 1.The prepared Kapton of measurement
Turbidity, yellowing and transmission, illustrate the difference with not formed cated Kapton substrate together in table 1.And
And refractive index (the n of polyimide base material and Kapton according to the embodiment 2 is illustrated in table 2Polyimides、
nCoating), the mist degree (Haze) of coating 20, total transmission degree (Total Transmittance), chromaticity coordinates value (L, a*, b*) and lead
Electrically.
[comparative example 3 and embodiment 3]The preparation of Kapton
In addition to using the polyimide base material with turbidity, yellowing shown in following table 1 and transmission, use Bar#10's
Except mayer stick applies, it is prepared for Kapton in the same manner as in Example 1.The prepared Kapton of measurement
Turbidity, yellowing and transmission, illustrate the difference with not formed cated Kapton substrate together in table 1.And
And refractive index (the n of polyimide base material and Kapton according to the embodiment 3 is illustrated in table 2Polyimides、nCoating)、
Mist degree (Haze), total transmission degree (Total Transmittance), chromaticity coordinates value (L, a*, b*) and the electric conductivity of coating 20.
[embodiment a, b, c]The preparation of Kapton
In order to obtain polysiloxane compound, mix the tetraethoxysilanes (TEOS) of 15 parts by weight, 26 parts by weight it is different
Propyl alcohol (IPA), the water of 53 parts by weight, 5.0% acetic acid dilute solution (aqueous solution) of 1 parts by weight and the silicon table of 0.1 parts by weight
Face activating agent has carried out colloidal sol under the conditions of 25 DEG C of temperature and has reacted 24 hours.In the deionized water (DIW) of 75.5 parts by weight
Dissolve the polysiloxane compound of 20 parts by weight, polyethylene dioxythiophene-polystyrolsulfon acid (PEDOT- of 0.5 parts by weight
PSS) prepare coating and form composition.It is sub- with turbidity, yellowing shown in following table 1 and the polyamides of transmission in addition to using
Amido material, the embodiment a are applied using the mayer stick of Bar#10, and embodiment b is applied using the mayer stick of Bar#6, and embodiment c is used
Except the mayer stick of Bar#10 applies, it is prepared for Kapton in the same manner as in Example 1.The prepared polyamides of measurement
Turbidity, yellowing and the transmission of imines film illustrate and not formed cated Kapton substrate together in table 1
Difference.
[table 1]
Become 4,6,10 according to Bar# as shown in Table 1, the thickness of coating increases, and Y1 becomes lower tendency.Also, it can
Even if being also able to maintain the optical characteristics such as transmission, mist degree to confirm that Y1 is lower.Exist known to i.e. and the same of yellowing is reduced by coating
When do not damage the effects of other optical characteristics.
In addition, the polyamides of the more embodiment a of content of polysiloxane compound known to comparing embodiment 1 and embodiment a
The hardness of imines film is higher, when to requiring the field of high rigidity using Kapton of the invention, can pass through poly- silicon oxygen
Hydride compounds reach high rigidity.
[comparative example 4 and 5]Adjust the thickness of coating
In addition to using the polyimide base material with turbidity, yellowing shown in following table 1 and transmission, Bar#2 (ratio is used
Compared with example 4) and Bar#20 (comparative example 5) mayer stick apply except, it is thin to be prepared for polyimides in the same manner as in Example 1
Film.Turbidity, yellowing and the transmission of the prepared Kapton of measurement.Polyimide base material and polyamides are illustrated in table 2
Refractive index (the n of imines filmPolyimides、nCoating), the mist degree (Haze) of coating 20, total transmission degree (Total Transmittance),
Chromaticity coordinates value (L, a*, b*) and electric conductivity.
[table 2]
The size (Bar size) for increasing coating can be confirmed by the table 1 and table 2, then whole yellowing is lower.Mean
The thickness of coating when thickeing, transmission is kept or slightly declines, but can larger adjust yellowing.On the contrary, such as comparative example
4, when the thickness of coating is excessively thin, yellowing cannot be caused to influence because the effect of the complementary color of coating is insufficient, therefore cannot get it
The effect that value is lower, if comparative example 5 excessively emphasizes that the thickness of complementary color effect or coating thickens when the thickness of coating is blocked up, because
This generates the phenomenon that total transmission degree is lower.
[embodiment 4,5,6 and comparative example 6,7]The preparation of Kapton
Composition is formed using coating identical with embodiment a, b and c, and is prepared using method same as Example 1
Kapton, at this point, keeping the thickness of coating mutually different, measuring and comparing the variation of its physical property.Institute is illustrated in table 3
The difference of the physical property of measurement.
[table 3]
If the analysis result of table 3 is it is found that the thickness with coating increases, the hardness of Kapton is improved.On the contrary, than
In the case where compared with example 6, effect that hardness improves cannot be shown because the thickness of coating is thin, in the case where comparative example 7, the thickness of coating
When degree is thick, because occur to be cracked (crack) due to coating fall off from polyimide base material the problem of, be unable to measure hardness.
[comparative example 7 and 8]The preparation of Kapton
In addition to using the polyimide base material with turbidity shown in following table 4 and 5, yellowing and transmission, and utilizes and step
Your stick is coated in polyimide base material and is respectively coated except the chromatic photoresist that methylenum careuleum and blue is presented, with same as Example 1
Method is prepared for Kapton.Methylenum careuleum used in embodiment 7 is the deionized water mixing in 99.99 parts by weight
After the Dynol 607 of the methylenum careuleum of 0.005 parts by weight and 0.005 parts by weight, it is coated onto polyimide base material (table 4),
Chromatic photoresist used in embodiment 8 is the chromatic photoresist product DJB-5000 that east is learned into generation beautification, in the PGMEA of 98 parts by weight
The DJB-5000 of 2 parts by weight is diluted, polyimide base material (table 5) is then coated onto.Then, the micro-wave oven at 80 DEG C is dry
The optical characteristics of comparative analysis coating front and back after 2 minutes.Table 4 and 5 illustrates mist degree (Haze), the total transmission degree of coating 20
(Total Transmittance), chromaticity coordinates value (L, a*, b*) and electric conductivity.
[table 4]
[table 5]
It, can be with by coating methylenum careuleum or chromatic photoresist DJB-5000 in polyimide base material as shown in above-mentioned table 4 and table 5
It reduces Y1 (b*).Methylenum careuleum and chromatic photoresist DJB-5000 are to meet L < 99.9, and a* < -0.01, b* < 0 substance passes through
Meet L < 99.9, a* < condition of -0.01, b* < 0 organic material or nothing in polyimide base material coating known to the analysis result
When machine material, the Y1 (b*) of polyimide base material can be reduced.
Claims (11)
1. a kind of Kapton, wherein include:
Polyimide base material;And
Coating is coated on the polyimide base material, has negative yellowing, wherein b*Coating< 0 or YICoating<0。
2. Kapton according to claim 1, wherein the refractive index n of the coatingCoatingLess than polyimide-based
The refractive index n of materialPolyimides。
3. Kapton according to claim 1, wherein the coating include chromaticity coordinates be L < 99.9, a* <-
0.01, the organic material or inorganic material of b* < 0.
4. Kapton according to claim 3, wherein the organic material is selected from by organic pigment, organic
The substance in group that dyestuff, macromolecule, electric conductive polymer and these mixture form.
5. Kapton according to claim 3, wherein the inorganic material be selected from by aluminium pigment, cobalt pigment,
The inorganic substances in group that copper pigment, iron pigment, manganese pigment and these mixture form.
6. Kapton according to claim 1, wherein the coating further comprises selected from by siloxanes, silicon
Silicone compounds in the group of siloxane derivative, siloxane polymer and these mixture composition.
7. Kapton according to claim 1, wherein the polyimide base material with a thickness of 50nm to 3000
μm, the coating with a thickness of 10nm to 1000 μm.
8. Kapton according to claim 1, wherein coating is 1:0.01 to the thickness ratio of polyimide base material
To 0.2.
9. Kapton according to claim 1, wherein mist degree<2, total transmission degree>90%.
10. Kapton according to claim 6, wherein the hardness of the Kapton is 1H to 7H.
11. Kapton according to claim 1, wherein the coating shows 1 Ω/ to 1G Ω/ conduction
Property.
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CN112574453A (en) * | 2019-09-30 | 2021-03-30 | Sk新技术株式会社 | Antistatic polyimide base film and flexible display panel using the same |
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