CN105814644A - 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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- CN105814644A CN105814644A CN201480067695.3A CN201480067695A CN105814644A CN 105814644 A CN105814644 A CN 105814644A CN 201480067695 A CN201480067695 A CN 201480067695A CN 105814644 A CN105814644 A CN 105814644A
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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 film excellent reliability for forming leading of liquid crystal indicator backplate
Conductive composition.
Background technology
In electrode formation technology, especially in liquid crystal indicator, backplate effect is that shielding comes
From outside electrostatic.
Past is used as backplate (Korean granted patent the 10-0603826th) in liquid crystal indicator
The ITO (Indium-tin-oxide, indium tin oxide) of material or IZO (Indium-Zinc-oxide, indium zinc
Oxide) need to carry out vacuum evaporation operation, for the characteristic of these backing electrode material, although resistance
Outstanding with case hardness, but transmittance is poor.
In view of the problem of indium resource exhaustion occurs recently, for replacing the various transparent electrode materials of ITO
Be developed into subject under discussion.But, present situation is the many transparent electrode material (examples developed up to now
Such as, electroconductive polymer or the inorganic conductive compositions etc. that comprises metal or metal-oxide) thoroughly
Luminosity aspect still demonstrates unsatisfactory result.
Utilize the film of electroconductive polymer, although there is outstanding transmittance, but sheet resistance with
And increase as electrode forms the period of material, therefore the problem that reliability reduces occurs.
Summary of the invention
Technical problem
In order to solve above-mentioned technical problem, it is an object of the invention to provide a kind of when forming electrode, special
It not when forming the backplate of liquid crystal indicator, the liquid of the reliability being coated with under membrane stage can be improved
The backplate formation conductive composition of crystal device and utilize the liquid crystal of this conductive composition
The backplate of display device.
Additionally, another object of the present invention is to provide one can improve coating, hardness and to greatest extent
Ground reduces the method for the sheet resistance increased over time after film is formed.
Technical scheme
The present invention provides the backplate formation conductive composition of a kind of liquid crystal indicator to comprise:
The silane coupler of 5 weight portions to 40 weight portions；
The solvent of 50 weight portions to 90 weight portions；
The hydrochloric acid of 0.1 weight portion to 10.0 weight portions or acetic acid dilute solution；
The conductive-polymer solution of 5 weight portions to 40 weight portions, it has 0.1 weight % to 5.0 weights
The solid content of amount %；And
The acid agent of 0.001 weight portion to 1.0 weight portions.
Described acid agent can be selected from amine end-blocking (Amine blocked), covalent bond end-blocking (covalent
Blocked), metal end-blocking (metal blocked) and quaternary ammonium end-blocking (Quaternary Ammonium
Blocked) at least one in thermal acid generator (thermal acid generator).
It addition, described acid agent can be selected from DBSA, p-toluenesulfonic acid, fluoroform
At least one in sulfonic acid and derivant thereof.
Described solvent preferably comprises selected from i) water, ii) alcohol compound and iii) dihydroxypropane single-ether, two
Methylformamide, acetylacetone,2,4-pentanedione, 1-methyl-2-pyrrole network alkanone, butyrone (dipropylketone)
With at least one solvent in ethyl lactate.
The solid content of described its electroconductive polymer of conductive-polymer solution is that 0.1 weight % is to 5 weights
Measure % and the solvent of 95 weight % to 99.9 weight % can be comprised.
Described electroconductive polymer can comprise in polyaniline, polypyrrole, polythiophene and derivant thereof
At least one, preferably comprise poly-(3,4-ethylene dioxythiophene).
It addition, described electroconductive polymer the most also comprise selected from DBSA, toluenesulfonic acid,
Camphorsulfonic acid (camphorsulfonic acid), benzenesulfonic acid, hydrochloric acid, styrene sulfonic acid (styrenesulfonic
Acid), 2-acrylamide-2-methylpro panesulfonic acid (2-acrylamido-2-methylpropanesulfonic
Acid), their salt compound, 2-sulfosuccinate ester salt (2-sulfosuccinate ester salt), 5-
Sulfo isophthalate sodium salt (5-sulfoisophthalic acid sodium salt), M-phthalic acid diformazan
Double (the beta-hydroxyethyl of ester-5-sodium sulfonate (dimethyl-5-sodium sulfoisophthalate), M-phthalic acid
Ester)-5-sodium sulfonate (5-sodium sulfo-bis (β-hydroxyethyl) isophthalate) and poly-(4-benzene second
Alkene sulfonate) at least one alloy.Described electroconductive polymer preferably comprises poly-as alloy
(4-styrene sulfonate).
Described electroconductive polymer is preferably used poly-(3,4-ethylenedioxy thiophene): poly-(4-styrene sulfonic acid
Salt) (PEDOT:PSS).
Described silane coupler can be selected from the alkoxyl silicone alkanes with C1 to C20 alkyl
(alkyloxy silane), amino silicone alkanes (amino silane), vinyl silanes class (vinyl silane),
Epoxy radicals silicone hydride class (epoxy silane), methacryloxypropyl silane class (methacryloxy silane),
In isocyanatosilanes class (isocyanate silane) and fluorine-based silane class (fluoro silane) at least one
Kind.
Additionally, according to the present invention, relative to the described total composition of 100 weight portions, 0.1 also can be comprised
Weight portion is to the surfactant of 1.0 weight portions.
It addition, relative to the described conductive composition of 100 weight portions, 0.1 weight portion also can be comprised
To 30 weight portions in polyacrylic resin, polyurethane resin, epoxy resin and polyester resin
At least one adhesive resin.
Additionally, the present invention provides the liquid crystal display device that a kind of described conductive composition is formed
Face electrode.
Beneficial effect
Present invention electrode conductive composition overleaf employs particular thermal acid agent (TAG), thus
Acid can be produced further during baking so that unreacted silane compound (such as, TEOS) enters after coating
One one-step hydrolysis, thus the film of the degree of cross linking having between stronger silane coupler can be formed.And
And, the present invention can optimize the dispersibility of electroconductive polymer in backplate conductive composition.
Therefore, the present invention is at liquid crystal indicator (LCD) (especially, the Transverse electric-field type such as IPS, FFS
Liquid crystal indicator) in can reduce the sheet resistance increased over time after formation film, i.e. improve
Reliability.
Detailed description of the invention
Below, describe the present invention.
There is provided the backplate of a kind of liquid crystal indicator to be formed according to the preferred embodiments of the invention to use
Conductive composition, this conductive composition comprises: the silane coupler of 5 weight portions to 40 weight portions；
The solvent of 50 weight portions to 90 weight portions；The hydrochloric acid of 0.1 weight portion to 10.0 weight portions or acetic acid dilution
Solution；The conductive-polymer solution of 5 weight portions to 40 weight portions, it has 0.1 weight % to 5.0
The solid content of weight %；And 0.001 weight portion to the acid agent of 1.0 weight portions.
Present invention electrode formation conductive composition overleaf employs acid agent TAG, thus has
The advantage having the reliability that can improve backplate film.This conductive composition may utilize silane
Coupling agent precursor composition, conductive-polymer solution and specific acid agent.
Described silane coupler precursor composition comprise 5 weight portions to 40 weight portions silane coupler,
The solvent of 50 weight portions to 90 weight portions, 0.1 weight portion dilute to hydrochloric acid or the acetic acid of 10.0 weight portions
Solution, obtains described silane coupler precursor composition by their sol gel reaction.And,
Described conductive-polymer solution refers to utilize electroconductive polymer and solvent and the solid content that obtains
It is the solution of 0.1 weight % to 5.0 weight %.
It addition, it is a feature of the present invention that by using specific acid agent to substantially increase electric conductivity group
The reliability of compound.Described acid agent uses the material producing acid under heat effect, and described acid agent is preferred
Use the thermal acid generator of amido end-blocking when adding material.And, the selection model of acid agent in the present invention
Enclose wide, can use from metal ion content be controlled as thermal acid generator (TAG) series of below 2ppm to
Metal ion content is controlled as the acid agent of the CXC grade (CXC Grade) of more than 2ppm.Preferably
Ground, described acid agent uses and can produce acid at a temperature of soft roasting (the soft bake) of 100 DEG C to 150 DEG C
Material.
Described acid agent can be selected from amine end-blocking (Amine blocked), covalent bond end-blocking (covalent
Blocked), metal end-blocking (metal blocked) and quaternary ammonium end-blocking (Quaternary Ammonium
Blocked) at least one in thermal acid generator (thermal acid generator).As described acid agent
Solubilized can be used or be dissolved in solvent used in the present invention (such as IPA, PGME or water etc.)
In product.
It addition, described acid agent can use selected from DBSA (Dodecylbenzene sulfonic
Acid), p-toluenesulfonic acid (p-Toluene sulfonic acid), trifluoromethanesulfonic acid (Trifluoromethane
Sulfonic acid) and derivant at least one.King can be used as described acid agent
All CXC and TAG grades (TAG Grade) product of inderstries company.
Now, for described conductive composition, when needing to improve reliability, only with known electrodes group
The component of laminate material can not coordinate its characteristic, therefore should use the specific product acid of the present invention further
Agent i.e. TAG.
During additionally, use TAG based on solvent composition or electroconductive polymer characteristic, the modification of material can
Can be the most serious, it is thus possible to cannot be applicable to the component not obtaining optimization.Such as, described TAG
May be applicable to the backing electrode material not obtaining optimization.But, used in the present invention specific
Acid agent is included in the component of optimization, therefore has cooperative effect, can play very improving reliability
Big effect.
It addition, described silane coupler plays the dispersibility of raising electroconductive polymer in the composition
Effect.Described silane coupler can use alkoxyl silicone alkanes, amino silicone alkanes, vinyl silanes class,
Epoxy radicals silicone hydride class, methacryloxypropyl silane class, isocyanatosilanes class, fluorine-based silane class etc..
More specifically, have TEOS (tetraethoxysilane), vinyl triethoxyl as described silane coupler
Silane, vinyltrimethoxy silane, vinyl three (beta-methoxy ethyoxyl) silane, γ-(methacryl
Epoxide) propyl trimethoxy silicane, β-(3,4-epoxycyclohexyl) ethyl trimethoxy silane, γ-epoxy third
Oxygen propyl trimethoxy silicane (γ-glycidoxypropyltrimethoxysilane), γ-mercapto propyl trimethoxy
Silane (γ-mercaptopropyltrimethoxysilane), gamma-aminopropyl-triethoxy-silane, N-β-(ammonia second
Base)-γ-aminopropyltrimethoxysilane, γ-ureidopropyltriethoxysilane
(γ-ureidopropyltriethoxysilane), phenyl triethoxysilane, MTES, first
Base trimethoxy silane, polyethylene oxide modified silane monomer, poly-methylethoxy radical siloxane
(polymethylethoxy siloxane), hexamethyldisiloxane (hexamethyldisilazane) etc., can
To select at least one in them.
Relative to total conductive composition, described silane coupler is preferably used 5 weight portions to 40 weight
Part, more preferably use 10 weight portions to 30 weight portions.If described content is less than 5 weight portions, then
Easily produce separated caused surface spot when forming coating and case hardness may reduce.As
The most described content is more than 40 weight portions, then resistance uprises and the stability of compositions declines.
Additionally, solvent used in the present invention can comprise selected from i) water, ii) alcohol compound and iii) third
2-ethoxyethanol, dimethylformamide, acetylacetone,2,4-pentanedione, 1-methyl-2-pyrrole network alkanone, butyrone
With at least one solvent in ethyl lactate.
It is to say, solvent used in the present invention is water, alcohol compound, water is as TEOS water
The primary solvent solved uses and comprises 10 weight portions to 50 weight portions, alcohol relative to total solvent content
Compounds mainly uses monohydric alcohol and dihydroxylic alcohols and can comprise 10 weight portions relative to total solvent content
The alcohol that boiling point is 50 DEG C to 200 DEG C to the C1 to C10 of 50 weight portions.Alcohol reacts as TEOS
Afterwards for making hydrolysis and esterification stably carry out keeping the solvent of the stability of sol particles
Use.And, in order to make coating be optimized, it is possible to use boiling point is 100 degree～160 degree left sides
Right methoxyl group, ethyoxyl, propyl group ethanol (propylethanol) kind solvent and relative to total solvent content
10 weight portions can be comprised to 50 weight portions.
Described alcohol compound comprises alcohol (alcohol), glycol (diol) or polyhydric alcohol (polyol), such as may be used
With use selected from methanol, ethanol, isopropanol, ethylene glycol, butanediol, neopentyl glycol, 1,3-pentanediol,
1,4 cyclohexane dimethanol, diethylene glycol, Polyethylene Glycol, polybutylene glycol (polybutylene glycol),
In dihydroxy methylpropane (dimethylol propane), trimethylolpropane and their derivant at least
A kind of.
Additionally, the present invention as desired as solvent can use further chloroform, dichloromethane,
The halogenation species such as tetrachloroethylene, trichloro ethylene, Bromofume, dibromopropane；N-Methyl pyrrolidone,
Dimethyl sulfoxide；Triethylamine, tri-n-butylamine, trioctylamine；Cresol etc..
The coating that the difference of the volatility produced when described solvent can eliminate surface-coated is caused is uneven
Property, and improve the density of TEOS film, thus play the effect that can increase sheet resistance reliability.
Relative to total composition, described solvent can comprise in the composition as surplus, but preferably to lead
The gross weight of conductive composition is for will definitely use 50 weight portions to 90 weight portions.
Described hydrochloric acid or acetic acid dilute solution can be used, in order to carry out with hydrolysis under acid atmosphere
Sol gel reaction.Described hydrochloric acid or acetic acid dilute solution can use water-reducible 0.1% to 10%
Hydrochloric acid or acetic acid dilute solution, but be not limited to this.Relative to total conductive composition, described hydrochloric acid
Or acetic acid dilute solution can use 0.1 weight portion to 10.0 weight portions.
Additionally, use conductive-polymer solution to prepare the conductive composition of the present invention, as
Upper described preferred solid content is that 0.1 weight % is to 5.0 weight %.Now, if described electric conductivity
In macromolecular solution, the content of solid content is less than 0.1 weight %, then there is the problem losing electrode effect,
And if it exceeds 5 weight %, then can promote the gathering (aggregation) with TEOS aerosol precursor compositions
And the gelation of conductive-polymer solution itself, thus it is difficult to prepare.
Relative to total conductive composition, described conductive-polymer solution uses 5 weight portions to 40 weights
Amount part.If the content of described conductive-polymer solution is less than 5 weight portions, then resistance drastically uprises,
And if it exceeds 40 weight portions, then transmittance reduces and is difficult to keep stablizing of dispersing characteristic and compositions
Property.
The solid content of this its electroconductive polymer of conductive-polymer solution is that 0.1 weight % is to 5 weights
Measure % and the solvent comprising 95 weight % to 99.9 weight %, or the solid content of electroconductive polymer can
It is 5 weight % to 60 weight % and the solvent comprising 40 weight % to 95 weight %.
It addition, described electroconductive polymer used in the present invention is Organic substance, also make the present invention
The base substance of compositions band electric conductivity.
Need doping process to make described electroconductive polymer have electric conductivity, and implement this process
Method make non-conductive powder type or form of film after it is carried out chemical doping or by non-
It is dissolved in organic solvent there is electric conductivity after electroconductive powder and alloy mixing.Wherein, this
Bright use the method utilizing described alloy.Therefore, described electroconductive polymer is preferably used and mixes
The form of foreign material mixing, the macromolecule during i.e. alloy is doped to electroconductive polymer.
Such as, substantially electroconductive polymer can use polyaniline, polypyrrole, polythiophene and derive
The macromolecule etc. that thing, the derivant of monomer whose (aniline, pyrroles, thiophene) are polymerized as monomer.This
Time, deriving of the most useful thiophene of macromolecule that the derivant of described monomer is polymerized as monomer
Poly-(the 3,4-enedioxy thiophene that thing i.e. 3,4-ethylenedioxy thiophene is polymerized
Fen) (poly (3,4-ethylenedioxythiophen), PEDOT).Described PEDOT is stable in an atmosphere
And room temperature conductivity is higher than other macromolecules.
In the present invention, it is possible to also comprise outside this electroconductive polymer selected from DBSA,
Toluenesulfonic acid, camphorsulfonic acid, benzenesulfonic acid, hydrochloric acid, styrene sulfonic acid, 2-acrylamido-2-methyl
Propane sulfonic acid, their salt compound, 2-sulfosuccinate ester salt, 5-sulfo isophthalate sodium salt,
Double (beta-hydroxyethyl the ester)-5-sodium sulfonates of dimethyl phthalate-5-sodium sulfonate, M-phthalic acid and poly-(4-benzene
Vinyl sulfonate) mixture of at least one alloy in (PSS, poly (4-styrene sulfonate))
Form is used for preparing composition for electrode formation.And, alloy is preferably used poly-(4-styrene sulfonic acid
Salt).
Therefore, the present invention is when preparing electrode formation conductive composition, it is possible to use described
Adulterate in PEDOT the PEDOT-PSS (also known as PEDOT:PSS) of PSS, PEDOT-PSS conduct
Electrode or antistatic material coating are good, and interfacial characteristics and caking property are the most outstanding.
And, according to the present invention, relative to total conductive composition of 100 weight portions, it is also possible to bag
Surfactant containing 0.1 weight portion to 1.0 weight portions.Described silicon surface active agent can be used, but
Kinds of surfactants is not limited to this.
Additionally, the present invention is as required, relative to the described conductive composition of 100 weight portions, also
Can comprise 0.1 weight portion to 30 weight portions selected from polyacrylic resin, polyurethane resin, asphalt mixtures modified by epoxy resin
At least one adhesive resin in fat and polyester resin.
It addition, the present invention is when preparing conductive composition, not use as in the past by disposably adding
Enter to add to each composition (such as, electroconductive polymer and the TEOS etc. in backplate formation component
Material) mode that is prepared, but silane coupler (TEOS) is at high temperature carried out sol-gel
Reaction and after preparing precursor solution, be mixed into electroconductive polymer and acid agent, formed and use preparing electrode
Conductive composition.Below, further illustrate and prepare each step of electrode formation conductive composition
Suddenly.
Prepare silane coupler precursor composition
Carry out the sol gel reaction by silane coupler in this step and prepare the operation of precursor.
Its final component of electrode formation conductive composition of the present invention can comprise electric conductivity high score
Son, alloy, silane coupler, acid agent and solvent, and the present invention is carried out utilize silane coupled
The operation of precursor solution is prepared in agent, so that conductive composition has described component.
It is to say, mode of the present invention is different from existing preparation method, first prepare logical
After crossing the precursor that the sol gel reaction of silane coupler obtains, it is carried out with electroconductive polymer
Mixing, therefore can provide a kind of electrode formation conductive composition, meet outstanding under membrane stage
Case hardness and time-based reliability area, it is also possible to demonstrate than conventional general room temperature system
The performance that standby mode is outstanding.
Particularly, different from the past by the electroconductive polymer under normal temperature condition with the polymerization of TEOS
The mode prepared, uses the back of the body prepared by the sol gel reaction by silane coupler in the present invention
The precursor of face electrode formation conductive composition.Therefore, the present invention can improve the back side finally given
The crosslinking degree of the film in electrode itself, and improve hardness by the effect thus brought and increase tool
There is the area density of the electroconductive polymer of opposite nature, such that it is able to reduce making of electroconductive polymer
Consumption, it is also possible to improve the reliability reduced because of Relatively centralized in the electroconductive polymer on surface.
It is known that described sol gel reaction is commonly used for the method preparing inorganic material, the method is led to
Cross make metal alkoxide be hydrolyzed under alcohols solvent-polycondensation comes synthesis of metal oxide or hydroxide
The ceramic powders of form.It addition, have TEOS sol-gel process as described sol gel reaction is known.
Therefore, in the present invention from this starting point, when carrying out the sol gel reaction of silane coupler, no
It is to react at normal temperatures, but higher than carrying out sol gel reaction at a temperature of room temperature, thus
Bridging property when forming film on metal can be improved, and hardness can be improved.It is to say, at this
By the silane coupler precursor composition obtained by described sol gel reaction and described later in invention
The combination of electroconductive polymer improves high molecular dispersibility and improves mechanical strength, the most also may be used
To improve hot property, thus provide the effect being suitable for electronic material.This composition can realize group
Become the performance of organic-inorganic hybrid composite, it may thereby be ensured that the rigidity of inorganic matter and heat are outstanding
Property, it is also possible to the performance such as flexibility and processability of guaranteeing polymer.And, shape of the present invention
Carry out the result of reliability assessment after film forming to show and guarantee reliability and improve hardness.
This sol gel reaction is by high temperature carrying out silane coupler and solvent certain time
Sol gel reaction prepare silane coupler precursor solution (such as, TEOS sol solutions).
Now, the high temperature mentioned in the present invention means above the temperature of room temperature.Preferably, described colloidal sol-
Gel reaction is carried out 1 hour to 5 hours at a temperature of 40 DEG C to 70 DEG C.Most preferably, described molten
Glue-gel reaction is carried out 3 hours at a temperature of 50 DEG C.If described sol gel reaction is being less than
Carry out at a temperature of 40 DEG C, then hydrolysis (Hydrolysis) degree that may result in TEOS reduces, and
And the speed of the subsidiary condensation reaction produced may be faster than hydrolysis, therefore hardness and TEOS colloidal sol grain
Son becomes long side it is possible that problem.And, if sol gel reaction is in the temperature higher than 70 DEG C
Under carry out, although then hydrolysis aspect can be reacted more reliably, but due to after this through hydrolysis and contracting
The growth rate of the TEOS sol particles closing reaction is too fast, it is possible that quick-gelatinizing
(Gellation) problem.
It addition, in the step preparing silane coupler precursor composition, it is also possible to add surface activity
React after agent.
Preferably, in the step preparing silane coupler precursor composition, relative to 100 weight portions
Described silane coupler precursor composition, it is also possible to add the surface of 0.1 weight portion to 1.0 weight portions
Activating agent.
The preparation of backplate formation conductive composition
In the present invention, after preparing silane coupler precursor composition by above-mentioned method, add tool
There is 5 weight portions electroconductive polymer to 40 weight portions of 0.1 weight % solid content to 5.0 weight %
The acid agent of solution and 0.001 weight portion to 1.0 weight portions mixes, and is finally made liquid crystal display dress
The backplate formation conductive composition put.
In the process, the mixing of silane coupler precursor composition and electroconductive polymer can be
Carry out at a temperature of 10 DEG C to 40 DEG C.
The backplate formation electric conductivity of the final liquid crystal indicator prepared according to the method described above combines
Thing can comprise: the conductive-polymer solution of 5 weight portions to 40 weight portions, and it has 0.1 weight %
Solid content to 5.0 weight %；The silane coupler of 3 weight portions to 30 weight portions；20 weight portions are extremely
The solvent of 60 weight portions；And 0.001 weight portion to the acid agent of 1.0 weight portions.
In final electrode formation conductive composition, if the content of described electroconductive polymer is not
Foot 5 weight portions, then resistance drastically uprises, and if it exceeds 40 weight portions, then transmittance reduces and difficult
To keep dispersing characteristic and the stability of compositions.
It addition, relative to the final composition for electrode formation of the present invention, described silane coupler is preferred
Comprise 3 weight portions to 30 weight portions, more preferably comprise 5 weight portions to 20 weight portions.If it is described
Content less than 3 weight portions, then easily produces separated caused surface spot and table when forming coating
Surface hardness may reduce, and if it exceeds 30 weight portions, then resistance uprises and the stability of compositions
Decline.
Relative to the final composition for electrode formation of the present invention, described solvent preferably comprises 20 weight portions
To 60 weight portions.If described content is less than 20 weight portions, then the stability of compositions declines, and
If it exceeds 60 weight portions, the most not only resistance uprises, and is unable to undergo impact.
The conductive composition of the present invention being grouped into by above-mentioned one-tenth the most also can comprise above-mentioned
Adhesive resin.Described adhesive resin can use polyacrylic resin, polyurethane resin, asphalt mixtures modified by epoxy resin
Fat, polyester resin etc., its content can be 0.1 weight relative to total conductive composition of 100 weight portions
Amount part is to 30 weight portions.
It addition, provide a kind of described conductive composition to be formed according to another embodiment of the present invention
Liquid crystal display device face electrode.
The electrode mentioned in the present invention not only comprises the backplate of common liquid crystals display device, and wraps
Containing alternative existing backplate the film (Korean granted patent of conductive Polarizer
No. 10-0592329).Preferably, the conductive composition of the present invention can be used for forming backplate.
The forming method of described backplate may be included in be formed on the electrode of substrate and coats according to above-mentioned
The backplate formation conductive composition prepared of method carry out the step of heat treatment.
In the backplate forming method of described liquid crystal indicator, the applicable routine of described coating
Painting method.Such as, applicable spraying process, stick coating method, doctor blade method, rolling method, dip coating etc. are originally
The conventional application method used in field.
Described coating is preferably coated to the thickness of 1 μm with 0.5 μm on substrate, then at 100 DEG C
Soft roasting (soft bake) is carried out to form thickness as 300nm～500nm on the hot plate (hot plate) of left and right
Film layer, thus form the backplate of liquid crystal indicator.
The electrode formation of the present invention as above is passed through to conduct electricity in optimum organization thing with conductive composition
The high molecular dispersibility of property can improve the transmittance of backplate.And, if can be by the present invention's
Conductive composition is coated in mode flawless on the bonding plane of substrate, then transmittance can obtain
To the biggest improvement.Moreover, its surface of backplate of the conductive composition of the coating present invention is hard
Spend the most outstanding.
Hereinafter, The present invention gives preferred embodiment to contribute to understanding, but following embodiment is simply
For illustrating the present invention, the scope of the present invention is not limited to following embodiment.
Embodiment 1
By the TEOS (tetraethoxysilane) of 15 weight portions, the IPA (isopropanol) of 9 weight portions, 13 weights
The amount propylene glycol monomethyl ether of part, the water of 26 weight portions, the acetylacetone,2,4-pentanedione of 5 weight portions, 1 weight portion
After 5.0% acetic acid dilute solution (aqueous solution) mixing, under the temperature conditions of 50 DEG C, carry out sol-gel anti-
Answer 3 hours.
Then, in the silane coupler precursor composition obtained by described reaction, interpolation has 2.0
The conductive-polymer solution of the solid content of weight % and thermal acid generator (the Amine Blocked of amine end-blocking
The TAG 2713S of thermal acid generator, King Industries company) mix, thus
It is prepared for the backplate formation conductive composition of liquid crystal indicator, relative to 100 weight portions
Described compositions, the addition of described conductive-polymer solution is 30 weight portions, described amine block
The addition of thermal acid generator be 1 weight portion.
Now, the solid content electroconductive polymer that conductive-polymer solution comprises 2 weight % (passes through
PEDOT/PSS prepared by EDOT monomer and the polymerization as the PSSA of alloy) and 98 weight %
Water.
Embodiment 2
By the TEOS (tetraethoxysilane) of 15 weight portions, the IPA (isopropanol) of 9 weight portions, 13 weights
The amount propylene glycol monomethyl ether of part, the water of 26 weight portions, the acetylacetone,2,4-pentanedione of 5 weight portions, 1 weight portion
After 5.0% acetic acid dilute solution (aqueous solution) mixing, under the temperature conditions of 50 DEG C, carry out sol-gel anti-
Answer 3 hours.
Then, add and embodiment in the silane coupler precursor composition obtained by described reaction
The conductive-polymer solution of the 1 identical solid content with 2.0 weight % and the thermal acid generator of amine end-blocking
The CXC 1820 of company (Amine Blocked thermal acid generator, the King Industries) enters
Row mixing, thus it is prepared for the backplate formation conductive composition of liquid crystal indicator, relatively
In the described compositions of 100 weight portions, the addition of described conductive-polymer solution is 30 weight portions,
The addition of the thermal acid generator of described amine end-blocking is 1 weight portion.
Embodiment 3
By the TEOS (tetraethoxysilane) of 15 weight portions, the IPA (isopropanol) of 9 weight portions, 13 weights
The amount propylene glycol monomethyl ether of part, the water of 26 weight portions, the acetylacetone,2,4-pentanedione of 5 weight portions, 1 weight portion
After 5.0% acetic acid dilute solution (aqueous solution) mixing, under the temperature conditions of 50 DEG C, carry out sol-gel anti-
Answer 3 hours.
Then, add and embodiment in the silane coupler precursor composition obtained by described reaction
The conductive-polymer solution of the 1 identical solid content with 2.0 weight % and the thermal acid generator of amine end-blocking
The TAG 1763 of company (Amine Blocked thermal acid generator, the King Industries) enters
Row mixing, thus it is prepared for the backplate formation conductive composition of liquid crystal indicator, relatively
In the described compositions of 100 weight portions, the addition of described conductive-polymer solution is 30 weight portions,
The addition of the thermal acid generator of described amine end-blocking is 1 weight portion.
Embodiment 4
By the TEOS (tetraethoxysilane) of 15 weight portions, the IPA (isopropanol) of 9 weight portions, 13 weights
The amount propylene glycol monomethyl ether of part, the water of 26 weight portions, the acetylacetone,2,4-pentanedione of 5 weight portions, 1 weight portion
After 5.0% acetic acid dilute solution (aqueous solution) mixing, under the temperature conditions of 50 DEG C, carry out sol-gel anti-
Answer 3 hours.
Then, add and embodiment in the silane coupler precursor composition obtained by described reaction
The conductive-polymer solution of the 1 identical solid content with 2.0 weight % and the thermal acid generator of amine end-blocking
The TAG 2712 of company (Amine Blocked thermal acid generator, the King Industries) enters
Row mixing, thus it is prepared for the backplate formation conductive composition of liquid crystal indicator, relatively
In the described compositions of 100 weight portions, the addition of described conductive-polymer solution is 30 weight portions,
The addition of the thermal acid generator of described amine end-blocking is 1 weight portion.
Embodiment 5
By the TEOS (tetraethoxysilane) of 15 weight portions, the IPA (isopropanol) of 9 weight portions, 13 weights
The amount propylene glycol monomethyl ether of part, the water of 26 weight portions, the acetylacetone,2,4-pentanedione of 5 weight portions, 1 weight portion
After 5.0% acetic acid dilute solution (aqueous solution) mixing, under the temperature conditions of 50 DEG C, carry out sol-gel anti-
Answer 3 hours.
Then, add and embodiment in the silane coupler precursor composition obtained by described reaction
The delivery in hot weather acid of the conductive-polymer solution of the 1 identical solid content with 2.0 weight % and quaternary ammonium end-blocking
(quaternary ammonium Blocked thermal acid generator, King Industries are public in agent
The CXC 1613 of department) mix, thus the backplate being prepared for liquid crystal indicator is formed with leading
Conductive composition, relative to the described compositions of 100 weight portions, described conductive-polymer solution
Addition is 30 weight portions, and the addition of the thermal acid generator of described quaternary ammonium end-blocking is 1 weight portion.
Comparative example 1
By the TEOS (tetraethoxysilane) of 15 weight portions, the IPA (isopropanol) of 9 weight portions, 13 weights
The amount propylene glycol monomethyl ether of part, the water of 27 weight portions, the acetylacetone,2,4-pentanedione of 5 weight portions, 1 weight portion
After 5.0% acetic acid dilute solution (aqueous solution) mixing, under the temperature conditions of 50 DEG C, carry out sol-gel anti-
Answer 3 hours.
Then, add and embodiment in the silane coupler precursor composition obtained by described reaction
The conductive-polymer solution of the 1 identical solid content with 2.0 weight %, thus it is prepared for electric conductivity
Compositions, the addition of wherein said conductive-polymer solution is 30 weight portions.Now, electric conductivity
Solid content electroconductive polymer that macromolecular solution comprises 2.0 weight % is (by EDOT monomer be used as
PEDOT/PSS prepared by the polymerization of the PSSA of alloy) and the water of 98 weight %.
Experimental example
Each conductive composition of described embodiment 1 to 5 and comparative example 1 is coated with the thickness of 0.5 μm
Overlay on after being formed on the electrode of substrate, on the hot plate of 120 DEG C soft roasting 600 seconds, to form thickness
Film layer for 300nm.
The reliability assessment of the backplate formation conductive material being coated on substrate make use of following
Method, the results are shown in table 1.
Room temperature reliability is estimated under the conditions of normal epidemic disaster (Rh less than 50%).High temperature can
Persistently it is placed in 80 DEG C of baking ovens by property and is estimated.It addition, high temperature/high humidity reliability assessment profit
With 65 DEG C, the hot and humid baking oven of Rh 90%.Assessment to substrate surface resistance uses SIMCO
The ST-4 equipment of company has carried out 500 hours.
[table 1]
As shown in Table 1, for using the embodiment 1 to 5 of TAG (acid agent), sour with not using product
The comparative example 1 of agent is compared, after 500 hours, in room temperature and high temperature, hot and humid reliability side
Face demonstrates outstanding result.Particularly, the result of embodiment 1 to 2 show ensure that classic
Reliability.
But, comparative example 1, due to poor reliability, is not suitable for forming electrode.
Claims (14)
1. a backplate formation conductive composition for liquid crystal indicator, comprises:
The silane coupler of 5 weight portions to 40 weight portions；
The solvent of 50 weight portions to 90 weight portions；
The hydrochloric acid of 0.1 weight portion to 10.0 weight portions or acetic acid dilute solution；
The conductive-polymer solution of 5 weight portions to 40 weight portions, it has 0.1 weight % to 5.0 weight %
Solid content；And
The acid agent of 0.001 weight portion to 1.0 weight portions.
The backplate formation conductive composition of liquid crystal indicator the most according to claim 1,
Wherein:
Described acid agent is selected from amine end-blocking, covalent bond end-blocking, metal end-blocking and the thermal acid generator of quaternary ammonium end-blocking
In at least one.
The backplate formation conductive composition of liquid crystal indicator the most according to claim 1,
Wherein:
Described acid agent is selected from DBSA, p-toluenesulfonic acid, trifluoromethanesulfonic acid and to derive
At least one in thing.
The backplate formation conductive composition of liquid crystal indicator the most according to claim 1,
Wherein:
Described solvent comprises selected from i) water, ii) alcohol compound and iii) dihydroxypropane single-ether, dimethyl methyl
At least one in amide, acetylacetone,2,4-pentanedione, 1-methyl-2-pyrrole network alkanone, butyrone and ethyl lactate is molten
Agent.
The backplate formation conductive composition of liquid crystal indicator the most according to claim 4,
Wherein:
Described alcohol compound be selected from methanol, ethanol, isopropanol, ethylene glycol, butanediol, neopentyl glycol,
1,3-pentanediol, 1,4 cyclohexane dimethanol, diethylene glycol, Polyethylene Glycol, polybutylene glycol, dihydroxy first
At least one in base propane, trimethylolpropane and their derivant.
The backplate formation conductive composition of liquid crystal indicator the most according to claim 1,
Wherein:
The solid content of described its electroconductive polymer of conductive-polymer solution is that 0.1 weight % is to 5 weight %
And comprise the solvent of 95 weight % to 99.9 weight %.
The backplate formation conductive composition of liquid crystal indicator the most according to claim 6,
Wherein:
Described electroconductive polymer comprises in polyaniline, polypyrrole, polythiophene and derivant thereof at least
A kind of.
The backplate formation conductive composition of liquid crystal indicator the most according to claim 6,
Wherein:
Described electroconductive polymer comprises poly-(3,4-ethylenedioxy thiophene).
The backplate formation conductive composition of liquid crystal indicator the most according to claim 8,
Wherein:
Described electroconductive polymer also comprises selected from DBSA, toluenesulfonic acid, camphorsulfonic acid, benzene
Sulfonic acid, hydrochloric acid, styrene sulfonic acid, 2-acrylamide-2-methylpro panesulfonic acid, their salt compound, 2-
Sulfosuccinate ester salt, 5-sulfo isophthalate sodium salt, Sodium Dimethyl Isophthalate-5-sulfonate, isophthalic
At least one alloy in double (beta-hydroxyethyl the ester)-5-sodium sulfonates of dioctyl phthalate and poly-(4-styrene sulfonate).
The backplate formation electric conductivity of liquid crystal indicator the most according to claim 6 combines
Thing, wherein:
Described electroconductive polymer use poly-(3,4-ethylenedioxy thiophene): poly-(4-styrene sulfonate) i.e.
PEDOT:PSS。
The backplate formation electric conductivity of 11. liquid crystal indicators according to claim 1 combines
Thing, wherein:
Described silane coupler be selected from have the alkoxyl silicone alkanes of C1 to C20 alkyl, amino silicone alkanes,
Vinyl silanes class, epoxy radicals silicone hydride class, methacryloxypropyl silane class, isocyanatosilanes class and fluorine
At least one of base silane apoplexy due to endogenous wind.
The backplate formation electric conductivity of 12. liquid crystal indicators according to claim 1 combines
Thing, also comprises surfactant, relative to the described total composition of 100 weight portions, described surfactant
Content be 0.1 to 1 weight portion.
The backplate formation electric conductivity of 13. liquid crystal indicators according to claim 1 combines
Thing, also comprises at least in polyacrylic resin, polyurethane resin, epoxy resin and polyester resin
Plant adhesive resin, relative to the described conductive composition of 100 weight portions, containing of described adhesive resin
Amount is that 0.1 weight portion is to 30 weight portions.
14. 1 kinds of liquid crystal display device face electrodes, by the conductive composition shape described in claim 1
Become.
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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105814644A true CN105814644A (en) | 2016-07-27 |
| CN105814644B CN105814644B (en) | 2018-08-24 |
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|---|---|---|---|
| CN201480067695.3A Active CN105814644B (en) | 2013-12-12 | 2014-11-12 | conductive composition for forming back electrode of liquid crystal display device |
Country Status (4)
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|---|---|
| JP (1) | JP6728045B2 (en) |
| KR (1) | KR20150068685A (en) |
| CN (1) | CN105814644B (en) |
| WO (1) | WO2015088146A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811009A (en) * | 2017-01-25 | 2017-06-09 | 新应材股份有限公司 | Conductive polymer composites solution and its antistatic film and flat-panel screens |
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| Publication number | Priority date | Publication date | Assignee | Title |
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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 |
Citations (4)
| 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 |
| US20120154976A1 (en) * | 2010-12-15 | 2012-06-21 | Samsung Electro-Mechanics Co., Ltd. | Conductive paste composition for inner electrode, laminated ceramic electronic part using the same and manufacturing method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| JP2004206082A (en) * | 2002-11-20 | 2004-07-22 | Rohm & Haas Electronic Materials Llc | Multilayer photoresist system |
| 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 |
-
2013
- 2013-12-12 KR KR1020130154635A patent/KR20150068685A/en not_active Application Discontinuation
-
2014
- 2014-11-12 CN CN201480067695.3A patent/CN105814644B/en active Active
- 2014-11-12 JP JP2016538648A patent/JP6728045B2/en active Active
- 2014-11-12 WO PCT/KR2014/010859 patent/WO2015088146A1/en active Application Filing
Patent Citations (4)
| 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 |
| US20120154976A1 (en) * | 2010-12-15 | 2012-06-21 | Samsung Electro-Mechanics Co., Ltd. | Conductive paste composition for inner electrode, laminated ceramic electronic part using the same and manufacturing method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811009A (en) * | 2017-01-25 | 2017-06-09 | 新应材股份有限公司 | Conductive polymer composites solution and its antistatic film and flat-panel screens |
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| Publication number | Publication date |
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| JP6728045B2 (en) | 2020-07-22 |
| JP2017502337A (en) | 2017-01-19 |
| WO2015088146A1 (en) | 2015-06-18 |
| CN105814644B (en) | 2018-08-24 |
| KR20150068685A (en) | 2015-06-22 |
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