CN105814644B - conductive composition for forming back electrode of liquid crystal display device - Google Patents
conductive composition for forming back electrode of liquid crystal display device Download PDFInfo
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- CN105814644B CN105814644B CN201480067695.3A CN201480067695A CN105814644B CN 105814644 B CN105814644 B CN 105814644B CN 201480067695 A CN201480067695 A CN 201480067695A CN 105814644 B CN105814644 B CN 105814644B
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1343—Electrodes
- G02F1/13439—Electrodes characterised by their electrical, optical, physical properties; materials therefor; method of making
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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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
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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
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2201/00—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00
- G02F2201/12—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00 electrode
- G02F2201/121—Constructional arrangements not provided for in groups G02F1/00 - G02F7/00 electrode common or background
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- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F2202/00—Materials and properties
- G02F2202/22—Antistatic materials or arrangements
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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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
- H01B1/12—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances organic substances
- H01B1/124—Intrinsically conductive polymers
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Abstract
The present invention relates to a conductive composition for forming a back electrode of a liquid crystal display device. Specifically, the present invention can provide an antistatic back electrode which has excellent transmittance and surface hardness in a liquid crystal display device and improved reliability of a coating film by adding a conductive polymer and a specific thermal acid generator to a composition obtained by a sol-gel reaction of a silane coupling agent to optimize the dispersibility of the conductive polymer in the composition. In particular, the present invention can ensure reliability to improve hardness and reduce surface resistance change with time after coating.
Description
Technical field
The present invention relates to a kind of electric conductivity groups for being used to form liquid crystal display device backplate of film excellent reliability
Close object.
Background technology
In electrode formation technology, backplate effect is shielded from the quiet of outside especially in liquid crystal display device
Electricity.
Past is used as the ITO of backplate (Korean granted patent the 10-0603826th) material in liquid crystal display device
(Indium-tin-oxide, indium tin oxide) or IZO (Indium-Zinc-oxide, indium-zinc oxide) need to carry out vacuum
Process is deposited, for the characteristic of these backing electrode materials, although resistance and case hardness are outstanding, light transmittance is poor.
In view of the problem for occurring indium resource exhaustion recently, for replacing the various transparent electrode materials of ITO to be developed into
Subject under discussion.However, present situation is many transparent electrode materials for being developed so far (for example, electroconductive polymer or comprising gold
The inorganic conductive composition etc. of category or metal oxide) unsatisfactory result is still shown in terms of light transmittance.
Using the film of electroconductive polymer, although having outstanding light transmittance, sheet resistance is with as electrode
Increase during forming material, therefore the problem of reliability reduction occurs.
Invention content
Technical problem
In order to solve the above-mentioned technical problem, the object of the present invention is to provide one kind when forming electrode, is especially being formed
When the backplate of liquid crystal display device, the backplate that the liquid crystal display device of the reliability under film state can be improved is formed
The backplate of liquid crystal display device with conductive composition and using the conductive composition.
Coating, hardness can be improved and reduces film to the maximum extent in addition, another object of the present invention is to provide one kind
With the method for time increased sheet resistance after formation.
Technical solution
The present invention provides a kind of backplate formation of liquid crystal display device：
The silane coupling agent of 5 parts by weight to 40 parts by weight；
The solvent of 50 parts by weight to 90 parts by weight；
The hydrochloric acid or acetic acid dilute solution of 0.1 parts by weight to 10.0 parts by weight；
The conductive-polymer solution of 5 parts by weight to 40 parts by weight, the solid with 0.1 weight % to 5.0 weight %
Object；And
The acid agent of 0.001 parts by weight to 1.0 parts by weight.
The acid agent can be selected from amine sealing end (Amine blocked), covalent bond sealing end (covalent
Blocked), the heat production of metal sealing end (metal blocked) and quaternary ammonium sealing end (Quaternary Ammonium Blocked)
At least one of sour agent (thermal acid generator).
In addition, the acid agent can selected from dodecyl benzene sulfonic acid, p- toluenesulfonic acid, trifluoromethanesulfonic acid and its be spread out
At least one of biology.
The solvent is preferably comprised selected from i) water, ii) alcohol compound and iii) dihydroxypropane single-ether, dimethyl formyl
At least one in amine, acetylacetone,2,4-pentanedione, 1- methyl -2- pyrrole networks alkanone, butyrone (dipropylketone) and ethyl lactate
Kind solvent.
The solid content of its electroconductive polymer of conductive-polymer solution, which is 0.1 weight %, to 5 weight % and can wrap
Containing 95 weight % to the solvent of 99.9 weight %.
The electroconductive polymer at least one of may include selected from polyaniline, polypyrrole, polythiophene and its derivative,
It preferably comprises poly- (3,4- ethylenedioxy thiophenes).
In addition, the electroconductive polymer preferably also includes selected from dodecyl benzene sulfonic acid, toluenesulfonic acid, camphorsulfonic acid
(camphorsulfonic acid), benzene sulfonic acid, hydrochloric acid, styrene sulfonic acid (styrenesulfonic Acid), 2- acryloyls
Amido -2- methyl propane sulfonic acids (2-acrylamido-2-methylpropanesulfonic acid), they salt compound,
2- sulfosuccinate ester salts (2-sulfosuccinate ester salt), 5- sulfo isophthalate sodium salts (5-
Sulfoisophthalic acid sodium salt), Sodium Dimethyl Isophthalate-5-sulfonate (dimethyl-5-
Sodium sulfoisophthalate), bis- (beta-hydroxyethyl ester) -5- sodium sulfonates (the 5-sodium sulfo- of M-phthalic acid
Bis (β-hydroxyethyl) isophthalate) and at least one of poly- (4- styrene sulfonates) dopant.It is described to lead
Electrical macromolecule preferably comprises poly- (4- styrene sulfonates) as dopant.
It is preferable to use poly- (3,4- ethylenedioxy thiophenes) for the electroconductive polymer:Poly- (4- styrene sulfonates)
(PEDOT:PSS)。
The silane coupling agent can be selected from the alkoxyl silicone alkanes (alkyloxy with C1 to C20 alkyl
Silane), amino silicone alkanes (amino silane), vinyl silanes class (vinyl silane), epoxy radicals silicone hydride class
(epoxy silane), methacryloxypropyl silane class (methacryloxy silane), isocyanatosilanes class
At least one of (isocyanate silane) and fluorine-based silane class (fluoro silane).
In addition, according to the present invention, relative to the total composition of 100 parts by weight, it also may include 0.1 parts by weight to 1.0
The surfactant of parts by weight.
In addition, the conductive composition relative to 100 parts by weight, also may include 0.1 parts by weight to 30 parts by weight
Selected from least one of polyacrylic resin, polyurethane resin, epoxy resin and polyester resin adhesive resin.
In addition, the present invention provides a kind of liquid crystal display device face electrode formed with the conductive composition.
Advantageous effect
Overleaf electrode thus is dried with having used specific thermal acid generator (TAG) in conductive composition the present invention after coating
Acid can be further generated when roasting so that unreacted silane compound (for example, TEOS) further hydrolyzes, and has so as to be formed
The film of the degree of cross linking between stronger silane coupling agent.It is combined with electric conductivity moreover, the present invention can optimize backplate
The dispersibility of electroconductive polymer in object.Therefore, (especially, IPS, FFS etc. are lateral in liquid crystal display device (LCD) by the present invention
The liquid crystal display device of Electric Field Mode) in can reduce to form film after with the time increased sheet resistance, that is, improve can
By property.
Specific implementation mode
In the following, the present invention will be described in detail.
Preferred embodiment according to the present invention provides a kind of backplate formation electric conductivity group of liquid crystal display device
Object is closed, which includes：The silane coupling agent of 5 parts by weight to 40 parts by weight；50 parts by weight are molten to 90 parts by weight
Agent；The hydrochloric acid or acetic acid dilute solution of 0.1 parts by weight to 10.0 parts by weight；The electroconductive polymer of 5 parts by weight to 40 parts by weight
Solution, the solid content with 0.1 weight % to 5.0 weight %；And 0.001 parts by weight to 1.0 parts by weight acid agent.
Overleaf electrode formation can be improved with acid agent TAG has been used in conductive composition to have the present invention
The advantages of reliability of backplate film.This conductive composition can utilize silane coupling agent precursor composition, electric conductivity
Polymer Solution and specific acid agent.
Silane coupling agent of the silane coupling agent precursor composition comprising 5 parts by weight to 40 parts by weight, 50 parts by weight are extremely
The solvent of 90 parts by weight, the hydrochloric acid of 0.1 parts by weight to 10.0 parts by weight or acetic acid dilute solution, pass through their sol-gel
The silane coupling agent precursor composition is obtained by the reaction.Moreover, the conductive-polymer solution refers to utilizing electric conductivity high score
Solid content obtained from son and solvent is the solution of 0.1 weight % to 5.0 weight %.
In addition, it is a feature of the present invention that substantially increasing the reliable of conductive composition by using specific acid agent
Property.The acid agent is using the material for generating acid under heat effect, and it is preferable to use amido sealing ends when material is added for the acid agent
Thermal acid generator.Moreover, the range of choice of acid agent is wide in the present invention, can be used from metal ion content be controlled as 2ppm with
Under thermal acid generator (TAG) series CXC grades (CXC Grade) that 2ppm or more is controlled as to metal ion content production it is sour
Agent.Preferably, the acid agent uses the material that acid can be generated at a temperature of 100 DEG C to 150 DEG C of soft roasting (soft bake).
The acid agent can be selected from amine sealing end (Amine blocked), covalent bond sealing end (covalent
Blocked), the heat production of metal sealing end (metal blocked) and quaternary ammonium sealing end (Quaternary Ammonium Blocked)
At least one of sour agent (thermal acid generator).It can be used as the acid agent dissolvable or dissolved
Product in solvent used in the present invention (such as IPA, PGME or water etc.).
In addition, the acid agent, which can be used, is selected from dodecyl benzene sulfonic acid (Dodecylbenzene sulfonic
Acid), p- toluenesulfonic acid (p-Toluene sulfonic acid), trifluoromethanesulfonic acid (Trifluoromethane
At least one of sulfonic acid) and its derivative.King inderstries can be used public as the acid agent
All CXC and TAG grades (TAG Grade) product of department.
At this point, for the conductive composition, when needing to be improved reliability, the group only with known electrodes composition material
Its characteristic cannot be coordinated by dividing, therefore should further use the specific acid agent i.e. TAG of the present invention.
In addition, when using TAG based on solvent composition or electroconductive polymer characteristic, the modification of material may be very serious,
Therefore possibly can not be suitable for the component not optimized.For example, the back of the body that the TAG possibly can not be suitable for not optimized
In the electrode material of face.But specific acid agent used in the present invention is included in the component of optimization, therefore has synergistic effect,
Great role can be played to improving reliability.
In addition, the silane coupling agent plays the effect for the dispersibility for improving electroconductive polymer in the composition.It is described
Alkoxyl silicone alkanes, amino silicone alkanes, vinyl silanes class, epoxy radicals silicone hydride class, methacryl can be used in silane coupling agent
Oxysilane class, isocyanatosilanes class, fluorine-based silane class etc..More specifically, having TEOS (tetrems as the silane coupling agent
Oxysilane), vinyltriethoxysilane, vinyltrimethoxysilane, vinyl three (beta-methoxy ethyoxyl) silane,
γ-(methacryloxy) propyl trimethoxy silicane, β-(3,4- epoxycyclohexyls) ethyl trimethoxy silane, γ-ring
The third oxygen propyl trimethoxy silicane of oxygen (γ-glycidoxypropyltrimethoxysilane), γ-mercapto propyl trimethoxy
Silane (γ-mercaptopropyltrimethoxysilane), gamma-aminopropyl-triethoxy-silane, N- β-(aminoethyl)-
γ-aminopropyltrimethoxysilane, γ-ureidopropyltriethoxysilane (γ-
Ureidopropyltriethoxysilane), phenyl triethoxysilane, methyltriethoxysilane, methyl trimethoxy oxygroup silicon
Alkane, polyethylene oxide modified silane monomer, poly- methylethoxy radical siloxane (polymethylethoxy siloxane), pregnancy
Base disilazane (hexamethyldisilazane) etc., can select at least one of they.
Relative to total conductive composition, it is preferable to use 5 parts by weight for the silane coupling agent to 40 parts by weight, more preferably makes
With 10 parts by weight to 30 parts by weight.If the content easy tos produce when forming coating caused by phase separation less than 5 parts by weight
Surface spot and case hardness may reduce.If the content is more than 40 parts by weight, resistance is got higher and composition
Stability declines.
In addition, solvent used in the present invention may include selected from i) water, ii) alcohol compound and iii) propylene glycol list second
At least one of ether, dimethylformamide, acetylacetone,2,4-pentanedione, 1- methyl -2- pyrrole networks alkanone, butyrone and ethyl lactate are molten
Agent.
That is, solvent used in the present invention is water, alcohol compound, water comes as the TEOS primary solvents hydrolyzed
Include 10 parts by weight to 50 parts by weight using and relative to total solvent content, alcohol compound mainly uses monohydric alcohol and dihydric alcohol
And it may include the alcohol that the boiling point of the C1 to C10 of 10 parts by weight to 50 parts by weight is 50 DEG C to 200 DEG C relative to total solvent content.Alcohol
Come as the solvent for making hydrolysis and esterification steadily carry out the stability to keep sol particles after TEOS reactions
It uses.Moreover, in order to make coating be optimized, can use methoxyl group, ethyoxyl that boiling point is 100 degree~160 degree or so,
Propyl ethyl alcohol (propylethanol) class solvent and it may include 10 parts by weight to 50 parts by weight relative to total solvent content.
The alcohol compound includes alcohol (alcohol), glycol (diol) or polyalcohol (polyol), be can be used for example
Selected from methanol, ethyl alcohol, isopropanol, ethylene glycol, butanediol, neopentyl glycol, 1,3- pentanediols, 1,4 cyclohexane dimethanol, two sweet
Alcohol, polyethylene glycol, polybutylene glycol (polybutylene glycol), dihydroxy methylpropane (dimethylol
Propane), at least one of trimethylolpropane and their derivative.
In addition, the present invention can further use chloroform, dichloromethane, tetrachloro-ethylene, three as desired as solvent
The halogenations species such as vinyl chloride, Bromofume, dibromopropane；N-Methyl pyrrolidone, dimethyl sulfoxide (DMSO)；Triethylamine, tri-n-butylamine, three
Octylame；Cresols etc..
The solvent can eliminate the coating inhomogeneities caused by the difference of the volatility generated when the coating of surface, Er Qieti
The density of high TEOS films, to play the role of that sheet resistance reliability can be increased.
Relative to total composition, it includes in the composition, but preferably with conductive composition that the solvent, which can be used as surplus,
Total weight subject to can be used 50 parts by weight to 90 parts by weight.
The hydrochloric acid or acetic acid dilute solution can be used, it is solidifying with the colloidal sol-of hydrolysis to be carried out under acid atmosphere
Glue reacts.The hydrochloric acid or acetic acid dilute solution can use water-reducible 0.1% to 10% hydrochloric acid or acetic acid dilute solution,
But not limited to this.Relative to total conductive composition, the hydrochloric acid or acetic acid dilute solution can use 0.1 parts by weight to 10.0
Parts by weight.
In addition, using conductive-polymer solution to prepare the conductive composition of the present invention, as described above preferably
Solid content is 0.1 weight % to 5.0 weight %.At this point, if in the conductive-polymer solution solid content content
Less than 0.1 weight %, then there are problems that losing electrode effect, and if it exceeds 5 weight %, then can promote with before TEOS colloidal sols
The aggregation (aggregation) of body composition and the gelation of conductive-polymer solution itself, to be difficult to prepare.
Relative to total conductive composition, the conductive-polymer solution uses 5 parts by weight to 40 parts by weight.If institute
The content of conductive-polymer solution is stated less than 5 parts by weight, then resistance is drastically got higher, and if it exceeds 40 parts by weight, then light transmission
Degree reduces and is difficult to keep the stability of dispersing characteristic and composition.
The solid content of this its electroconductive polymer of conductive-polymer solution is that 0.1 weight % to 5 weight % and includes
The solvent of 95 weight % to 99.9 weight % or the solid content of electroconductive polymer can be 5 weight % to 60 weight % and packet
Containing 40 weight % to the solvent of 95 weight %.
In addition, the electroconductive polymer used in the present invention is organic matter, and the composition band of the present invention is made to lead
Electrical base substance.
In order to make the electroconductive polymer is conductive to need doping process, and the method for implementing this process has system
At chemical doping is carried out after non-conductive powder type or form of film to it or mixes non-conductive powder and dopant
After be dissolved in organic solvent with conductive.Wherein, the method using the dopant can be used in the present invention.Therefore, institute
Electroconductive polymer is stated it is preferable to use the form mixed with dopant, i.e. dopant is doped to the high score in electroconductive polymer
Son.
For example, substantially polyaniline, polypyrrole, polythiophene and its derivative, monomer (benzene can be used in electroconductive polymer
Amine, pyrroles, thiophene) derivative as macromolecule made of monomer polymerization etc..At this point, using the derivative of the monomer as single
Poly- (the 3,4- ethylenes that the derivative i.e. 3,4- ethylenedioxy thiophenes of for example useful thiophene of the macromolecule that body is polymerized are polymerized
Dioxy thiophene) (poly (3,4-ethylenedioxythiophen), PEDOT).The PEDOT stablizes in an atmosphere and room temperature
Conductivity is higher than other macromolecules.
In the present invention, can with also include outside this electroconductive polymer selected from dodecyl benzene sulfonic acid, toluenesulfonic acid,
Camphorsulfonic acid, benzene sulfonic acid, hydrochloric acid, styrene sulfonic acid, 2- acrylamide-2-methylpro panesulfonic acids, their salt compound, 2- sulphurs
Bis- (the β-hydroxyl of base succinate salt, 5- sulfo isophthalate sodium salts, Sodium Dimethyl Isophthalate-5-sulfonate, M-phthalic acid
Ethyl ester) in -5- sodium sulfonates and poly- (4- styrene sulfonates) (PSS, poly (4-styrene sulfonate)) at least one
The form of mixtures of kind dopant is used to prepare composition for electrode formation.Moreover, it is preferable to use poly- (4- styrene sulphurs for dopant
Hydrochlorate).
Therefore, the present invention can use in the PEDOT when preparing electrode formation conductive composition and adulterate PSS
PEDOT-PSS (be also known as PEDOT:PSS), PEDOT-PSS is good as electrode or antistatic material coating, and interface is special
Property and caking property are also outstanding.
Moreover, according to the present invention, it, can also be comprising 0.1 parts by weight extremely relative to total conductive composition of 100 parts by weight
The surfactant of 1.0 parts by weight.The silicon surface active agent can be used, but kinds of surfactants is without being limited thereto.
In addition, the present invention is as needed, relative to the conductive composition of 100 parts by weight, it also may include 0.1 weight
Part is to 30 parts by weight selected from the bonding of at least one of polyacrylic resin, polyurethane resin, epoxy resin and polyester resin
Agent resin.
In addition, the present invention when preparing conductive composition, is not used as being added to the back of the body by being added at one time in the past
Face electrode forms the mode prepared with each ingredient (for example, the substances such as electroconductive polymer and TEOS) in component, but
After silane coupling agent (TEOS) is carried out sol gel reaction at high temperature and prepares precursor solution, it is mixed into electroconductive polymer
And acid agent, to prepare electrode formation conductive composition.Electrode formation electric conductivity group is prepared in the following, further illustrating
Close each step of object.
Prepare silane coupling agent precursor composition
In the process that this step carries out preparing precursor by the sol gel reaction of silane coupling agent.
May include in electrode formation conductive composition its final component of the present invention electroconductive polymer, dopant,
Silane coupling agent, acid agent and solvent, and the process for preparing precursor solution using silane coupling agent is carried out in the present invention, so as to lead
Conductive composition has the component.
That is, mode of the present invention is different from existing preparation method, prepared first by silane coupled
The sol gel reaction of agent after obtained precursor, it is mixed with electroconductive polymer, therefore can provide a kind of electricity
Pole formation conductive composition, outstanding case hardness and time-based reliability area are met under membrane stage, may be used also
To show the performance more outstanding than previous general room temperature preparation method.
In particular, the side for polymerizeing to prepare of the electroconductive polymer and TEOS different from the past by under normal temperature condition
Formula, the backplate formation prepared using the sol gel reaction by silane coupling agent in of the invention are combined with electric conductivity
The precursor of object.Therefore, the crosslinking degree of film in finally obtained backplate itself can be improved in the present invention, and passes through thus band
The effect come improves hardness and increases the superficial density of the electroconductive polymer with opposite nature, so as to reduce conduction
The high molecular usage amount of property, can also improve the reliability because Relatively centralized is reduced in the electroconductive polymer on surface.
It is known that the sol gel reaction is commonly used for the method for preparing inorganic material, this method is by making metal
Alkoxide is hydrolyzed under alcohols solvent-and polycondensation carrys out the ceramic powders of synthesis of metal oxide or hydroxide form.In addition, making
For the sol gel reaction, it has been known that there is TEOS sol-gel methods.Therefore, in the present invention from this starting point, silane is being carried out
It when the sol gel reaction of coupling agent, is not reacted not instead of at normal temperatures, colloidal sol-is carried out at a temperature of higher than room temperature
Gel reaction forms bridging property when film so as to improve, and can improve hardness on metal.That is, in this hair
Pass through the knot of the silane coupling agent precursor composition and aftermentioned electroconductive polymer that are obtained by the sol gel reaction in bright
It closes to improve high molecular dispersibility and raising mechanical strength, while hot property can also be improved, be suitable for provide
The effect of electronic material.The performance of composition organic-inorganic hybrid composite material may be implemented in this composition, it may thereby be ensured that nothing
The rigidity and the outstanding property of heat of machine object, it may also be ensured that the performances such as the flexibility of polymer and processability.Moreover, of the invention
The result of progress reliability assessment, which is shown, after formation film ensures reliability and raising hardness.
This sol gel reaction is solidifying by the colloidal sol-that silane coupling agent and solvent are carried out to certain time at high temperature
Glue reacts to prepare silane coupling agent precursor solution (for example, TEOS sol solutions).
At this point, the high temperature referred in the present invention refers to the temperature higher than room temperature.Preferably, the sol gel reaction exists
It is carried out 1 hour to 5 hours at a temperature of 40 DEG C to 70 DEG C.Most preferably, the sol gel reaction at a temperature of 50 DEG C into
Row 3 hours.If the sol gel reaction carries out at a temperature of less than 40 DEG C, the hydrolysis of TEOS may result in
(Hydrolysis) degree reduce, and the speed of the condensation reaction incidentally generated may than hydrolyze it is fast, therefore hardness and
It is possible that problem in terms of the growth of TEOS sol particles.Moreover, if sol gel reaction at a temperature of higher than 70 DEG C into
Row, although then can more reliably be reacted in terms of hydrolysis, due to the TEOS colloidal sol grains through hydrolysis and condensation reaction after this
The growth rate of son is too fast, it is possible that the problem of quick-gelatinizing (Gellation).
In addition, in the step of preparing silane coupling agent precursor composition, carried out instead after surfactant can also be added
It answers.
Preferably, in the step of preparing silane coupling agent precursor composition, the silane relative to 100 parts by weight is even
Join agent precursor composition, 0.1 parts by weight can also be added to the surfactant of 1.0 parts by weight.
The preparation of backplate formation conductive composition
In the present invention, after preparing silane coupling agent precursor composition by above-mentioned method, addition has 0.1 weight %
To the conductive-polymer solution and 0.001 parts by weight to 1.0 weights of 5 parts by weight to 40 parts by weight of the solid content of 5.0 weight %
The acid agent of amount part is mixed, and the backplate formation conductive composition of liquid crystal display device is finally made.
In the method, the mixing of silane coupling agent precursor composition and electroconductive polymer can be at 10 DEG C to 40 DEG C
At a temperature of carry out.
The backplate formation of the final liquid crystal display device prepared according to the method described above may include with conductive composition：
The conductive-polymer solution of 5 parts by weight to 40 parts by weight, the solid content with 0.1 weight % to 5.0 weight %；3 weight
Part to 30 parts by weight silane coupling agent；The solvent of 20 parts by weight to 60 parts by weight；And 0.001 parts by weight to 1.0 parts by weight
Acid agent.
In final electrode formation conductive composition, if the content of the electroconductive polymer less than 5 parts by weight,
Then resistance is drastically got higher, and if it exceeds 40 parts by weight, then light transmittance reduces and be difficult to keep the steady of dispersing characteristic and composition
It is qualitative.
In addition, the final composition for electrode formation relative to the present invention, the silane coupling agent preferably comprise 3 parts by weight
More preferably include 5 parts by weight to 20 parts by weight to 30 parts by weight.If the content is held less than 3 parts by weight when forming coating
Being also easy to produce surface spot and case hardness caused by phase separation may reduce, and if it exceeds 30 parts by weight, then resistance change
High and composition stability declines.
Relative to the final composition for electrode formation of the present invention, the solvent preferably comprises 20 parts by weight to 60 weight
Part.If the content declines less than 20 parts by weight, the stability of composition, and if it exceeds 60 parts by weight, then not only electric
Resistive is high, and is unable to undergo to impact.
Above-mentioned adhesive tree also may include by the above-mentioned conductive composition at the present invention being grouped as needed
Fat.Polyacrylic resin, polyurethane resin, epoxy resin, polyester resin etc. can be used in described adhesive resin, and content is opposite
In total conductive composition of 100 parts by weight can be 0.1 parts by weight to 30 parts by weight.
In addition, another embodiment according to the present invention provides a kind of liquid crystal display formed with the conductive composition
Device backplate.
Electrode mentioned in the present invention not only includes the backplate of common liquid crystals display device, but also includes alternative existing
Have backplate conductive polarizer film (Korean granted patent the 10-0592329th).Preferably, of the invention
Conductive composition can be used to form backplate.
The forming method of the backplate may include that coating is according to above-mentioned method system on the electrode for be formed in substrate
The step of standby backplate formation is heat-treated with conductive composition.
In the backplate forming method of the liquid crystal display device, the applicable conventional painting method of coating.
For example, the conventional application method used in the art such as applicable spray coating method, stick coating method, scraper method, rolling method, dip coating.
The coating is coated preferably on substrate with 0.5 μm to 1 μm of thickness, then in 100 DEG C or so of hot plate
The soft roasting film layer of (soft bake) to form thickness as 300nm~500nm is carried out on (hot plate), to form liquid crystal
The backplate of showing device.
Electrode formation conductive composition present invention as described above passes through electroconductive polymer in optimum organization object
Dispersibility the light transmittance of backplate can be improved.Moreover, if can be by the conductive composition of the present invention with the viscous of substrate
Flawless mode is coated in junction, then light transmittance can be greatly improved.Moreover, the conduction of the present invention is coated
Its case hardness of the property backplate of composition is also very outstanding.
Hereinafter, in order to help to understand that The present invention gives preferred embodiments, but following embodiments are only intended to illustrate this
Invention, the scope of the present invention are not limited to following embodiments.
Embodiment 1
By the propylene glycol of the TEOS (tetraethoxysilane) of 15 parts by weight, the IPA (isopropanol) of 9 parts by weight, 13 parts by weight
5.0% acetic acid dilute solution (aqueous solution) mixing of monomethyl ether, the water of 26 parts by weight, the acetylacetone,2,4-pentanedione of 5 parts by weight, 1 parts by weight
Afterwards, sol gel reaction is carried out under 50 DEG C of temperature condition 3 hours.
Then, to by adding consolidating with 2.0 weight % in the silane coupling agent precursor composition obtained by the reaction
Thermal acid generator (the Amine Blocked thermal acid of conductive-polymer solution and the amine sealing end of shape object
The TAG 2713S of generator, King Industries companies) it is mixed, to be prepared for the back of the body of liquid crystal display device
Face electrode formation conductive composition, relative to the composition of 100 parts by weight, the conductive-polymer solution adds
Dosage is 30 parts by weight, and the additive amount of the thermal acid generator of the amine sealing end is 1 parts by weight.
At this point, the solid content electroconductive polymer that conductive-polymer solution includes 2 weight % (passes through EDOT monomers and use
Make the polymerization of the PSSA of dopant the PEDOT/PSS for preparing) and 98 weight % water.
Embodiment 2
By the propylene glycol of the TEOS (tetraethoxysilane) of 15 parts by weight, the IPA (isopropanol) of 9 parts by weight, 13 parts by weight
5.0% acetic acid dilute solution (aqueous solution) mixing of monomethyl ether, the water of 26 parts by weight, the acetylacetone,2,4-pentanedione of 5 parts by weight, 1 parts by weight
Afterwards, sol gel reaction is carried out under 50 DEG C of temperature condition 3 hours.
Then, tool same as Example 1 is added in by the silane coupling agent precursor composition obtained by the reaction
There are thermal acid generator (the Amine Blocked thermal of the conductive-polymer solution and amine sealing end of the solid content of 2.0 weight %
The CXC 1820 of acid generator, King Industries companies) it is mixed, to be prepared for liquid crystal display device
Backplate formation conductive composition, relative to the composition of 100 parts by weight, the conductive-polymer solution
Additive amount be 30 parts by weight, the additive amount of the thermal acid generator of amine sealing end is 1 parts by weight.
Embodiment 3
By the propylene glycol of the TEOS (tetraethoxysilane) of 15 parts by weight, the IPA (isopropanol) of 9 parts by weight, 13 parts by weight
5.0% acetic acid dilute solution (aqueous solution) mixing of monomethyl ether, the water of 26 parts by weight, the acetylacetone,2,4-pentanedione of 5 parts by weight, 1 parts by weight
Afterwards, sol gel reaction is carried out under 50 DEG C of temperature condition 3 hours.
Then, tool same as Example 1 is added in by the silane coupling agent precursor composition obtained by the reaction
There are thermal acid generator (the Amine Blocked thermal of the conductive-polymer solution and amine sealing end of the solid content of 2.0 weight %
The TAG 1763 of acid generator, King Industries companies) it is mixed, to be prepared for liquid crystal display device
Backplate formation conductive composition, relative to the composition of 100 parts by weight, the conductive-polymer solution
Additive amount be 30 parts by weight, the additive amount of the thermal acid generator of amine sealing end is 1 parts by weight.
Embodiment 4
By the propylene glycol of the TEOS (tetraethoxysilane) of 15 parts by weight, the IPA (isopropanol) of 9 parts by weight, 13 parts by weight
5.0% acetic acid dilute solution (aqueous solution) mixing of monomethyl ether, the water of 26 parts by weight, the acetylacetone,2,4-pentanedione of 5 parts by weight, 1 parts by weight
Afterwards, sol gel reaction is carried out under 50 DEG C of temperature condition 3 hours.
Then, tool same as Example 1 is added in by the silane coupling agent precursor composition obtained by the reaction
There are thermal acid generator (the Amine Blocked thermal of the conductive-polymer solution and amine sealing end of the solid content of 2.0 weight %
The TAG 2712 of acid generator, King Industries companies) it is mixed, to be prepared for liquid crystal display device
Backplate formation conductive composition, relative to the composition of 100 parts by weight, the conductive-polymer solution
Additive amount be 30 parts by weight, the additive amount of the thermal acid generator of amine sealing end is 1 parts by weight.
Embodiment 5
By the propylene glycol of the TEOS (tetraethoxysilane) of 15 parts by weight, the IPA (isopropanol) of 9 parts by weight, 13 parts by weight
5.0% acetic acid dilute solution (aqueous solution) mixing of monomethyl ether, the water of 26 parts by weight, the acetylacetone,2,4-pentanedione of 5 parts by weight, 1 parts by weight
Afterwards, sol gel reaction is carried out under 50 DEG C of temperature condition 3 hours.
Then, tool same as Example 1 is added in by the silane coupling agent precursor composition obtained by the reaction
There are thermal acid generator (the quaternary ammonium of the conductive-polymer solution and quaternary ammonium sealing end of the solid content of 2.0 weight %
The CXC 1613 of Blocked thermal acid generator, King Industries companies) it is mixed, to make
It is described relative to the composition of 100 parts by weight for the backplate formation conductive composition of liquid crystal display device
The additive amount of conductive-polymer solution is 30 parts by weight, and the additive amount of the thermal acid generator of the quaternary ammonium sealing end is 1 parts by weight.
Comparative example 1
By the propylene glycol of the TEOS (tetraethoxysilane) of 15 parts by weight, the IPA (isopropanol) of 9 parts by weight, 13 parts by weight
5.0% acetic acid dilute solution (aqueous solution) mixing of monomethyl ether, the water of 27 parts by weight, the acetylacetone,2,4-pentanedione of 5 parts by weight, 1 parts by weight
Afterwards, sol gel reaction is carried out under 50 DEG C of temperature condition 3 hours.
Then, tool same as Example 1 is added in by the silane coupling agent precursor composition obtained by the reaction
The conductive-polymer solution for having the solid content of 2.0 weight %, to be prepared for conductive composition, wherein the electric conductivity is high
The additive amount of molecular solution is 30 parts by weight.At this point, conductive-polymer solution includes the solid content electric conductivity height of 2.0 weight %
The water of molecule (by EDOT monomers and PEDOT/PSS for polymerizeing to prepare of the PSSA as dopant) and 98 weight %.
Experimental example
Each conductive composition of the embodiment 1 to 5 and comparative example 1 is coated in 0.5 μm of thickness and is formed in base
It is soft 600 seconds roasting on 120 DEG C of hot plate after on the electrode of plate, to form thickness as the film layer of 300nm.
Following methods are utilized in reliability assessment coated on the backplate formation conductive material on substrate, knot
Fruit is shown in Table 1.
Room temperature reliability is assessed under the conditions of normal epidemic disaster (Rh 50% or less).High temperature reliability is to continue
It is placed on and is assessed in 80 DEG C of baking ovens.In addition, high temperature/high humidity reliability assessment be utilized 65 DEG C, the high temperature of Rh 90% it is high
Wet baking oven.The assessment of substrate surface resistance has been carried out 500 hours using the ST-4 equipment of SIMCO companies.
[table 1]
As shown in Table 1, for using the embodiment 1 to 5 of TAG (acid agent), 1 phase of comparative example with unused acid agent
Than after 500 hours, outstanding result is shown in terms of room temperature and high temperature, high temperature and humidity reliability.In particular, implementing
The result of example 1 to 2, which is shown, ensures classic reliability.
However, comparative example 1 is not suitable for forming electrode due to poor reliability.
Claims (12)
1. a kind of backplate formation conductive composition of liquid crystal display device, including：
The silane coupling agent of 5 parts by weight to 40 parts by weight；
The solvent of 50 parts by weight to 90 parts by weight；
The hydrochloric acid or acetic acid dilute solution of 0.1 parts by weight to 10.0 parts by weight；
The conductive-polymer solution of 5 parts by weight to 40 parts by weight, the solid content with 0.1 weight % to 5.0 weight %；With
And
The acid agent of 0.001 parts by weight to 1.0 parts by weight,
The acid agent is at least one in the thermal acid generator selected from amine sealing end, covalent bond sealing end, metal sealing end and quaternary ammonium sealing end
Kind.
2. the backplate formation conductive composition of liquid crystal display device according to claim 1, wherein：
The solvent includes selected from i) water, ii) alcohol compound and iii) dihydroxypropane single-ether, dimethylformamide, levulinic
At least one of ketone, 1-Methyl-2-Pyrrolidone, butyrone and ethyl lactate solvent.
3. the backplate formation conductive composition of liquid crystal display device according to claim 2, wherein：
The alcohol compound is to be selected from methanol, ethyl alcohol, isopropanol, ethylene glycol, butanediol, neopentyl glycol, 1,3- pentanediols, 1,
In 4- cyclohexanedimethanols, diethylene glycol (DEG), polyethylene glycol, polybutylene glycol, dihydroxy methylpropane, trimethylolpropane at least
It is a kind of.
4. the backplate formation conductive composition of liquid crystal display device according to claim 1, wherein：
The solid content of its electroconductive polymer of conductive-polymer solution is 0.1 weight % to 5 weight % and includes 95 weights
Measure the solvent of % to 99.9 weight %.
5. the backplate formation conductive composition of liquid crystal display device according to claim 4, wherein：
The electroconductive polymer includes selected from least one of polyaniline, polypyrrole, polythiophene.
6. the backplate formation conductive composition of liquid crystal display device according to claim 4, wherein：
The electroconductive polymer includes poly- (3,4- ethylenedioxy thiophenes).
7. the backplate formation conductive composition of liquid crystal display device according to claim 6, wherein：
The electroconductive polymer also includes selected from dodecyl benzene sulfonic acid, toluenesulfonic acid, camphorsulfonic acid, benzene sulfonic acid, hydrochloric acid, benzene
Vinyl sulfonic acid, 2- acrylamide-2-methylpro panesulfonic acids and their salt compound or 2- sulfosuccinate ester salts, 5- sulfo groups
Bis- (beta-hydroxyethyl the ester) -5- sodium sulfonates of M-phthalic acid sodium salt, Sodium Dimethyl Isophthalate-5-sulfonate, M-phthalic acid and
At least one of poly- (4- styrene sulfonates) dopant.
8. the backplate formation conductive composition of liquid crystal display device according to claim 4, wherein：
The electroconductive polymer uses poly- (3,4- ethylenedioxy thiophenes):Poly- (4- styrene sulfonates) i.e. PEDOT:PSS.
9. the backplate formation conductive composition of liquid crystal display device according to claim 1, wherein：
The silane coupling agent is selected from alkoxyl silicone alkanes, amino silicone alkanes, vinyl silanes with C1 to C20 alkyl
At least one of class, epoxy radicals silicone hydride class, methacryloxypropyl silane class, isocyanatosilanes class and fluorine-based silane class.
10. the backplate formation conductive composition of liquid crystal display device according to claim 1 also includes surface
Activating agent, relative to the conductive composition of 100 parts by weight, the content of the surfactant is 0.1 to 1 parts by weight.
11. the backplate formation conductive composition of liquid crystal display device according to claim 1 also includes to be selected from
At least one of polyacrylic resin, polyurethane resin, epoxy resin and polyester resin adhesive resin, relative to 100 weights
The conductive composition of part is measured, the content of described adhesive resin is 0.1 parts by weight to 30 parts by weight.
12. a kind of liquid crystal display device face electrode, is formed with conductive composition described in claim 1.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2013-0154635 | 2013-12-12 | ||
| KR1020130154635A KR20150068685A (en) | 2013-12-12 | 2013-12-12 | Conductive composition forming ground electrodes of liquid crystal display |
| PCT/KR2014/010859 WO2015088146A1 (en) | 2013-12-12 | 2014-11-12 | Conductive composition for forming rear electrode of liquid crystal display device |
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| CN105814644A CN105814644A (en) | 2016-07-27 |
| CN105814644B true CN105814644B (en) | 2018-08-24 |
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| KR102562916B1 (en) * | 2022-12-07 | 2023-08-03 | (주)에버켐텍 | Forming composition of ground electrodes comprising conductive polymer and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1255513A (en) * | 1998-11-05 | 2000-06-07 | 三星综合化学株式会社 | Polythiophene conductive polymer liquid compsn. with high conductive rate and transparency |
| KR20100047440A (en) * | 2008-10-29 | 2010-05-10 | 주식회사 동진쎄미켐 | Conductive composition forming ground electrodes of liquid crystal display |
| CN101880460A (en) * | 2003-06-18 | 2010-11-10 | 信越聚合物株式会社 | Electrically conductive composition and preparation method thereof |
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| JPH0826231B2 (en) * | 1991-08-16 | 1996-03-13 | インターナショナル・ビジネス・マシーンズ・コーポレイション | Conductive polymer material and its use |
| KR20040044369A (en) * | 2002-11-20 | 2004-05-28 | 쉬플리 캄파니, 엘.엘.씨. | Multilayer photoresist systems |
| KR20120066944A (en) * | 2010-12-15 | 2012-06-25 | 삼성전기주식회사 | A conductive paste composition for inner electrode, a laminated ceramic electronic parts by using the same and a process thereof |
| KR102002325B1 (en) * | 2011-12-29 | 2019-07-23 | 주식회사 동진쎄미켐 | Conductive composition for forming ground electrodes of liquide crystal display and method for forming ground electrodes using the same |
| KR101933383B1 (en) * | 2012-11-19 | 2019-04-05 | 주식회사 동진쎄미켐 | Method for preparing conductive composition forming ground electrodes of liquid crystal display and using the same |
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- 2013-12-12 KR KR1020130154635A patent/KR20150068685A/en not_active Application Discontinuation
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- 2014-11-12 JP JP2016538648A patent/JP6728045B2/en active Active
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1255513A (en) * | 1998-11-05 | 2000-06-07 | 三星综合化学株式会社 | Polythiophene conductive polymer liquid compsn. with high conductive rate and transparency |
| CN101880460A (en) * | 2003-06-18 | 2010-11-10 | 信越聚合物株式会社 | Electrically conductive composition and preparation method thereof |
| KR20100047440A (en) * | 2008-10-29 | 2010-05-10 | 주식회사 동진쎄미켐 | Conductive composition forming ground electrodes of liquid crystal display |
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| KR20150068685A (en) | 2015-06-22 |
| JP2017502337A (en) | 2017-01-19 |
| JP6728045B2 (en) | 2020-07-22 |
| WO2015088146A1 (en) | 2015-06-18 |
| CN105814644A (en) | 2016-07-27 |
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