CN106164711A - Low refractive composition and preparation method thereof and nesa coating - Google Patents
Low refractive composition and preparation method thereof and nesa coating Download PDFInfo
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- CN106164711A CN106164711A CN201580018312.8A CN201580018312A CN106164711A CN 106164711 A CN106164711 A CN 106164711A CN 201580018312 A CN201580018312 A CN 201580018312A CN 106164711 A CN106164711 A CN 106164711A
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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Abstract
The present invention provides and comprises organopolysiloxane (organopolysiloxane) and the average diameter low refractive composition of inorganic particulate being about 30nm to about 70nm and preparation method thereof and nesa coating.
Description
Technical field
The present invention relates to low refractive composition and preparation method thereof and nesa coating.
Background technology
There is the electricity such as the smart mobile phone of touch screen function, panel computer, ATM, notebook computer, TV (TV)
Subset includes to be reacted by touch, thus inputs information or the touch panel of operation and liquid crystal display
Or the display device such as Organic Light Emitting Diode (OLED) (LCD).
Typically, touch panel comprises nesa coating, thus can realization transparency and electric conductivity simultaneously, and then play logical
Cross and touch the performance reacted.Further, such as, touch panel according to detection position method have ultrasound wave mode,
Capacitance-type, the touch panel etc. of resistive film mode, successively can be by comprising nesa coating, such as, and Optical transparent adhesive
The light of (OCA, optically clear adhesive), optical clear resin (OCR, Optically Clear Resin) etc.
The duplexer learning the multiple structure with adhesive film, glass substrate or transparent plastic substrate etc. is formed.
This nesa coating includes that substrate layer and conductive layer etc., above-mentioned conductive layer comprise by conductive materials, such as, aoxidize
The electrode that indium stannum (ITO) is formed, generally, with roll forming state winding or is circulated by multiple thin film stackings, but thus there is transparent leading
Electrolemma mutually clings, and during being launched to be applicable to touch panel, there is the performance of nesa coating
The problem declined.
And, as the material of the electrode forming conductive layer, in addition to tin indium oxide, it be also possible to use nano silver wire etc.,
And in the case of using this material, the amplitude of electrode pattern or width increase relatively, thus can not meet refractive index match
Property, cause the consumer using product can observe by the naked eye electrode pattern so that visuality likely declines.
Summary of the invention
The technical problem to be solved in the present invention
In an example of the present invention, it is provided that realize outstanding anti performance and outstanding optics physical property, and prevent from leading
The low refractive composition electrically declined.
In another example of the present invention, it is provided that the preparation method of above-mentioned low refractive composition.
In another example of the present invention, it is provided that include the forming low-refractive-index layer formed by above-mentioned low refractive composition, realize
Outstanding anti performance, outstanding optics physical property and the nesa coating of outstanding electric conductivity.
Technical scheme
In an example of the present invention, it is provided that comprise organopolysiloxane and average diameter is about 30nm to about 70nm's
The low refractive composition of inorganic particulate.
Relative to the above-mentioned organopolysiloxane of about 100 weight portions, can include about 0.5 weight portion to about 20 weight portions
Above-mentioned inorganic particulate.
Above-mentioned organopolysiloxane can comprise the choosing freely alkyl of 1 to 18 carbon number, 1 to 18 carbon number
Alkoxyl, the ester group of 2 to 6 carbon numbers, the epoxy radicals of 2 to 12 carbon numbers, the thiazolinyl of 2 to 12 carbon numbers, 6 to
The aryl of 12 carbon numbers, the acrylic of 3 to 18 carbon numbers, glycidyl, amido, mercapto, halogen radical and
At least one functional group in the group of combinations thereof composition.
Above-mentioned organopolysiloxane can include linear structure, network structure, or above-mentioned organopolysiloxane can be same
Time include linear structure and network structure.
Above-mentioned organopolysiloxane can be by the silane of the silane compound and formula 2 below comprising formula 1 below
The compositions generation sol gel reaction of compound forms,
Chemical formula 1:
R1 xSi(OR2)4-x
Chemical formula 2:
Si(OR3)4
In above-mentioned chemical formula 1, above-mentioned R1Be the alkyl of 1 to 18 carbon number, the ester group of 2 to 6 carbon numbers, 2
To the epoxy radicals of 12 carbon numbers, the thiazolinyl of 2 to 12 carbon numbers, the aryl of 6 to 12 carbon numbers, 3 to 18 carbon
The acrylic of atomic number, glycidyl, amido, mercapto or halogen radical, above-mentioned R2And above-mentioned R3Be each independently H or 1 to
The alkyl of 18 carbon numbers, above-mentioned x is 1,2 or 3.
Before there is above-mentioned sol gel reaction, above-mentioned low refractive composition the most also can comprise
State inorganic particulate.
The weight average molecular weight of above-mentioned organopolysiloxane can be about 3000g/mol to about 55000g/mol.
Above-mentioned inorganic particulate can comprise choosing free silicon dioxide granule, aluminium oxide particles, Zirconia particles, titanium oxide grain
At least one particle in the group of son, stibium oxide particle and combinations thereof composition.
Above-mentioned low refractive composition can not comprise substituted or unsubstituted unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure, or also may be used
Comprise substituted or unsubstituted unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure.
In another example of the present invention, it is provided that include that the transparent of forming low-refractive-index layer formed by above-mentioned low refractive composition is led
Electrolemma.
Upper side at above-mentioned forming low-refractive-index layer can be formed with micro concavo-convex；Above-mentioned micro concavo-convex can pass through above-mentioned inorganic particulate
Formed.
The thickness of above-mentioned forming low-refractive-index layer can be about 10nm to about 50nm.
The refractive index of above-mentioned forming low-refractive-index layer can be about 1.40 to about 1.50.
High refracting layer and substrate layer is may also be formed with successively in the bottom of above-mentioned forming low-refractive-index layer；Upper at above-mentioned forming low-refractive-index layer
Portion may also be formed with conductive layer.
The present invention may also include the hard conating that the one or both sides with above-mentioned substrate layer connect.
The light transmittance of above-mentioned nesa coating can be about more than 85%, and mist degree can be about 0.1% to about 0.8%.
In another example of the present invention, it is provided that the preparation method of low refractive composition, the system of above-mentioned low refractive composition
Preparation Method includes: the mixing silane compound of formula 1 below, the silane compound of formula 2 below and average diameter are
The inorganic particulate of about 30nm to about 70nm, prepares the step of the feedstock composition comprising mentioned component；And make above-mentioned raw materials
Compositions generation sol gel reaction, prepares the step of low refractive composition.
Chemical formula 1:
R1 xSi(OR2)4-x
Chemical formula 2:
Si(OR3)4
In above-mentioned chemical formula 1, above-mentioned R1Be the alkyl of 1 to 18 carbon number, the ester group of 2 to 6 carbon numbers, 2
To the epoxy radicals of 12 carbon numbers, the thiazolinyl of 2 to 12 carbon numbers, the aryl of 6 to 12 carbon numbers, 3 to 18 carbon
The acrylic of atomic number, glycidyl, amido, mercapto or halogen radical, above-mentioned R2And above-mentioned R3Be each independently H or 1 to
The alkyl of 18 carbon numbers, above-mentioned x is 1,2 or 3.
Silane compound relative to the silane compound of above-mentioned chemical formula 1 of about 100 weight portions and above-mentioned chemical formula 2
Summation, can mix the above-mentioned inorganic particulate of about 0.5 weight portion to about 20 weight portions to prepare above-mentioned raw materials compositions.
In the period that above-mentioned sol gel reaction occurs, between above-mentioned silane compound, mutually there is chemical reaction
Form organopolysiloxane.
Beneficial effect
Above-mentioned low refractive composition is capable of outstanding anti performance and outstanding optics physical property, and prevents electric conductivity
Decline.
Accompanying drawing explanation
(a) part of Fig. 1 and two kinds of examples of the nesa coating that (b) part is the different instances representing the present invention of Fig. 1
The diagrammatic cross-sectional view in each cross section shown.
Detailed description of the invention
Hereinafter, referring to the drawings the example of the present invention is described in detail, it is possible to make the general of the technical field of the invention
Logical technical staff easily implements the present invention.The present invention can realize with multiple different form, it is not limited to described herein
Example.
In order to clearly state the present invention, eliminate and unrelated part be described, in the specification, for identical or class
As structural element, mark identical reference.
In the drawings, in order to explicitly indicate that multilamellar and region, enlarged representation thickness.Further, in the drawings, for the ease of saying
Bright, illustrate the thickness in a part of layer and region turgidly.
Hereinafter, " upper (under or) " at " top (or the bottom) " of base material or base material forms arbitrary structures, does not mean onlys that
Arbitrary structures connects with (or following) above of above-mentioned base material and formed, and is not limited to above-mentioned base material and is formed at base material
Other structures are not included between the arbitrary structures of upper (under or).
Low refractive composition
The one example offer of the present invention comprises organopolysiloxane (organopolysiloxane) and average diameter is
The low refractive composition of the inorganic particulate of e.g., from about 30nm to about 70nm.Specifically, the average diameter of above-mentioned inorganic particulate is permissible
It is about 35nm to about 60nm.
Typically, nesa coating with roll forming state winding or is circulated by multiple thin film stackings, but thus, nesa coating phase
Cling mutually, and during being launched to be applicable to touch panel etc. or be separated, the performance of nesa coating
Likely decline.Thus, in the process of circulation, in order to prevent being attached to each other between nesa coating, can be by making inorganic particulate
It is included in hard conating, forms protuberance, to reduce the area that they connect, thus degree of adhesion can be made to die down, thus, play
Can be in the case of the performance not reducing nesa coating, the anti performance launched or be separated.
Simply, as resin glue, in the hard painting compositions comprise acrylic resin etc., inorganic particulate is comprised
In the case of, the compatibility between acrylic resin and inorganic particulate is low, when the thing considering the proportion of resin glue, surface energy etc.
Property and during the thickness of hard conating, in order to form protuberance at hard conating, need to comprise the inorganic particulate that average diameter is big, thus add
Man-hour appearance fraction defective and mist degree increase, cause the problem that the electric conductivity that there is optics physical property and conductive layer more declines.
Further, as the material of the electrode forming conductive layer, in addition to tin indium oxide, it be also possible to use nano silver wire etc.,
And in the case of using this material, the amplitude of electrode pattern or width increase relatively, thus can not meet refractive index match
Property, cause the consumer using product can observe by the naked eye electrode pattern so that refractive index match or visuality have can
Can decline.
To this, in one example, the low refractive composition comprise organopolysiloxane comprises inorganic particulate, thus
Improve the compatibility between the composition being included in above-mentioned low refractive composition, and when considering the proportion of organopolysiloxane, table
Face can etc. physical property and during the thickness of forming low-refractive-index layer, it is possible to reduce realizing anti performance with suitable level, i.e. tissue adhesion
The average diameter of the inorganic particulate needed for performance.
Thus, the nesa coating including the forming low-refractive-index layer formed by above-mentioned low refractive composition realizes outstanding anti
Performance, and during applying above-mentioned low refractive composition, reduce the fraction defective of appearance, and realize with suitable level
Refractive index and mist degree, thus have and be capable of outstanding refractive index match, outstanding visuality and outstanding optics thing
The advantage of property.Further, like this, by reducing the mean diameter of above-mentioned inorganic particulate with suitable level, be more prone to into
Row forms annealing operation (annealing process) adjoint during conductive layer on the top of above-mentioned forming low-refractive-index layer, thus can drop
The resistance of low conductive layer, thus outstanding electric conductivity can be realized.
Above-mentioned low refractive composition, relative to the above-mentioned organopolysiloxane of about 100 weight portions, such as, can include about
The above-mentioned inorganic particulate of 0.5 weight portion to about 20 weight portions, specifically, can include about the above-mentioned of 7 weight portions to about 13 weight portions
Inorganic particulate.Outstanding anti performance and low-refraction can be realized by comprising above-mentioned inorganic particulate with above-mentioned scope, and
Maintain mist degree with suitable level, thus realize outstanding optics physical property and outstanding visuality simultaneously.
Specifically, in the case of the above-mentioned inorganic particulate comprising less than about 0.5 weight portion, it is possible to can not fully realize
Tissue adhesion performance, in the case of the above-mentioned inorganic particulate comprising greater than about 20 weight portions, after conductive layer film forming, hinders conduction
Layer crystallinity, thus there is the problem reducing electrical characteristics.
Above-mentioned inorganic particulate such as can comprise choosing free silicon dioxide granule, aluminium oxide particles, Zirconia particles, titanium oxide
At least one particle in the group of particle, stibium oxide particle and combinations thereof composition.
In the past, hard painting compositions is mixed with the inorganic particulate of powder morphology, thus occurs to condense or in coating work
Sequence precipitates, thus anti performance and low-refraction can not be realized equably.
In one example, above-mentioned low refractive composition comprises the inorganic particulate of colloidal sol (sol) form, i.e. containing inorganic grain
The colloidal sol of son, thus dispersibility can be improved, thereby, it is possible to all realize anti performance and low-refraction with uniform level.
That is, above-mentioned inorganic particulate is dispersed among disperseing matchmaker to be comprised with the form of dispersion sol.
Such as, above-mentioned inorganic particulate is as being scattered in such as the form of the dispersion matchmaker such as water or organic solvent, it is possible to above-mentioned nothing
The solid component content of machine particle about 5 percentage by weight is comprised to the colloidal of about 40 percentage by weights, but does not limit to
In this.As can use for the organic solvent of above-mentioned dispersion matchmaker can use methanol (methanol), isopropanol (IPA,
Isopropyl alcohol), ethylene glycol (ethylene glycol), the alcohols such as butanol (butanol)；Methyl ethyl ketone
The ketones such as (methyl ethyl ketone), methylisobutylketone (MIBK, methyl iso butyl ketone)；Toluene
(toluene), the hydrocarbon class of aromatic series such as dimethylbenzene (xylene)；Dimethylformamide (dimethyl formamide), diformazan
The amide-types such as yl acetamide (dimethyl acetamide), N-Methyl pyrrolidone (N-methyl pyrrolidone)；Second
The esters such as acetoacetic ester (ethyl acetate), butyl acetate (butyl acetate), gamma-butyrolacton (γ-butyrolactone)
(ester) class；Ether (ether) classes such as oxolane (tetrahydrofuran), Isosorbide-5-Nitrae-dioxanes (Isosorbide-5-Nitrae-dioxane) or it
Mixture.
Such as, the average diameter of above-mentioned inorganic particulate can be about 30nm to about 70nm, specifically, can be about 35nm extremely
About 60nm.
The average diameter of above-mentioned inorganic particulate means to measure the meansigma methods of the diameter of each particle.By having above-mentioned model
Enclose interior average diameter, be adequately formed protuberance at forming low-refractive-index layer, thus outstanding anti performance can be realized, even if sending out
Raw micro concavo-convex phenomenon, when Conductive Layer Etch, also will not reduce visuality, thus can realize outstanding visuality, and prevent
At forming low-refractive-index layer generation resistance, and then outstanding electric conductivity can be realized, thus priming coat can be performed in conductive layer bottom fully
Effect.
Specifically, in the case of the average diameter of above-mentioned inorganic particulate is less than about 30nm, owing to the size of particle is the least
And anti performance can not be played, in the case of the average diameter of above-mentioned inorganic particulate is greater than about 70nm, in above-mentioned low refraction
During conductive layer is formed at the top of layer, it is necessary to be suitable for annealing operation, but owing to the average diameter of above-mentioned inorganic particulate is too big,
Hindering annealing operation, thus, the resistive of conductive layer increases so that electric conductivity more declines, and causes and there is a possibility that touch panel
Etc. breaking down, and there is the problem that optics physical property declines owing to mist degree increases.And, to the two sides being laminated in forming low-refractive-index layer
High refracting layer and the cohesive force of conductive layer be also possible to more reduce.
In one example, above-mentioned low refractive composition such as can include about 10 percentage by weights to about 80 percentage by weights
Above-mentioned organopolysiloxane.By comprising the content in above-mentioned scope, it is possible to realize refractive index with the lowest level, and hold
It is easily formed forming low-refractive-index layer.
Above-mentioned organopolysiloxane can comprise the choosing freely alkyl of 1 to 18 carbon number, 1 to 18 carbon number
Alkoxyl, the ester group of 2 to 6 carbon numbers, the epoxy radicals of 2 to 12 carbon numbers, the thiazolinyl of 2 to 12 carbon numbers, 6 to
The aryl of 12 carbon numbers, the acrylic of 3 to 18 carbon numbers, glycidyl, amido, mercapto, halogen radical and
At least one functional group in the group of combinations thereof composition.By comprising above-mentioned functional group, can hold in various organic solvents
Easily there is chemical reaction so that operation and the compatibility are outstanding, can easily be coated on various base material, and realize outstanding attachment
Property.
Above-mentioned aryl means that all elements of the substituent group of annular has p track (p-orbital), and these p tracks
Form the substituent group of conjugation (conjugation).Concrete example has phenyl, aryl etc..Further, the example of above-mentioned halogen radical have F ,-
Cl ,-Br ,-I etc..
Further, above-mentioned organopolysiloxane can include linear structure, network structure, or above-mentioned organopolysiloxane
Linear structure and network structure can be included simultaneously.That is, above-mentioned organopolysiloxane can be by siloxane bond, i.e. Si-O-Si key
Combine with chain structure and be formed as linear structure, and be formed as network structure with stereochemical structure combination, may also be formed as simultaneously
Including linear structure and network structure.Further, above-mentioned network structure can include the structure that part is opened by above-mentioned functional group, specifically
Ground, it may include by above-mentioned functional group, the structure that above-mentioned cancellated bound fraction disconnects and is opened.
In the case of above-mentioned organopolysiloxane includes linear structure, solid speed is slow, thus can realize outstanding
Process stability, in the case of being coated on base material, flatness is more excellent, thus when forming conductive layer, such as, easily real
The crystallization of existing tin indium oxide (ITO, Indium Tin Oxide), thus electric conductivity can be improved.On the other hand, above-mentioned organic
In the case of polymolecular silicon ether includes network structure, due to architectural characteristic, outstanding chemical resistance and outstanding resistance to molten can be realized
Agent, thus, is not subject to the etching work procedure needed for formation conductive layer or the acidity used in washing step or alkaline chemical
The impact of matter, thus outstanding stability can be realized.
The weight average molecular weight of above-mentioned organopolysiloxane can be about 3000g/mol to about 55000g/mol.By tool
There is the weight average molecular weight in above-mentioned scope, favourable in terms of regulation thickness when forming forming low-refractive-index layer, and can easily realize uniformly
Maintain the effect of surface roughness.
Above-mentioned organopolysiloxane can be by the silane of the silane compound and formula 2 below comprising formula 1 below
The feedstock composition generation sol gel reaction of compound forms.
Chemical formula 1:
R1 xSi(OR2)4-x
Chemical formula 2:
Si(OR3)4
In above-mentioned chemical formula 1, above-mentioned R1Be the alkyl of 1 to 18 carbon number, the ester group of 2 to 6 carbon numbers, 2
To the epoxy radicals of 12 carbon numbers, the thiazolinyl of 2 to 12 carbon numbers, the aryl of 6 to 12 carbon numbers, 3 to 18 carbon
The acrylic of atomic number, glycidyl, amido, mercapto or halogen radical, above-mentioned R2And above-mentioned R3Be each independently H or 1 to
The alkyl of 18 carbon numbers, above-mentioned x is 1,2 or 3.
Above-mentioned aryl means that all elements of the substituent group of annular has p track, and these p tracks form conjugation
(conjugation) substituent group.Concrete example has phenyl, aryl etc..Further, the example of above-mentioned halogen radical has F ,-Cl ,-Br ,-I
Deng.
Above-mentioned sol gel reaction may imply that the precursor molecule generation hydrolysis such as silane compound etc., condensation are anti-
Should, dehydration condensation, hydrolysis-condensation reaction etc., cause linear structure, tridimensional network etc. form the reaction of cross-bonds.
In the period of above-mentioned raw materials compositions generation sol gel reaction, mutually occur between above-mentioned silane compound
Chemical reaction, can form above-mentioned organopolysiloxane.Such as, the silane compound of above-mentioned chemical formula 1 mutually reacts,
Or the silane compound of above-mentioned chemical formula 2 mutually reacts, or the silane compound of above-mentioned chemical formula 1 and above-mentioned chemistry
The silane compound of formula 2 mutually reacts, or reacts with combinations thereof form, can form above-mentioned organic many points
Sub-silicon ether.
Above-mentioned chemical reaction such as can include selecting free hydrolysis, condensation reaction, dehydration condensation, hydrolysis-condensation
At least one in the group of reaction and combinations thereof composition, by performing above-mentioned chemical reaction, carrys out the silanization at chemical formula 1
Compound, siloxane bond between the silane compound of above-mentioned chemical formula 2 or all of which, can be formed, i.e. Si-O-Si key, thus, can
Form above-mentioned organopolysiloxane.
Such as, the silane compound of above-mentioned chemical formula 1 can comprise selected from comprise trimethoxy silane, triethoxysilane,
MTMS, MTES, ethyl trimethoxy silane, ethyl triethoxysilane, n-pro-pyl three
Methoxy silane, n-pro-pyl triethoxysilane, isobutyl triethoxy silane, cyclohexyl trimethoxy silane, phenyl front three
TMOS, phenyl triethoxysilane, vinyltrimethoxy silane, VTES, pi-allyl trimethoxy
Base silane, allyltriethoxysilane, dimethyldimethoxysil,ne, dimethyldiethoxysilane, diphenyl dimethoxy
Base silane, diphenyl diethoxy silane, trichloromethyl silane, trichlorine chloromethyl silane, trichlorine dichloro methyl silane, tetrachloro silicon
Alkane, dimethoxydimethylsilane, triacetic acid vinyl silanes, trichlorine octadecylsilane, trichlorine octyl group silane, acryloyl-oxy
Propyl trimethoxy silicane, acryloxypropyl triethoxysilane, methacryloxypropyl trimethoxy silane, methyl
Acryloxypropyl triethoxysilane, methacryloxymethyl trimethoxy silane, methacryloxymethyl
Triethoxysilane, methacryloxymethyl methyl dimethoxysilane, methacryloxymethyl methyl diethoxy
Base silane, methacryloyloxypropyl methyl dimethoxysilane, methacryloyloxypropyl methyl diethoxy silane,
Methacryloxypropyl dimethyl methoxy silane, methacryloxypropyl dimethylethoxysilane, epoxide ring
Hexyl ethyl trimethoxy silane, glycidylpropyl trimethoxy silane, glycidylpropyl methyldiethoxysilane, contracting
Water glycerol propyl-triethoxysilicane, octadecyl trimethoxysilane (stearyl trimethoxysilane), aminoethyl
Trimethoxy silane, aminopropyl trimethoxysilane, aminoethyl triethoxysilane, aminopropyl triethoxysilane, three ethoxies
In the group of base silicyl dimethyl butyrate subunit propylamine, phenylamino propyl trimethoxy silicane and combinations thereof at least one
Kind.
The silane compound of above-mentioned chemical formula 2 can comprise selected from comprising tetramethoxy-silicane, tetraethoxysilane, 4 third oxygen
Base silane, tetraisopropoxysilan, four n-butoxy silane, four sec-butoxy silane, four tert-butoxy silane and their group
At least one in the group closed.
In one example, silane compound and the above-mentioned chemical formula 2 of the above-mentioned chemical formula 1 of above-mentioned raw materials compositions it are included in
The weight ratio of silane compound can be about 1:5 to about 1:99.By comprising with the weight ratio in above-mentioned scope, can suitably adjust
Joint is included in the organic moiety of above-mentioned organopolysiloxane and the content of inorganic part, thus realizes outstanding refractive index match
Property, outstanding tack and oxidative resistance.Specifically, at silane compound and the silane of above-mentioned chemical formula 2 of above-mentioned chemical formula 1
In the case of the weight ratio of compound is less than about 1:5, owing to organic moiety is too many, cause coating because of spendable during washing step
Alkaline chemical and damage, it is possible to change refractive index match, and, at the silane compound of above-mentioned chemical formula 1
In the case of being greater than about 1:99 with the weight ratio of the silane compound of above-mentioned chemical formula 2, owing to inorganic part is too many, cause coating
Pliability decline, it is possible to reduce tack and oxidisability.
Above-mentioned raw materials compositions such as can include about the above-mentioned chemical formula 1 of 1 percentage by weight to about 19 percentage by weights
Silane compound, but be not limited thereto.
In one example, before there is above-mentioned sol gel reaction, in above-mentioned low refractive composition in a mixed way
Also comprise above-mentioned inorganic particulate.Above-mentioned organopolysiloxane formed and in the compositions that comprised in a mixed way also
In the case of comprising above-mentioned inorganic particulate, dispersibility likely declines.To this, above-mentioned low refractive composition is by making to comprise simultaneously
The silane compound of above-mentioned chemical formula 1 and the compositions generation sol gel reaction of above-mentioned inorganic particulate, make above-mentioned inorganic grain
Can be effective between the above-mentioned organopolysiloxane of son reaction result thing between the silane compound as above-mentioned chemical formula 1
Ground dispersion, and it is possible to realize anti performance, low-refraction and optics physical property with level evenly.
Typically, in the case of conductive layer is formed at the top of forming low-refractive-index layer, under vacuum, such as, sputtering method is passed through
Perform the film forming of conductive layer.
Under above-mentioned vacuum condition, above-mentioned low refractive composition comprises above-mentioned unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure
In the case of, it is possible to discharge as VOC (VOC, volatile from the forming low-refractive-index layer being consequently formed
Organic compounds) above-mentioned unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure, thus hinder formed above-mentioned conductive layer time annealing
Operation, accordingly, there are the problem making electric conductivity decline because the resistive of above-mentioned conductive layer increases.And, at hot and humid bar
Under part, in above-mentioned forming low-refractive-index layer, there is migration (migration) phenomenon of above-mentioned unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure so that
Mist degree increases, and then makes surface characteristic likely decline, and thus, optics physical property and electric conductivity are also possible to reduce.
To this, in one example, above-mentioned low refractive composition can not comprise substituted or unsubstituted unimolecule alkoxyl silicone
Hydride compounds, or also can comprise substituted or unsubstituted unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure.Specifically, replacement can not be comprised
Or unsubstituted unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure, thus, do not discharge as volatile organic compound when forming conductive layer
The unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure of thing, thus annealing operation can be easily performed, and then outstanding electric conductivity can be realized, with this
Meanwhile, under the conditions of hot and humid, prevent transport phenomena, thus maintain mist degree and surface characteristic, so can realize outstanding can
By property.
In this manual, as long as no extra definition, " replacement " mean that by halogen atom (F, Cl, Br or I),
Hydroxyl, nitro, cyano group, amino, carboxyl, the alkyl of 1 to 30 carbon number, the cycloalkyl of 3 to 30 carbon numbers, 6 to 30
The aryl of individual carbon number or the alkoxyl of 1 to 30 carbon number replace.Abovementioned alkyl can be straight chain type or branching type.
Above-mentioned unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure is to comprise the implication of known all kinds, example in this technical field
As, can comprise the silane compound selected from above-mentioned chemical formula 1 plants at least one of apoplexy due to endogenous wind, but is not limited thereto.
Above-mentioned low refractive composition also can comprise the free acid catalyst of choosing, water, organic solvent and combinations thereof composition
At least one in group.
Above-mentioned acid catalyst such as can use mineral acid or organic acid, specifically, can use nitric acid, hydrochloric acid, sulphuric acid or vinegar
Acid etc..
Above-mentioned organic solvent such as can comprise choosing free methanol, isopropanol, ethylene glycol (ethylene glycol), butanol
Deng alcohols；The ketone such as methyl ethyl ketone, methylisobutylketone；Ester (ester) classes such as ethyl acetate, butyl acetate, gamma-butyrolacton；
At least one in the group of ether (ether) classes such as oxolane, Isosorbide-5-Nitrae-dioxanes and combinations thereof composition.
Nesa coating
In another example of the present invention, it is provided that include that the transparent of forming low-refractive-index layer formed by above-mentioned low refractive composition is led
Electrolemma.Above-mentioned low refractive composition is as described in one example, and above-mentioned forming low-refractive-index layer is endowed anti performance, thus can perform
Effect as tissue adhesion forming low-refractive-index layer.
Thus, the nesa coating comprising above-mentioned forming low-refractive-index layer realizes outstanding anti performance, and above-mentioned low in coating
During refractive composition, reduce the fraction defective of appearance, and be horizontally formed refractive index and mist degree with suitable, thus have
Have and can realize outstanding refractive index match, outstanding visuality and the advantage of outstanding optics physical property.Further, so, pass through
Reduce the mean diameter of above-mentioned inorganic particulate with suitable level, can easily perform and form conduction on the top of above-mentioned forming low-refractive-index layer
Annealing operation adjoint during layer, thus the resistive of conductive layer can be reduced, thus outstanding electric conductivity can be realized.
Such as, as be described hereinafter, after can being formed at the above-mentioned low refractive composition of the top of high refracting layer of bottom coating, can hold
Row heat cure reaction forms above-mentioned forming low-refractive-index layer.Such as, the coating method of above-mentioned low refractive composition can use intaglio plate
(gravure) coating process, channel mould (slot die) coating process, whirl coating, spraying and applying method, rolling method, deposition coating process
Deng, but be not limited thereto.
Further, above-mentioned heat cure reaction can perform heat treatment with the temperature of about 100 DEG C to about 170 DEG C, but does not limit to
In this.
Further, after performing above-mentioned heat cure reaction, can also carry out ageing treatment process (aging process), on
State ageing treatment process to be performed by condition known in this technical field and method.
Upper side at above-mentioned forming low-refractive-index layer is formed with micro concavo-convex, and above-mentioned micro concavo-convex can be by above-mentioned inorganic particulate shape
Becoming, such as, a part for above-mentioned inorganic particulate can highlight from the surface of above-mentioned forming low-refractive-index layer, and forms above-mentioned micro concavo-convex, by
This, another part of above-mentioned inorganic particulate can exist to be buried in the state of above-mentioned forming low-refractive-index layer.Further, above-mentioned inorganic particulate
Average diameter likely more than the thickness of above-mentioned forming low-refractive-index layer, thus, it is easier to form above-mentioned micro concavo-convex.
That is, above-mentioned micro concavo-convex shape is when applying above-mentioned low refractive composition, can be about 30nm to about by average diameter
The inorganic particulate of 70nm is formed, specifically, in the case of above-mentioned low refractive composition is coated on substrate layer, due to above-mentioned nothing
The average diameter of machine particle highlights more than the thickness of forming low-refractive-index layer, thus can be more readily formed micro concavo-convex shape, thus, on
State forming low-refractive-index layer and can realize more excellent anti performance.
The thickness of above-mentioned forming low-refractive-index layer can be about 10nm to about 50nm.Thickness at above-mentioned forming low-refractive-index layer is less than about 10nm
In the case of, there is the worry making visual decline because of optical interference, the thickness at above-mentioned forming low-refractive-index layer is greater than about 50nm's
In the case of, owing to absorbance is the lowest, cause optics physical property likely to decline, thus can come by having the thickness of above-mentioned scope
Meet refractive index match, and maintain high transmission rate and low haze such that it is able to realize outstanding visuality and outstanding optics
Physical property.
Further, the refractive index of above-mentioned forming low-refractive-index layer can be about 1.40 to about 1.50.Low by have in above-mentioned scope
The refractive index of level, it is possible to all together regulate visuality and the optics of above-mentioned nesa coating with outstanding level and high refracting layer
Physical property.
(a) part of Fig. 1 and (b) part of Fig. 1 briefly express two kinds of examples of the nesa coating of different instances of the present invention
The each cross section shown.
Above-mentioned nesa coating may also be formed with high refracting layer and substrate layer successively in the bottom of above-mentioned forming low-refractive-index layer；Upper
The top stating forming low-refractive-index layer may also be formed with conductive layer.Specifically, with reference to (a) part of Fig. 1, the one side at above-mentioned substrate layer can
It is sequentially formed with high refracting layer, above-mentioned forming low-refractive-index layer and conductive layer.
Above-mentioned high refracting layer performs to improve insulation characterisitic and the effect of absorbance between substrate layer and conductive layer.Above-mentioned height
Refracting layer can be by inorganic matter, Organic substance or comprise inorganic matter and organic material is formed simultaneously.Above-mentioned inorganic matter such as has
SiO2、MgF2、Al2O3、NaF、Na3AlF6、LiF、CaF2、BaF2、LaF3、CeF3Deng, above-mentioned Organic substance such as can use melamine
Amine (melamine) resin, alkyd resin, urethane resin, acrylic resin, siloxane type polymers, organosilan
Condensation substance etc..
Such as, after above-mentioned high refracting layer can apply according to the kind of above-mentioned material, heat cure or photocuring processes, injection are used
In this technical field such as method, sputtering method, known coating method is formed.
Further, such as, the thickness of above-mentioned high refracting layer can be about 15nm to about 100nm.By maintaining above-mentioned high refraction
The thickness of layer, can improve outstanding absorbance and visuality, and reduces stress and the crackle (Crack) that occurs and curling
(Curl)。
Further, such as, the refractive index of above-mentioned high refracting layer can be about 1.65 to about 1.8.There is the height in above-mentioned scope
The refractive index of level, it is possible to all with outstanding level and above-mentioned forming low-refractive-index layer together regulate above-mentioned nesa coating visuality and
Optics physical property.
Above-mentioned substrate layer is transparent substrate layer, such as can be by comprising the free polyethylene terephthalate of choosing (PET), gathering
(ethylene naphthalate) (PEN), polyether sulfone (PES), Merlon (PC), polypropylene (PP), polrvinyl chloride (PVC), poly-second
Alkene (PE), polymethyl methacrylate (PMMA), ethylene-vinyl alcohol (EVA), polyvinyl alcohol (PVA) and combinations thereof composition
Group in the material of at least one formed, but be not limited thereto.
Further, above-mentioned substrate layer can be the thin film of single or multiple lift structure, and the gross thickness of above-mentioned substrate layer is the most permissible
It is about 20 μm to about 500 μm.
Such as, above-mentioned conductive layer can comprise choosing free tin indium oxide, zinc oxide (ZnO), zinc-tin oxide (ZTO, Zinc Tin
Oxide), fluorine-doped tin oxide (FTO, Fluorine-doped Tin Oxide), nano silver wire (aluminium-doped zinc oxide (AZO,
Al-doped ZnO)) and combinations thereof composition group at least one.
The thickness of above-mentioned conductive layer can be about 5nm to about 50nm, by maintaining above-mentioned by the thickness of above-mentioned conductive layer
In the range of, can prevent the gross thickness of above-mentioned nesa coating from excessively increasing, and realize outstanding optics physical property.
The present invention may also include the hard conating that the one or both sides with above-mentioned substrate layer connect, and thus, can fully support
State forming low-refractive-index layer and above-mentioned high refracting layer protected, improve the hardness of above-mentioned nesa coating, and suitably regulate refractive index,
Thus the phenomenons such as the destructive interference of light occur, and then can be easier to meet refractive index match.
Such as, above-mentioned hard conating can select free ultraviolet curable resin, average diameter to be about 1nm to about by making to comprise
The hard coating composition of at least one in the group of the nano inoganic particle of 30nm, Photoepolymerizationinitiater initiater and combinations thereof composition
Photocuring is formed, and the nano inoganic particle of above-mentioned average diameter about 1nm to about 30nm is buried in inside above-mentioned hard conating, from
And case hardness can be improved, but it is little to realize anti performance.Specifically, in order to give adhesion inhibiting properties to above-mentioned hard conating
Can, the average diameter of inorganic particulate should be about more than 1 μm, and like this, in the situation comprising the big inorganic particulate of average diameter
Under, when coating, it is possible to occur appearance bad, and mist degree excessively increases and causes optics physical property likely to decline, and
And, in preparation process in the case of quantity-produced, each product is likely difficult to have uniform physical property.
The thickness of above-mentioned hard conating can be about 900nm to about 2000nm.Thickness at above-mentioned hard conating is less than about 900nm
In the case of, it is impossible to realize the case hardness of above-mentioned nesa coating with sufficient level, cause durability the lowest, upper
State in the case of the thickness of hard conating is greater than about 2000nm, there is above-mentioned hard conating and likely crimp the worry of (Curling), from
And by having the thickness of above-mentioned scope, outstanding case hardness can be realized, and prevent curling.
The refractive index of above-mentioned hard conating can be about 1.45 to about 1.7, but is not limited thereto.
In another example, the light transmittance of above-mentioned nesa coating can be about more than 85%, and mist degree can be about 0.1%
To about 0.8%, specifically, above-mentioned light transmittance can be about 87% to about 92%.By have the light transmittance in above-mentioned scope and
Mist degree, can realize refractive index match, and realize outstanding optics physical property.In this manual, above-mentioned light transmittance and above-mentioned mist
The value that degree measures on the basis of such as meaning thickness is about the nesa coating of 100 μm.
In another example of the present invention, it is provided that the preparation method of low refractive composition, the system of above-mentioned low refractive composition
Preparation Method includes: the mixing silane compound of formula 1 below, the silane compound of formula 2 below and average diameter are
The inorganic particulate of 30nm to 70nm, prepares the step of the feedstock composition comprising mentioned component；And make above-mentioned raw materials combine
Thing generation sol gel reaction, prepares the step of low refractive composition.
Chemical formula 1:
R1 xSi(OR2)4-x
Chemical formula 2:
Si(OR3)4
In above-mentioned chemical formula 1, above-mentioned R1Be the alkyl of 1 to 18 carbon number, the ester group of 2 to 6 carbon numbers, 2
To the epoxy radicals of 12 carbon numbers, the thiazolinyl of 2 to 12 carbon numbers, the aryl of 6 to 12 carbon numbers, 3 to 18 carbon
The acrylic of atomic number, glycidyl, amido, mercapto or halogen radical, above-mentioned R2And above-mentioned R3Be each independently H or 1 to
The alkyl of 18 carbon numbers, above-mentioned x is 1,2 or 3.That is, can prepare the most aforesaid by above-mentioned preparation method
Low refractive composition, the silane compound of above-mentioned chemical formula 1, above-mentioned chemical formula 2 silane compound as described in one example.
Such as, relative to the silane compound of above-mentioned chemical formula 1 and the silane chemical combination of above-mentioned chemical formula 2 of 100 weight portions
The summation of thing, can mix the above-mentioned inorganic particulate of about 0.5 weight portion to about 20 weight portions to prepare above-mentioned raw materials compositions, specifically
Ground, can include about the above-mentioned inorganic particulate of 7 weight portions to about 13 weight portions.
Further, above-mentioned raw materials compositions also can mix the free acid catalyst of choosing, water, organic solvent and combinations thereof composition
Group at least one prepare, above-mentioned acid catalyst and above-mentioned organic solvent are as described in one example.
In the period that above-mentioned sol gel reaction occurs, can be by mutually there is chemistry between above-mentioned silane compound
Reaction forms organopolysiloxane, above-mentioned organopolysiloxane and above-mentioned chemical reaction as described in one example.
Further, so that above-mentioned low refractive composition comprises the above-mentioned organic of about 10 percentage by weights to about 80 percentage by weights
The mode of polymolecular silicon ether, can regulate respectively the above-mentioned chemical formula 1 being included in above-mentioned raw materials compositions silane compound and on
State the content sum of the silane compound of chemical formula 2, i.e. total content.
For instance, it is possible to so that the weight ratio of the silane compound of the silane compound of above-mentioned chemical formula 1 and above-mentioned chemical formula 2
The mode becoming to be about 1:5 to about 1:99 prepares above-mentioned raw materials compositions.By mixing with the weight ratio in above-mentioned scope, can be suitable
Regulation is included in organic moiety and the content of inorganic part of the above-mentioned organopolysiloxane formed, thus realizes outstanding
Refractive index match, outstanding tack and oxidative resistance.Specifically, in silane compound and above-mentionedization of above-mentioned chemical formula 1
In the case of the weight ratio of the silane compound of formula 2 is less than about 1:5, owing to organic moiety is too many, cause coating because of washing work
Spendable alkaline chemical during sequence and damage, it is possible to change refractive index match, and, at above-mentioned chemical formula 1
Silane compound and in the case of the weight ratio of silane compound of above-mentioned chemical formula 2 is greater than about 1:99, due to inorganic part
Too much, the pliability of coating is caused to decline, it is possible to reduce tack and oxidisability.
For instance, it is possible to comprise about 1 percentage by weight to the silane compound of the above-mentioned chemical formula 1 of about 19 percentage by weights
Mode prepare above-mentioned raw materials compositions, but be not limited thereto.
In above-mentioned preparation method, such as, above-mentioned sol gel reaction can at a temperature of about 20 DEG C to about 60 DEG C stir about
Within 8 hours, performed to about 48 hours, but be not limited thereto.By stirring under the conditions of temperature and time within the above range
Mix, the chemical reaction such as hydrolysis, condensation reaction can fully occur, thus be more readily formed above-mentioned organopolysiloxane.
Further, after terminating above-mentioned sol gel reaction, in the range of without departing from the scope of the present invention, can basis
The purpose of the present invention and purposes, in above-mentioned low refractive composition, suitable mixed organic solvents dilutes and uses.Above-mentioned organic
Solvent is as described in one example.
Hereinafter, the specific embodiment of the present invention is proposed.But following described embodiment only belongs to particular instantiation or explanation
The present invention, the present invention should not be limited to this.
Preparation example
The low refractive composition of preparation example 1-1.
Mix trimethoxy (methyl) silane and the tetraethoxy orthosilicate of 15 percentage by weights of 1 percentage by weight
(TEOS, tetraethoxy orthosilicate), average diameter are that (day is newly changed for the silicon dioxide granule dispersion sol of 50nm
Learn, MEK-ST-up), water, ethanol and the nitric acid of 1M, prepare feedstock composition, above-mentioned raw materials compositions is relative to 100 weight
Above-mentioned trimethoxy (methyl) silane of part and the summation of above-mentioned tetraethoxy orthosilicate, contain above-mentioned the two of 10 weight portions
Silicon oxide particle.
Further, at a temperature of 40 DEG C, above-mentioned raw materials compositions is stirred 24 hours, sol gel reaction occurs, thus
It is prepared for low refractive composition, in above-mentioned low refractive composition, by above-mentioned trimethoxy (methyl) silane and above-mentioned tetrem
Chemical reaction is mutually occurred to form organopolysiloxane between the silane compound of epoxide orthosilicate composition.
Specifically, above-mentioned low refractive composition contains the above-mentioned organopolysiloxane of about 30 percentage by weights, with 100
On the basis of the above-mentioned organopolysiloxane of weight portion, contain the above-mentioned silicon dioxide granule of 10 weight portions.
The low refractive composition of preparation example 1-2.(the silicon dioxide granule dispersion sol using average diameter to be 30nm)
Except use average diameter be 30nm silicon dioxide granule dispersion sol (day is the most chemical, MEK-ST) outside, with
The method identical with above-mentioned preparation example 1-1 is prepared for low refractive composition.
The low refractive composition of preparation example 1-3.(the silicon dioxide granule dispersion sol using average diameter to be 70nm)
Except use average diameter be 70nm silicon dioxide granule dispersion sol (day is the most chemical, IPAST-up) outside,
It is prepared for low refractive composition with the method identical with above-mentioned preparation example 1-1.
The low refractive composition of preparation example 1-4.(the silicon dioxide granule dispersion sol using average diameter to be 20nm)
Except use average diameter be 20nm silicon dioxide granule dispersion sol (day is the most chemical, IPAST) outside, with
The method that above-mentioned preparation example 1-1 is identical is prepared for low refractive composition.
The low refractive composition of preparation example 1-5.(the silicon dioxide granule dispersion sol using average diameter to be 200nm)
Except use average diameter be 200nm silicon dioxide granule dispersion sol (day is the most chemical, MEK20) outside, with
The method identical with above-mentioned preparation example 1-1 is prepared for low refractive composition.
The low refractive composition of preparation example 1-6.(not mixing silicon dioxide granule)
In addition to not mixing silicon dioxide granule, it is prepared for low refraction group with the method identical with above-mentioned preparation example 1-1
Compound.
The high refractive composition of preparation example 2.
Relative to the total solid composition of 100 weight portions, mix the ultraviolet hardening acrylate (trade name of 36 weight portions
HX-920UV, common prosperity society (Kyoeisha)), the high refraction nanoparticle (ZrO of 60 weight portions2Nanoparticle), the light of 4 weight portions
Polymerization initiator (trade name Irgacure-184, BASF), and utilize the methyl ethyl ketone (MEK) as retarder thinner to carry out
Dilution, thus it is prepared for the high refractive composition (refractive index is 1.68) that solid constituent is 5%.
Preparation example 3. painting compositions firmly
Relative to the total solid composition of 100 weight portions, mix the double pentaerythritol methacrylate of 20 weight portions
Ultraviolet hardening acrylate (trade name HX-of (dipentaerythritol hexaacrylate), 60 weight portions
920UV, common prosperity society), the silicon dioxide particles (trade name XBA-ST, Nissan Chemical) of 15 weight portions, the photopolymerization of 5 weight portions
Initiator Irgacure-184 (vapour bar (Ciba) company), and utilize the methyl ethyl ketone (MEK) as retarder thinner to carry out
Dilution, thus it is prepared for the hard painting compositions (refractive index is 1.50) that solid constituent is 45%.
Embodiment and comparative example
Embodiment 1
Utilize silk rod (Meyer bar), in the way of making the thickness of desciccator diaphragm become 1.5 μm, by the hard painting of preparation example 3
Layer composition is coated on polyethylene terephthalate (PET) film of 50 μm, utilizes the high voltage mercury lamp of 180W to irradiate
The ultraviolet of 300mJ also solidifies, thus is prepared for being formed with the thin film of hard conating in cross section.
Afterwards, on the top of above-mentioned hard conating, utilize the high refractive composition prepared by preparation example 2, so that desciccator diaphragm
Thickness become the mode of 50nm and be coated, utilize the high voltage mercury lamp of 180W to irradiate the ultraviolet of 300mJ and to solidify,
Thus define high refracting layer.
Then, on the top of above-mentioned high refracting layer, utilizing the low refractive composition prepared by preparation example 1-1, coming so that doing
The thickness of dry film becomes the mode of 20nm and is coated, and solidifies 1 minute in the baking oven of 150 DEG C of temperature, thus defines low
Refracting layer.Further, then, utilize indium: the tin indium oxide target material of the tin indium oxide of stannum=95:5, to steam on the top of forming low-refractive-index layer
After plating tin indium oxide, at a temperature of 150 DEG C, perform the heat treatment of 1 hour, be thus suitable for annealing operation to form thickness as 20nm
Conductive layer (indium tin oxide layer), and then be prepared for nesa coating.
Embodiment 2
Except use above-mentioned preparation example 1-2 low refractive composition form forming low-refractive-index layer in addition to, with above-described embodiment 1
Identical method is prepared for nesa coating.
Embodiment 3
Except use above-mentioned preparation example 1-3 low refractive composition form forming low-refractive-index layer in addition to, with above-described embodiment 1
Identical method is prepared for nesa coating.
Comparative example 1
Except use above-mentioned preparation example 1-4 low refractive composition form forming low-refractive-index layer in addition to, with above-described embodiment 1
Identical method is prepared for nesa coating.
Comparative example 2
Except use above-mentioned preparation example 1-5 low refractive composition form forming low-refractive-index layer in addition to, with above-described embodiment 1
Identical method is prepared for nesa coating.
Comparative example 3
Except use above-mentioned preparation example 1-6 low refractive composition form forming low-refractive-index layer in addition to, with above-described embodiment 1
Identical method is prepared for nesa coating.
Experimental example
Evaluate embodiment 1-3 and each nesa coating of comparative example 1-3 and the thing of each forming low-refractive-index layer being included in them
Property, and be recorded in lower list 1.
Anti performance
Assay method: shear the saturating of above-described embodiment and comparative example with the size of 10cm × 10cm (laterally × longitudinally) respectively
Bright conducting film, after preparing 10 test pieces, respectively above-mentioned 10 test pieces of stacking, put between metallic plate and be consequently formed
The thin film of 10 Rotating fields, and be pointed to the metallic plate on top at the counterweight using 5kg and execute under stressed state, at 50 DEG C
At a temperature of place after 24 hours, take out and remove one by one the thin film of above-mentioned 10 Rotating fields, and have rated adhesion inhibiting properties
Energy.The physical property of above-mentioned nesa coating will be maintained so that the information slip of anti excellent performance because above-mentioned thin film can be easily separated
It is shown as "○", is difficult to separate by above-mentioned thin film and reduces the physical property of above-mentioned nesa coating so that the situation of anti poor performance
It is expressed as "×".
Refractive index match
Assay method: outside the surface of each nesa coating being observed above-described embodiment and comparative example by naked eyes mode respectively
See, and have rated whether can see the pattern formed by the conductive materials within conductive layer.To can't see completely by above-mentioned conduction
Pattern that material is formed and in refractive index match or visual outstanding information slip is shown as "○", can obscure see and in folding
Penetrate rate matching or visuality belongs to general information slip and is shown as " △ ", and can be clearly visible and in refractive index match or can
The information slip poor depending on property is shown as "×".
Screening characteristics
Assay method: as described in above-described embodiment 1-3 and above-mentioned comparative example 1-3, form low refraction respectively at high refracting layer
After Ceng, see whether appearance generation nebulousurine, crackle or partial coagulation etc. at each forming low-refractive-index layer by naked eyes mode, and comment
Valency screening characteristics.Specifically, in the case of entirely without occurring nebulousurine, crackle or partial coagulation to make screening characteristics outstanding, table
It is shown as "○", in the case of to occur nebulousurine, crackle or partial coagulation to make screening characteristics general on a small quantity, is expressed as " △ ", bright
Show in the case of occurring nebulousurine, crackle or partial coagulation to make screening characteristics difference, be expressed as "×".
Electric conductivity
Assay method: after conductive layer film forming, carries out crystallization step, afterwards, uses resistance measuring instrument (Mitsubishi Chemical
(MITSUBISHI CHEMICAL), LORESTA-GP [MCP-T610]) measure sheet resistance, and have rated electric conductivity, and
And, according to physical law, above-mentioned sheet resistance is the lowest, and above-mentioned electric conductivity is the most outstanding.Above-mentioned surface resistance be determined as 150 Ω/ with
Lower and outstanding in electric conductivity in the case of, be expressed as "○", above-mentioned surface resistance be determined as 150～170 Ω/ and in electric conductivity one
In the case of as, be expressed as " △ ", above-mentioned surface resistance be determined as 170 Ω/more than and in poorly conductive in the case of, be expressed as
“×”。
Light transmittance and mist degree
Assay method: for each above-mentioned nesa coating, uses haze measurement instrument (hazemeter) (Japan's electricity color
(Nippon Denshoku) company, NDH5000) it is determined.The thickness of above-mentioned nesa coating is about 100 μm.
Table 1
As shown in Table 1 above, the physical property of the nesa coating of embodiment 1 to embodiment 3 is almost evaluated as outstanding level,
Especially, in the case of example 1, can confirm clearly, concurrently appear and realize anti performance, folding with outstanding level
Penetrate rate matching and electric conductivity.
On the contrary, in the case of the nesa coating of comparative example 1 and comparative example 3, silicon dioxide granule is forming conductive layer
Time do not hinder annealing operation so that being suitable for, the electric conductivity before the process of circulation is good, and especially, anti performance is evaluated as significantly
Low level, thus, can clearly predict that in the case of being wound into roll forming state or being circulated by multiple thin film stackings, they are the most viscous
Live, and can be impaired during being launched to be applicable to touch panel etc. or be separated, cause nesa coating
Performance be remarkably decreased, thus can not normally perform the effect as nesa coating.And, at the electrically conducting transparent of comparative example 2
In the case of film, refractive index match and screening characteristics are also evaluated as less than comparative example 1.
Further, the refractive index match of the nesa coating of comparative example 2, screening characteristics are evaluated as mean level, but due to mist
It is poor to spend so that optics physical property is low, and, when forming conductive layer, annealing operation is hindered by silicon dioxide granule so that conduction
The resistive of layer increases, thus it is the lowest to be evaluated as electric conductivity, thus, can clearly predict and can not normally perform as electrically conducting transparent
The effect of film.
Claims (19)
1. a low refractive composition, it is characterised in that comprise organopolysiloxane and average diameter is 30nm's to 70nm
Inorganic particulate.
Low refractive composition the most according to claim 1, it is characterised in that described organic many relative to 100 weight portions
Molecule silicon ether, comprises the described inorganic particulate of 0.5 weight portion to 20 weight portions.
Low refractive composition the most according to claim 1, it is characterised in that described organopolysiloxane comprises choosing freely
The alkyl of 1 to 18 carbon number, the alkoxyl of 1 to 18 carbon number, the ester group of 2 to 6 carbon numbers, 2 to 12 carbon
The epoxy radicals of atomic number, the thiazolinyl of 2 to 12 carbon numbers, the aryl of 6 to 12 carbon numbers, 3 to 18 carbon numbers
At least one functional group in the group of acrylic, glycidyl, amido, mercapto, halogen radical and combinations thereof composition.
Low refractive composition the most according to claim 1, it is characterised in that described organopolysiloxane includes linear junction
Structure, network structure, or described organopolysiloxane includes linear structure and network structure simultaneously.
Low refractive composition the most according to claim 1, it is characterised in that described organopolysiloxane is following by comprising
The compositions generation sol gel reaction of the silane compound of chemical formula 1 and the silane compound of formula 2 below forms,
Chemical formula 1:
R1 xSi(OR2)4-x
Chemical formula 2:
Si(OR3)4
In described chemical formula 1, described R1Be the alkyl of 1 to 18 carbon number, the ester group of 2 to 6 carbon numbers, 2 to 12
The epoxy radicals of carbon number, the thiazolinyl of 2 to 12 carbon numbers, the aryl of 6 to 12 carbon numbers, 3 to 18 carbon numbers
Acrylic, glycidyl, amido, mercapto or halogen radical, described R2And described R3It is each independently H or 1 to 18 carbon
The alkyl of atomic number, described x is 1,2 or 3.
Low refractive composition the most according to claim 5, it is characterised in that before there is described sol gel reaction,
Described low refractive composition the most also comprises described inorganic particulate.
Low refractive composition the most according to claim 1, it is characterised in that the Weight-average molecular of described organopolysiloxane
Amount is 3000g/mol to 55000g/mol.
Low refractive composition the most according to claim 1, it is characterised in that described inorganic particulate comprises the free titanium dioxide of choosing
In the group of silicon particle, aluminium oxide particles, Zirconia particles, Titanium particles, stibium oxide particle and combinations thereof composition extremely
Few a kind of particle.
Low refractive composition the most according to claim 1, it is characterised in that do not comprise substituted or unsubstituted unimolecule alkane
TMOS compound, or also comprise substituted or unsubstituted unimolecule alkoxysilane compound containing trialkylsilyl group in molecular structure.
10. a nesa coating, it is characterised in that include by the low refractive composition according to any one of claim 1 to 9
The forming low-refractive-index layer formed.
11. nesa coatings according to claim 10, it is characterised in that
Upper side at described forming low-refractive-index layer is formed with micro concavo-convex；
Described micro concavo-convex is formed by inorganic particulate.
12. nesa coatings according to claim 10, it is characterised in that the thickness of described forming low-refractive-index layer be 10nm extremely
50nm。
13. nesa coatings according to claim 10, it is characterised in that the refractive index of described forming low-refractive-index layer be 1.40 to
1.50。
14. nesa coatings according to claim 10, it is characterised in that
High refracting layer and substrate layer it is also formed with successively in the bottom of described forming low-refractive-index layer；
It is also formed with conductive layer on the top of described forming low-refractive-index layer.
15. nesa coatings according to claim 14, it is characterised in that also include the one side or two with described substrate layer
The hard conating that face connects.
16. nesa coatings according to claim 10, it is characterised in that light transmittance is more than 85%, mist degree is 0.1%
To 0.8%.
The preparation method of 17. 1 kinds of low refractive composition, it is characterised in that including:
The mixing silane compound of formula 1 below, the silane compound of formula 2 below and average diameter be 30nm extremely
The inorganic particulate of 70nm, prepares to comprise the step of the feedstock composition of described composition；And
Make described feedstock composition generation sol gel reaction, prepare the step of low refractive composition,
Chemical formula 1:
R1 xSi(OR2)4-x
Chemical formula 2:
Si(OR3)4
In described chemical formula 1, described R1Be the alkyl of 1 to 18 carbon number, the ester group of 2 to 6 carbon numbers, 2 to 12
The epoxy radicals of carbon number, the thiazolinyl of 2 to 12 carbon numbers, the aryl of 6 to 12 carbon numbers, 3 to 18 carbon numbers
Acrylic, glycidyl, amido, mercapto or halogen radical, described R2And described R3It is each independently H or 1 to 18 carbon
The alkyl of atomic number, described x is 1,2 or 3.
The preparation method of 18. low refractive composition according to claim 17, it is characterised in that comprise the steps: phase
For the silane compound of described chemical formula 1 of 100 weight portions and the summation of the silane compound of described chemical formula 2, mix 0.5
Weight portion prepares described feedstock composition to the described inorganic particulate of 20 weight portions.
The preparation method of 19. low refractive composition according to claim 17, it is characterised in that occur described colloidal sol-
The period of gel reaction, chemical reaction is mutually occurred to form organopolysiloxane between described silane compound.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR10-2014-0040782 | 2014-04-04 | ||
| KR20140040782 | 2014-04-04 | ||
| PCT/KR2015/002883 WO2015152559A1 (en) | 2014-04-04 | 2015-03-24 | Low refractive composition, preparation method therefor, and transparent conductive film |
Publications (1)
| Publication Number | Publication Date |
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| CN106164711A true CN106164711A (en) | 2016-11-23 |
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|---|---|---|---|
| CN201580018312.8A Pending CN106164711A (en) | 2014-04-04 | 2015-03-24 | Low refractive composition and preparation method thereof and nesa coating |
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| Country | Link |
|---|---|
| JP (1) | JP2017522581A (en) |
| KR (1) | KR20150116396A (en) |
| CN (1) | CN106164711A (en) |
| TW (1) | TW201538636A (en) |
| WO (1) | WO2015152559A1 (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| FI20155713A (en) * | 2015-10-09 | 2017-04-10 | Inkron Ltd | Electrically conductive siloxane particle films and devices containing the same |
| WO2017068789A1 (en) * | 2015-10-21 | 2017-04-27 | 富士フイルム株式会社 | Antireflective film and functional glass |
| JP6681726B2 (en) * | 2016-02-01 | 2020-04-15 | 日東電工株式会社 | Transparent conductive film |
| KR102159491B1 (en) * | 2016-05-09 | 2020-09-24 | 주식회사 엘지화학 | A conductive transparent film |
| KR102267503B1 (en) * | 2017-12-22 | 2021-06-21 | 주식회사 엘지화학 | Manufacturing method of optical member comprising low-reflection silica coating layer and optical member menufactured by the same |
| JP7247220B2 (en) * | 2018-12-12 | 2023-03-28 | 大塚化学株式会社 | Substrate for forming transparent conductive layer, transparent conductive film, touch panel, and method for producing substrate for forming transparent conductive layer |
| WO2023210436A1 (en) * | 2022-04-27 | 2023-11-02 | 日東電工株式会社 | Antireflection film and method for producing same, and image display device |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101981134A (en) * | 2008-02-05 | 2011-02-23 | 原子能和替代能源委员会 | Hybrid organic-inorganic material, optical thin layer made of said material, optical material containing same, and method for making same |
| KR20120030029A (en) * | 2010-09-17 | 2012-03-27 | (주)엘지하우시스 | Transparent conductive film with excellent visibility and method of manufacturing the transparent conductive film |
| KR20140030910A (en) * | 2012-09-04 | 2014-03-12 | (주)엘지하우시스 | Anti-reflection coating composition containing siloxane compound, anti-reflection film using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2005165010A (en) * | 2003-12-03 | 2005-06-23 | Konica Minolta Opto Inc | Antireflection film, polarizing plate, and picture display device |
| JP2011088787A (en) * | 2009-10-22 | 2011-05-06 | Hitachi Maxell Ltd | Composition for antireflection film, antireflection film, method for producing antireflection film, and substrate with antireflection film |
| JP5999808B2 (en) * | 2012-03-29 | 2016-09-28 | 日本タングステン株式会社 | Manufacturing method of light reflecting film |
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2015
- 2015-03-24 JP JP2016560665A patent/JP2017522581A/en active Pending
- 2015-03-24 CN CN201580018312.8A patent/CN106164711A/en active Pending
- 2015-03-24 WO PCT/KR2015/002883 patent/WO2015152559A1/en active Application Filing
- 2015-03-30 KR KR1020150044346A patent/KR20150116396A/en unknown
- 2015-03-31 TW TW104110516A patent/TW201538636A/en unknown
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101981134A (en) * | 2008-02-05 | 2011-02-23 | 原子能和替代能源委员会 | Hybrid organic-inorganic material, optical thin layer made of said material, optical material containing same, and method for making same |
| KR20120030029A (en) * | 2010-09-17 | 2012-03-27 | (주)엘지하우시스 | Transparent conductive film with excellent visibility and method of manufacturing the transparent conductive film |
| KR20140030910A (en) * | 2012-09-04 | 2014-03-12 | (주)엘지하우시스 | Anti-reflection coating composition containing siloxane compound, anti-reflection film using the same |
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| Publication number | Publication date |
|---|---|
| WO2015152559A1 (en) | 2015-10-08 |
| KR20150116396A (en) | 2015-10-15 |
| TW201538636A (en) | 2015-10-16 |
| JP2017522581A (en) | 2017-08-10 |
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