CN103376650B - Light shield layer forms the manufacture method with photonasty substrate composition - Google Patents
Light shield layer forms the manufacture method with photonasty substrate composition Download PDFInfo
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- CN103376650B CN103376650B CN201310135839.1A CN201310135839A CN103376650B CN 103376650 B CN103376650 B CN 103376650B CN 201310135839 A CN201310135839 A CN 201310135839A CN 103376650 B CN103376650 B CN 103376650B
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Abstract
The invention provides the light shield layer formation photonasty substrate composition of the high-quality not producing pin hole etc.The feature of the manufacture method of light shield layer formation photonasty substrate composition of the present invention is, be filter weight-average molecular weight after the surfactant component (H) of the polymkeric substance of 10000 ~ 50000 is diluted to 2.5 ~ 10 quality %, this surfactant component (H) after filtration, photonasty base material component (A), pigment composition (G) and Elements in Organic Solvents (S) are disperseed.Above-mentioned filtration is preferably undertaken by the PTFE film that aperture is less than 1 μm.
Description
Technical field
The present invention relates to a kind of manufacture method of light shield layer formation photonasty substrate composition.
Background technology
Such as, for the color filter used in colour display device, the cancellate black light shield layer to be usually called as with black matrix surrounds the structure of the pixel be made up of red (R), green (G), blue (B) colors.
As one of the manufacture method of described color filter, propose using black matrix as next door, formed with ink-jetting style the method (such as, following patent documentation 1) of the dyed layer of color filter.
In addition, not only in color filter, sometimes also in various display device, the contrast realizing image by the border between each pixel being arranged black matrix improves.
Black matrix such as uses the anti-corrosion agent composition containing black pigment and is lithographically formed.As black pigment, generally use carbon black (such as, patent documentation 1).
But the impurity existed in anti-corrosion agent composition, foreign matter, become and produce the flaw (surface imperfection) of Resist patterns, the reason of pin hole.Describing a kind of manufacture method of anti-corrosion agent composition in patent documentation 2, in order to remove the minuteness particle produced in Resist Solution keeping, and comprising the operation using and there is the frit anti-corrosion agent composition of specific potential.
In addition, manufacture in the process of color filter, make the uniform film thickness after coating be important, therefore generally add the surfactant (such as, patent documentation 3) photonasty substrate composition to levelling effect.
In the manufacture method of the above-mentioned anti-corrosion agent composition containing filter progress, normally after base material component etc. is all mixed, through filter progress.
Prior art document
Patent documentation
[patent documentation 1] Japanese Unexamined Patent Publication 2004-325736 publication
[patent documentation 2] Japanese Unexamined Patent Publication 2004-212975 publication
[patent documentation 3] Japanese Unexamined Patent Publication 2010-107957 publication
Summary of the invention
When manufacturing black matrix, the impurity existed in photonasty base material, organic solvent, foreign matter etc. can make black matrix surface produce pin hole etc., cause the uneven homogenize etc. of pattern.
In order to manufacture the black matrix of the high-quality not producing pin hole etc., need to remove the impurity, foreign matter etc. in photonasty base material, organic solvent.
In view of the foregoing, the present inventor etc. find a kind of method, when manufacturing black matrix, by the laggard row filtration of surfactivity dilution agent as the polymkeric substance made an addition in anti-corrosion agent composition is manufactured anti-corrosion agent composition, the black matrix of the high-quality not producing pin hole etc. can be manufactured thus.
The present invention is a kind of manufacture method of light shield layer formation photonasty substrate composition, it is characterized in that, be filter weight-average molecular weight after the surfactant component (H) of the polymkeric substance of 10000 ~ 50000 is diluted to 2.5 ~ 10 quality %, this surfactant component (H) after filtration, photonasty base material component (A), pigment composition (G) and Elements in Organic Solvents (S) are disperseed.
According to the present invention, the manufacture method of the light shield layer formation photonasty substrate composition of the high-quality not producing pin hole etc. can be provided.
Accompanying drawing explanation
Fig. 1 is the schematic diagram representing uneven width evaluation method.
Embodiment
" light shield layer forms the manufacture method with photonasty substrate composition "
The feature of the manufacture method of light shield layer formation photonasty substrate composition of the present invention is, be filter weight-average molecular weight after the surfactant component (H) of the polymkeric substance of 10000 ~ 50000 is diluted to 2.5 ~ 10 quality %, this surfactant component (H) after filtration, photonasty base material component (A), pigment composition (G) and Elements in Organic Solvents (S) are disperseed.
For the light shield layer formation photonasty substrate composition utilizing manufacture method of the present invention to manufacture (hereinafter sometimes referred to photonasty substrate composition.), because the surfactant component (H) diluted is (hereinafter referred to as (H) composition.) through filter progress, the condensed matter therefore produced in dilution is removed, and presents the high-quality not producing pin hole etc. when forming light shield layer.
As above-mentioned (H) composition, the commercially available product of the concentration of usual use 40 ~ 50 quality %, synthesis and the material prepared, be engaged in photonasty substrate composition in the mode that the ultimate density of (H) composition in composition is 2.5 ~ 10 quality %.Now, it can be the method that (H) composition of the concentration of above-mentioned 40 ~ 50 quality % itself directly makes an addition in composition, also can beforehand dilution become (H) composition of the concentration of above-mentioned 2.5 ~ 10 quality % after prepare composition, but need to dilute this procedure.The Late Cambrian such as the present inventor: owing to diluting the surfactant of this higher concentration of 40 ~ 50 quality %, for some reason, a part for this surfactant may be condensed.And, find by removing this condensation product in advance in the lump, thus the generation of pin hole etc. can be suppressed, complete the present invention thus.
(H) composition
(H) composition contained by photonasty substrate composition in the present invention, such as, be preferably fluoro-alkyl side chain with carbon number 1 ~ 20 and (wherein, can be interrupted by ehter bond, ester bond, carbonyl, amino-formate bond.) and the polymkeric substance of lyophily group.
As fluoro-alkyl, as long as make carbon number be 1 ~ 20, be not particularly limited, can be interrupted by ehter bond (-O-), ester bond (-CO-O-), carbonyl (-CO-), amino-formate bond (-NH-CO-O-), but preferably not by the fluoro-alkyl that these groups interrupt, namely with-C
kh
lf
m(k represents the integer of 1 ~ 20, and l represents the integer of 0 ~ 40, and m represents the integer of 1 ~ 41, l+m=2k+1.) fluoro-alkyl that represents.
At this, in recent years, report that to have the carbon number that fluorine replaces be that the compound of the perfluoroalkyl of more than 7 exists the ecology influences such as carcinogenicity, also may become the object of the important new service regeulations (SNUR) as the ecology influence dependency rule of the U.S..Therefore, as fluoro-alkyl, preferably containing the perfluoroalkyl of carbon number 1 ~ 5 and the fluoro-alkyl that do not replaced by fluorine of remaining carbon atom.The carbon number of perfluoroalkyl is more preferably 3 ~ 5.
On the other hand, as lyophily group, the group be included in known nonionic system surfactant can be enumerated, the group preferably containing the alkylidene interrupted by ehter bond, ester bond or carbonyl.Wherein, the material preferably containing polyalkylene oxide base (polyethylene oxide base, polypropyleneoxide base, polybutylene oxide base etc.).
The mol ratio of fluoro-alkyl and lyophily group, also different and different according to the composition of photonasty substrate composition, but preferably 4: 6 ~ 9: 1, be more preferably 4: 6 ~ 8: 2, more preferably 5: 5 ~ 7: 3.
Such surfactant, can be polymerized with the monomer with above-mentioned lyophily group by the monomer that makes at least to have above-mentioned fluoro-alkyl and to obtain.As having the monomer of fluoro-alkyl and there is the monomer of lyophily group, preferred following formula (h1), monomer represented by (h2) respectively.
In above-mentioned formula (h1), R
1hrepresent hydrogen atom or methyl, R
2hrepresent the alkylidene of the straight-chain of carbon number 1 ~ 15, preferably carbon number 1 ~ 10, branched or ring-type, R
frepresent the perfluoroalkyl of carbon number 1 ~ 5, preferably carbon number 3 ~ 5.
In above-mentioned formula (h2), R
3hrepresent hydrogen atom or methyl, R
4hrepresent the alkylidene of carbon number 2 ~ 4, R
5hrepresent the alkyl of hydrogen atom or carbon number 1 ~ 15, preferably carbon number 1 ~ 10.
In addition, in above-mentioned formula (h2), p represents the integer of 1 ~ 50.
As the concrete example of the monomer represented by above-mentioned formula (h1), (methyl) acrylic acid 2 can be enumerated, 2,2-trifluoro ethyl ester, (methyl) acrylic acid 2,2,3,3,3-five fluorine propyl ester, (methyl) acrylic acid 2-(perfluoro butyl) ethyl ester, (methyl) acrylic acid 2-(perfluor-3-methyl butyl) ethyl ester etc.
In addition, as the concrete example of the monomer represented by above-mentioned formula (h2), (methyl) methoxyethyl macrogol ester can be enumerated [such as, the quantity (r) of ethylene glycol repeat units is the material of 1 ~ 50], (methyl) methoxyethyl polypropylene glycol ester [such as, the quantity (r) of propylene glycol repetitive is the material of 1 ~ 50], diol ester [such as (methyl) methoxyethyl poly-(ethylidene-propylidene), the summation (r) of the quantity of ethylene glycol repeat units and the quantity of propylene glycol repetitive is the material of 2 ~ 50], diol ester [such as (methyl) methoxyethyl poly-(ethylidene-tetramethylene), the summation (r) of the quantity of ethylene glycol repeat units and the quantity of tetramethylene glycol repetitive is the material of 2 ~ 50], diol ester [such as (methyl) acrylate, butoxy poly-(ethylidene-propylidene), the summation (r) of the quantity of ethylene glycol repeat units and the quantity of propylene glycol repetitive is the material of 2 ~ 50], diol ester [such as (methyl) acrylic acid octyloxy poly-(ethylidene-propylidene), the summation (r) of the quantity of ethylene glycol repeat units and the quantity of propylene glycol repetitive is the material of 2 ~ 50], (methyl) lauryl oxygen base macrogol ester [such as, the quantity (r) of ethylene glycol repeat units is the material of 2 ~ 50], diol ester [such as (methyl) lauryl oxygen base poly-(ethylidene-propylidene), the summation (r) of the quantity of ethylene glycol repeat units and the quantity of propylene glycol repetitive is the material of 2 ~ 50], polyglycol (methyl) acrylate, polypropylene glycol (methyl) acrylate, polyethylene glycol-propylene glycol (methyl) acrylate, polyethylene glycol-butylene glycol (methyl) acrylate, polystyrene-based ethyl (methyl) acrylate, or the LIGHTESTERHOA-MS of chemical company of common prosperity society, LIGHTESTERHOMS etc.
Make the mol ratio when monomer represented by above-mentioned formula (h1) and the monomer polymerization represented by above-mentioned formula (h2), be preferably 4: 6 ~ 9: 1, be more preferably 4: 6 ~ 8: 2, more preferably 5: 5 ~ 7: 3.
(H) composition, in the scope not damaging effect of the present invention, can also on the basis of the monomer represented by the monomer represented by above-mentioned formula (h1) and above-mentioned formula (h2), polymerization (methyl) alkyl acrylate.As the concrete example of (methyl) alkyl acrylate, (methyl) acrylate methyl esters can be enumerated, (methyl) ethyl acrylate, (methyl) n-propyl, (methyl) isopropyl acrylate, (methyl) n-butyl acrylate, (methyl) isobutyl acrylate, (methyl) n-octyl, (methyl) 2-EHA, (methyl) acrylic acid ester in the different ninth of the ten Heavenly Stems, (methyl) lauryl acrylate, (methyl) acrylic acid hexadecane ester, (methyl) stearyl acrylate ester, (methyl) cyclohexyl acrylate, (methyl) benzyl acrylate, (methyl) isobornyl acrylate etc.
This surfactant can be any one in atactic polymers and graft polymer, but is preferably graft polymer.By being set as graft polymer, the intermiscibility with (A) alkali-soluble base material can being kept, and levelling effect can be improved further.In addition, when graft polymer, even if increase content, also can not worry and occur gonorrhoea.
The sp value of surfactant is preferably 8.0 ~ 9.5 (cal/cm
3)
1/2.By making sp value be above-mentioned scope, can improve with the intermiscibility of base material component and solvent and the effect improved as surfactant.In addition, sp value can measure according to the method recorded in such as Japanese Unexamined Patent Publication 2005-290128 publication.
In addition, the weight-average molecular weight of base material contained in surfactant is 10000 ~ 50000, is preferably 10000 ~ 30000.The levelling effect of the surfactant be usually made up of the compound that the carbon number in fluoro-alkyl is few is low, but be above-mentioned scope by making weight-average molecular weight, even if thus when the carbon number of fluoro-alkyl be such as less than 5 carbon number less, also can obtain sufficient levelling effect.In addition, by making weight-average molecular weight be above-mentioned scope, the photonasty substrate layer that coating homogeneity, flatness are excellent can be obtained.
That is, usually in surfactant, by having, surface-active effect is played to the insoluble position of solvent and solubility position.But, in low-molecular-weight surfactant, when employing the few fluoro-alkyl of carbon number as insoluble position, because the effect as insoluble position is too small, therefore can not get sufficient surface-active effect.In addition, when increasing the ratio at insoluble position, solubility position can be reduced, and therefore can not obtain sufficient dissolubility.On the other hand, when employing the few fluoro-alkyl of carbon number, be more than 10000 by making the weight-average molecular weight of surfactant, the amount at the insoluble position (fluoro-alkyl) in 1 molecular surface active agent can be increased, therefore can reduce the dissolubility to solvent, can surface-active effect be guaranteed.In addition, the ratio at solubility position also gets a promotion, sterically hindered therefore by based on this solubility position, can prevent the intensive of fluoro-alkyl.In addition, due to the dissolubility to solvent can be guaranteed, even if the addition therefore increasing surfactant is also difficult to produce gonorrhoea.
In addition, when spin coating photonasty substrate composition, photonasty substrate composition is dripped in substrate, make substrate rotate and be coated with.When employing low-molecular-weight surfactant in the past, streak (striation) can be eliminated, but the liquid holdup of photonasty substrate composition can be there is in the end of substrate, therefore the final bossing that can form photonasty substrate composition in end.That is, coating homogeneity, flatness is caused to be deteriorated.On the other hand, in photonasty substrate composition in the present invention, owing to using weight-average molecular weight to be the surfactant of more than 10000, even if the projection of end therefore also can be eliminated in spin coating.Solid component concentration particularly in photonasty substrate composition is more than 30 quality %, the elimination for end bosses has larger effect.
And then, when utilizing slot coated to be coated with, usually there is the tendency of the solid component concentration reducing photonasty substrate composition.When reducing the solid component concentration of photonasty substrate composition, the mobility of photonasty substrate composition can become large, and the thickness therefore through the photonasty substrate composition of coating easily becomes uneven.In addition, although have the operation of the photonasty substrate composition drying through coating, but once the impact of the surface tension being subject to producing at coated photonasty substrate composition, temperature, dry concentration change etc., cause when drying process and return liquid from the end of substrate to central portion, the homogeneity of thickness is more easily deteriorated.Particularly when employing large substrate, very large on the impact of the homogeneity of thickness.To this, use in photonasty substrate composition of the present invention weight-average molecular weight be more than 10000 surfactant, therefore, it is possible to improve film thickness uniformity.
In the present invention, (H) composition as polymkeric substance adjusts with the concentration of 40 ~ 50 quality % in a solvent usually.As this solvent, such as, can enumerate with Elements in Organic Solvents described later (S) (hereinafter referred to as (S) composition.) identical solvent, preferably identical with the solvent used as (S) composition solvent.
In the manufacture method of light shield layer formation photonasty substrate composition of the present invention, utilize solvent by (H) component diluent to 2.5 ~ 20 quality %, the solution after utilizing frit to dilute.As this solvent, such as preferably identical with the solvent containing stoste solvent or the solvent identical with (S) composition.
The filter used in above-mentioned filter progress is not particularly limited, and can use known filter.Preferred use PTFE film (poly tetrafluoroethylene), PP film (polypropylene screen), PE film (polyethylene film), particularly preferably use PTFE film (poly tetrafluoroethylene).
As above-mentioned filter, in order to remove the condensation product produced in solution after dilution, preferably making aperture be 0.01 ~ 0.9 μm, being more preferably 0.02 ~ 0.6 μm, being particularly preferably 0.05 ~ 0.3 μm.
In above-mentioned filter progress, filtration unit, filter method are not particularly limited, and can use known filtration unit, filter method.
This surfactant component (H) after filtration, photonasty base material component (A), pigment composition (G) and Elements in Organic Solvents (S) are disperseed, manufactures light shield layer formation and use photonasty substrate composition.
(A) composition
(A) composition used in the manufacture method of light shield layer formation photonasty substrate composition of the present invention is not particularly limited, and can use known composition.Such as, can enumerate containing alkali-soluble base material (A1) (hereinafter referred to as (A1) composition.), photopolymerizable compound (A2) is (hereinafter referred to as (A2) composition.) and Photoepolymerizationinitiater initiater (A3) (hereinafter referred to as (A3) composition.) and the composition be cured by light such as irradiation ultraviolet radiations.By making the partially cured of illuminated light, the pattern of required form can be obtained.
(A1) composition
In the present invention, (A1) composition can apply following alkali-soluble base material (A1-1) (hereinafter referred to as (A1-1) composition.) or the following alkali-soluble base material (A1-2) with photo-curable (hereinafter referred to as (A1-2) composition.)。
(A1-1) composition
As (A1-1) composition, can enumerate: be selected from acrylic acid, methacrylic acids etc. have more than a kind in the monomer of carboxyl and are selected from methyl acrylate, methyl methacrylate, ethyl acrylate, β-dimethyl-aminoethylmethacrylate, acrylic acid 2-hydroxy methacrylate, 2-hydroxyethyl methacrylate, methacrylic acid 2-hydroxy propyl ester, n-butyl acrylate, n-BMA, isobutyl acrylate, isobutyl methacrylate, benzyl acrylate, benzyl methacrylate, acrylic acid benzene oxygen ester, methacrylic acid benzene oxygen ester, isobornyl acrylate, isobornyl methacrylate, glycidyl methacrylate, styrene, acrylamide, more than a kind in vinyl cyanide etc. the multipolymer formed,
The base materials such as phenol novolak-type epoxy acrylate polymer, phenol novolak-type epoxy methacrylate polymers, cresol novolak type epoxy acrylate polymer, cresol novolak type epoxy methacrylate polymers, bisphenol-a epoxy acrylate polymkeric substance, bisphenol S type epoxy acrylate polymer.
These base materials are owing to having imported acryloyl group or methacryl, and therefore cross-linking efficiency is improved, and photostability, the drug resistance of film are excellent.
Form in the monomer component of above-mentioned (A1-1) composition, the content that acrylic acid, methacrylic acid etc. have a monomer component of carboxyl is preferably the scope of 5 ~ 40 quality %.
(A1-2) composition
As (A1-2) composition, the polymkeric substance shown in following general formula (1) can be enumerated.Compound shown in this general formula (1) is owing to itself having optical polymerism (photo-curable), therefore the photomask formation of this compound is being contained with in photonasty base material, by improving transmission of ultraviolet rays, light sensitivity can be improved further.
(in formula, X is the group shown in following chemical formula (2), and Y is the residue removing acid anhydride (-CO-O-CO-) and obtain from dicarboxylic anhydride, and Z is the residue removing 2 acid anhydrides and obtain from tetracarboxylic dianhydride.)
As the concrete example of the dicarboxylic anhydride derived from above-mentioned Y (dicarboxylic anhydride before removing acid anhydride), such as, can enumerate maleic anhydride, succinic anhydride, itaconic anhydride, phthalic anhydride, tetrabydrophthalic anhydride, hexahydrophthalic anhydride, methylendomethylene tetrabydrophthalic anhydride, chlorendic anhydride, methyl tetrahydrophthalic anhydride, glutaric anhydride etc.
In addition, as the concrete example of the tetracarboxylic dianhydride derived from above-mentioned Z (removing the tetracarboxylic dianhydride before 2 acid anhydrides), such as, can enumerate the tetracarboxylic dianhydrides etc. such as pyromellitic dianhydride, benzophenone tetracarboxylic dianhydride, biphenyl tetracarboxylic dianhydride, xenyl ether tetracarboxylic dianhydride.
(A1) composition can be used alone a kind, also can be mixed with two or more.In addition, only can use above-mentioned (A1-1) composition, also only can use (A1-2) composition, can also both and use.
The weight-average molecular weight (Mw) (utilizing the polystyrene conversion benchmark of gel permeation chromatography) of (A1) composition in the present invention is not particularly limited, but be preferably 1000 ~ 1000000, be more preferably 3000 ~ 50000, most preferably be 5000 ~ 15000.When less than the upper limit of this scope, have the dissolubility to resist solvent being enough to be used as resist, when larger than the lower limit of this scope, Resist patterns cross sectional shape is good.
(A2) composition
As (A2) composition in the present invention, methyl acrylate can be enumerated, methyl methacrylate, acrylic acid 2-hydroxy methacrylate, 2-hydroxyethyl methacrylate, methacrylic acid 2-hydroxy propyl ester, glycol diacrylate, ethylene glycol dimethacrylate, triethylene glycol diacrylate, TEGDMA, tetraethylene glycol diacrylate, TEG dimethylacrylate, propylene glycol diacrylate, dimethacrylate, trimethylolpropane triacrylate, trimethylol-propane trimethacrylate, tetra methylol tetraacrylate, tetra methylol propane tetramethyl acrylate, pentaerythritol triacrylate, pentaerythritol acrylate trimethyl, tetramethylol methane tetraacrylate, pentaerythritol tetramethylacrylate, Dipentaerythritol Pentaacrylate, dipentaerythritol pentamethacrylates, dipentaerythritol tetraacrylate, dipentaerythritol acrylate, dipentaerythritol hexamethacrylate, 1,6-hexanediyl ester, benzyl acrylate, benzyl methacrylate, phenolphthalein base (Cardo) epoxy diacrylate, acrylic acid, methacrylic acid etc., but be not limited to these materials.
(A2) composition can be used alone or two or more kinds may be used.
In addition, in the present invention, the polymkeric substance with the alkali-soluble of optical polymerism is included in above-mentioned (A1) composition, and the monomer with optical polymerism is included in (A2) composition.
When using above-mentioned (A1-1) composition, (A2) composition, relative to this (A1-1) composition 100 mass parts, is preferably the scope of 5 ~ 500 mass parts.Preferred scope is 20 ~ 300 mass parts.
By making the use level of (A2) composition be more than the lower limit of above-mentioned scope, thus the solidification be difficult to when producing exposure is bad, can obtain sufficient thermotolerance, drug resistance.In addition, obtaining good tunicle Forming ability, prevent the film after developing residual in, below the higher limit being preferably set to above-mentioned scope.
(A3) composition
As (A3) composition in the present invention, be not particularly limited, the material proposed as photosensitive composite Photoepolymerizationinitiater initiater up to now can be used.Such as, 1-hydroxycyclohexylphenylketone can be enumerated, 2-hydroxy-2-methyl-1-phenyl-propane-1-ketone, 1-(4-(2-hydroxyl-oxethyl) phenyl)-2-hydroxy-2-methyl-1-propane-1-ketone, 1-(4-isopropyl phenyl)-2-hydroxy-2-methyl propane-1-ketone, 1-(4-dodecylphenyl)-2-hydroxy-2-methyl propane-1-ketone, 2,2-dimethoxy-1,2-diphenylethane-1-ketone, two (4-dimethylaminophenyl) ketone, 2-methyl isophthalic acid-(4-(methyl mercapto) phenyl)-2-morpholino propane-1-ketone, 2-benzyl-2-dimethylamino-1-(4-morphlinophenyl)-butane-1-ketone, TMDPO, 4-benzoyl-4 '-methyl dimethoxy base thioether, 4-dimethylaminobenzoic acid, 4-dimethylaminobenzoic acid methyl esters, EDMAB, 4-dimethylaminobenzoic acid butyl ester, 4-dimethylamino-2-ethylhexyl Benzoic acid, 4-dimethylamino-2-isoamyl benzene formic acid, benzyl-'beta '-methoxy ethyl acetal, benzil dimethyl ketal, 1-phenyl-1,2-propanedione-2-(adjacent ethoxy carbonyl) oxime, o-benzoyl yl benzoic acid methyl esters, 2,4-diethyl thioxanthone, CTX, 2,4-dimethyl thioxanthone, the chloro-4-propoxythioxanthone of 1-, thioxanthene, 2-diuril ton, 2,4-diethyl thioxanthene, 2-methyl thioxanthene, 2-isopropylthioxanthones, 2-EAQ, prestox anthraquinone, 1,2-benzo anthraquinone, 2,3-diphenyl anthraquinone, azoisobutyronitrile, benzoyl peroxide, cumene peroxide, 2-mercaptobenzimidazole, 2-mercaptobenzoxazole, 2-mercaptobenzothiazole, 2-(Chloro-O-Phenyl)-4,5-bis-(m-methoxyphenyl)-imidazole radicals dipolymer, benzophenone, 2-chlorobenzophenone, p, p '-bis-(dimethylamino) benzophenone, 4,4 '-bis-(diethylamino) benzophenone, 4,4 '-dichloro benzophenone, 3,3-dimethyl-4-methoxy benzophenone, benzil, benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin n-butyl ether, benzoin isobutyl ether, benzoin butyl ether, acetophenone, 2,2-diethoxy acetophenone, to dimethyl acetophenone, to dimethylamino propiophenone, dichloroacetophenone, trichloroacetophenone, p-tert.-butyl acetophenone, to dimethylamino benzoylformaldoxime, to tert-butyl group trichloroacetophenone, to tert-butyl group dichloroacetophenone, α, α,α-dichloro-4-phenoxy acetophenone, thioxanthones, 2-methyl thioxanthones, ITX, Dibenzosuberone, amyl group-4-dimethylaminobenzoic acid ester, 9-phenylacridine, 1,7-pair-(9-acridinyl) heptane, 1,5-pair-(9-acridinyl) pentane, 1,3-pair-(9-acridinyl) propane, to methoxyl triazine, 2,4,6-tri-(trichloromethyl) s-triazine, two (trichloromethyl) s-triazine of 2-methyl-4,6-, two (trichloromethyl) s-triazine of 2-[2-(5-methylfuran-2-base) vinyl]-4,6-, two (trichloromethyl) s-triazine of 2-[2-(furans-2-base) vinyl]-4,6-, two (trichloromethyl) s-triazine of 2-[2-(4-diethylamino-2-aminomethyl phenyl) vinyl]-4,6-, two (trichloromethyl) s-triazine of 2-[2-(3,4-Dimethoxyphenyl) vinyl]-4,6-, two (trichloromethyl) s-triazine of 2-(4-methoxyphenyl)-4,6-, two (trichloromethyl) s-triazine of 2-(4-ethoxystyrene base)-4,6-, two (trichloromethyl) s-triazine of 2-(4-n-butoxyphenyl)-4,6-, 2,4-pair-trichloromethyl-6-(the bromo-4-methoxyl of 3-) phenyl s-triazine, 2,4-pair-trichloromethyl-6-(the bromo-4-methoxyl of 2-) phenyl s-triazine, 2,4-pair-trichloromethyl-6-(the bromo-4-methoxyl of 3-) styryl phenyl s-triazine, 2,4-pair-trichloromethyl-6-(the bromo-4-methoxyl of 2-) styryl phenyl s-triazine etc.
Among these, can preferably use triazines such as methoxyl triazines, 2, 4, 6-tri-(trichloromethyl) s-triazine, 2-methyl-4, two (trichloromethyl) s-triazine of 6-, 2-[2-(5-methylfuran-2-base) vinyl]-4, two (trichloromethyl) s-triazine of 6-, 2-[2-(furans-2-base) vinyl]-4, two (trichloromethyl) s-triazine of 6-, 2-[2-(4-diethylamino-2-aminomethyl phenyl) vinyl]-4, two (trichloromethyl) s-triazine of 6-, 2-[2-(3, 4-Dimethoxyphenyl) vinyl]-4, two (trichloromethyl) s-triazine of 6-, 2-(4-methoxyphenyl)-4, two (trichloromethyl) s-triazine of 6-, 2-(4-ethoxystyrene base)-4, two (trichloromethyl) s-triazine of 6-, 2-(4-n-butoxyphenyl)-4, two (trichloromethyl) s-triazine of 6-etc. have the triaizine compounds such as the triazines of halogenated methyl, the imidazole-based compounds such as 2-(Chloro-O-Phenyl)-4,5-bis-(m-methoxyphenyl)-imidazole radicals dipolymer, and the aminoketone compounds such as 2-benzyl-2-dimethylamino-1-(4-morphlinophenyl)-butane-1-ketone.
In the present invention, as (A3) composition, can be used together Multiple components.
In the manufacture method of light shield layer formation photonasty substrate composition of the present invention, the use level of above-mentioned (A3) composition is preferably the scope of 0.1 ~ 30 mass parts relative to (A1) composition 100 mass parts.
(S) composition
In the manufacture method of light shield layer formation photonasty substrate composition of the present invention, in order to improve coating, adjustment viscosity, and make (A) component dissolves in (S) composition.
As (S) composition, benzene can be enumerated, toluene, dimethylbenzene, MEK, acetone, methyl isobutyl ketone, cyclohexanone, methyl alcohol, ethanol, propyl alcohol, butanols, hexanol, cyclohexanol, ethylene glycol, diethylene glycol, glycerine, ethylene glycol monomethyl ether, ethylene glycol monomethyl ether, propylene glycol monomethyl ether, propylene glycol monoethyl, diethylene glycol monomethyl ether, TC, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, acetic acid 3-methoxybutyl, acetic acid 3-methyl-3-methoxybutyl, propylene glycol monomethyl ether (PGMEA), propylene glycol monomethyl ether propionic ester, propylene glycol monoethyl propionic ester, methyl carbonate, ethyl carbonate, propyl carbonate, butyl carbonate etc.Wherein, acetic acid 3-methoxybutyl not only shows excellent dissolubility for the soluble ingredient in light shield layer formation photonasty substrate composition, and makes the dispersiveness of the insoluble compositions such as pigment become good, is therefore preferred.
(S) use amount of composition is not particularly limited to, and suitably can set with the concentration that can be applied to substrate etc. according to coating film thickness.The viscosity of the light shield layer formation photonasty substrate composition in the present invention is 5 ~ 100cp, is preferably 10 ~ 50cp, is more preferably 20 ~ 30cp.In addition, solid component concentration is 5 ~ 100 quality %, is preferably the scope of 20 ~ 50 quality %.
Manufacture method of the present invention preferably has following operation: make (A) component dissolves in (S) composition, the filter being less than 1 μm by the substrate solution aperture of gained filters.
When manufacture method of the present invention has the filter progress of substrate solution, as concrete embodiment, such as can enumerate following operation: in advance (A) composition is dissolved in (S) composition, (H) composition filtered out after dilution being added in this substrate solution separately, filtering the substrate solution containing being somebody's turn to do (H) composition.
The filter used in the filter progress of above-mentioned substrate solution is not particularly limited, and can use known filter.Preferred use PTFE film (poly tetrafluoroethylene), PP film (polypropylene screen), PE film (polyethylene film), particularly preferably use PTFE film (poly tetrafluoroethylene).
As above-mentioned filter, owing to also needing to remove fine impurity, foreign matter, therefore preferably make aperture be 0.01 ~ 0.9 μm, be more preferably 0.05 ~ 0.6 μm, be particularly preferably 0.1 ~ 0.3 μm.
In the present invention, preferably: make (H) composition after filtration and (A) component dissolves in (S) composition and after filtering the substrate solution of gained as described above, then disperse with (G) composition.The method of dispersion (G) composition is not particularly limited, can by adding (G) composition and carry out the method such as stir to carry out in substrate solution.
(G) composition
In the present invention, as (G) composition, the black pigments such as carbon black can be used.In addition, can also use and adjust the material of tone etc. with black, red, blue, green, yellow, purple pigment.Pigment can suitably use known pigment.
Particularly, when as pigment and with carbon black and other pigments, if 15 quality % in the not enough all pigment of carbon black, then can improve shading rate when not reducing the light sensitivity of above-mentioned light shield layer formation photonasty substrate composition.
In the present invention, as (G) composition, You selects Shi perylene system black pigment, and (under Yi, Jian Cheng is perylene pigment.)。As concrete example, perylene pigment represented by perylene pigment represented by following general formula (I) and following general formula (II) can be enumerated.In addition, the product that can preferably use BASF AG to manufacture is called the commercially available product etc. of K0084, K0086.
(in formula, R
1, R
2separately represent the alkylidene of carbon number 1 ~ 3, R
3, R
4separately represent hydrogen atom, hydroxyl, methoxyl or acetyl group.)
(in formula, R
5, R
6separately represent the alkylidene of carbon number 1 ~ 7.)
Compound represented by above-mentioned general formula (I) and the compound represented by general formula (II) can use the method recorded in such as Japanese Laid-Open Patent Publication 62-1753 publication, Japanese Patent Publication 63-26784 publication to synthesize.That is, with perylene-3,5,9,10-tetrabasic carboxylic acid or its dianhydride and amine, as raw material, carry out adding thermal response in water or organic solvent.Then, by being precipitated again in sulfuric acid by the crude product of gained or carry out recrystallization in water, organic solvent or their mixed solvent, object can be obtained thus.
， perylene pigment can be used alone or two or more kinds may be used in the present invention.
In addition, in order to make light shield layer formation photonasty substrate composition Zhong perylene pigment be in disperse state, the mean grain size of You Xuan Shi perylene pigment is 10 ~ 1000nm.
The content of light shield layer formation photonasty substrate composition Zhong perylene pigment of the present invention is preferably 5 ~ 250 mass parts relative to (A1) composition 100 mass parts.More preferably scope is 10 ~ 200 mass parts.The content of Tong Guo Shi perylene pigment is more than the lower limit of above-mentioned scope, can obtain good light-proofness.In addition, prevent ill-exposed, solidify bad in, the content of You Xuan Shi perylene pigment is below the higher limit of above-mentioned scope.
When Hun closes Shi perylene pigment and above-mentioned pigment, pigment, the preferred ratio shared by the summation of Zhao perylene pigment at the overall, of pigment and perylene pigment and other pigments of other pigment, the use amount of pigment is that the mode of more than 85 quality % sets.Being more preferably more than 90 quality %, also can be 100 quality %.
By more than above-mentioned lower limit, thus light sensitivity when can obtain the thick film using the formation of above-mentioned light shield layer formation photonasty substrate composition more than 2 μm, and the good shading rate of photomask can be reached.
In addition, in the manufacture method of light shield layer formation photonasty substrate composition of the present invention, the operation of again filtering after disperseing preferably through making (G) composition.Now, in order to prevent (G) composition after disperseing to be removed, the filter that preferably use aperture is large, such as aperture are the filter of 0.6 ~ 1.5 μm.As long as the filter that the filter again used in filter progress does not remove pigment is just not particularly limited, known filter can be used.Preferably can use PTFE film (poly tetrafluoroethylene), PP film (polypropylene screen), PE film (polyethylene film).
In addition, in light shield layer formation with in photonasty substrate composition, hot polymerization inhibitor, defoamer can be added.
As above-mentioned hot polymerization inhibitor, can be known material, can quinhydrones, Hydroquinone monoethylether etc. be enumerated.
As above-mentioned defoamer, can be known defoamer, silicone-based, fluorine based compound can be enumerated.
The formation method > of < light shield layer
Below, as the embodiment using light shield layer formation photonasty substrate composition to form the method for light shield layer, the example of the method forming black matrix is described.
First, use roll coater, reverse the non-contact type apparatus for coating such as contact transfer printing type apparatus for coating or spin coater (rotary apparatus for coating), curtain curtain coater (curtainflowcoater) etc. such as coating machine (reversecoater), bar coater, substrate is coated with light shield layer formation photonasty substrate composition.Substrate can use the substrate with transmitance, and such as thickness is the glass substrate of 0.5 ~ 1.1mm.
In order to improve the adaptation of glass substrate and light shield layer formation photonasty substrate composition, can silane-coating coupling agent on the glass substrate in advance.Or add silane coupling agent when the preparation of light shield layer formation with photonasty substrate composition.
After above-mentioned coating, make it dry and remove desolventizing.Drying means is not particularly limited, such as, can be any one following method: (1) utilize heating plate at the 80 DEG C ~ temperature of 120 DEG C, preferably 90 DEG C ~ 100 DEG C method of dry 60 seconds ~ 120 seconds; (2) method of several hours ~ several days is at room temperature placed; (3) storage heater, infrared heater dozens of minutes ~ several hours and except the method for desolventizing is put into.
Then, across minus mask, irradiation ultraviolet radiation, excimer laser isoreactivity energy-ray, carry out Partial exposure.The energy-ray amount of irradiating is different by the difference of the composition of photonasty substrate composition according to light shield layer formation, such as preferred 30 ~ 2000mJ/cm
2left and right.
Use developer solution to develop to the film after exposure, form black matrix pattern thus.Developing method is not particularly limited, such as, can use infusion process, spray-on process etc.As the concrete example of developer solution, the developer solution of the organic systems such as monoethanolamine, diethanolamine, triethanolamine can be enumerated, the aqueous solution of NaOH, potassium hydroxide, sodium carbonate, ammoniacal liquor, quaternary ammonium salt etc.
According to the light shield layer formation photonasty substrate composition utilizing manufacture method of the present invention to obtain, even if thickness is more than 2 μm, photoetching process also can be utilized to form good pattern.Therefore, the light shield layer of the thick films such as the black matrix of thick film can be formed.
This be considered to due to Tong cross Shi perylene pigment as light-proofness pigment thus can realize substrate composition transmission exposure light and cover the such characteristic of visible ray.
< distance piece >
In addition, in order to make the interval between two substrates keep certain having liquid crystal and be accommodated in the liquid crystal display of the structure between two substrates, use that light shield layer formation photosensitive polymer combination of the present invention is formed, that thickness is certain light shield layer, the distance piece that the state between these two substrates that is held on is arranged can be doubled as.The thickness of the light shield layer with such distance piece function is not particularly limited, preferably more than 2 μm.
In liquid crystal display in the past, by the spacer arrangement that formed by spherical spacer particle or photonasty substrate composition between 2 plate bases.When employing spherical spacer particle, when applying vibration, impact, distance piece moves in liquid crystal, and the alignment films be located on substrate inner face may be impaired, if but utilize the present invention, this kind of problem can be solved.In addition, when employing the distance piece formed by photonasty substrate composition as described above, need to form black matrix separately, if but utilize the present invention, do not need to form black matrix separately, the manufacturing process of liquid crystal display can be reduced.
And then, because distance piece has light-proofness, therefore, it is possible to prevent spacer portion from causing " whiting " owing to being often in Transmission light state.
< color filter >
According to the present invention, black matrix can be formed with thick film.Therefore, especially passing through in the peristome of preformed black matrix, to form dyed layer with ink-jetting style thus formed in the formation of the black matrix in the method for color filter, preferred light shield layer formation photonasty substrate composition of the present invention.Black matrix in the method plays the effect of so-called next door (cofferdam (bank)).
In the present invention, the thickness of the black matrix used as the next door (cofferdam) in ink-jetting style is not particularly limited, preferably greater than 2 μm.
Use the light shield layer formation photonasty substrate composition formation manufactured in manufacture method of the present invention as the method for the black matrix in next door (cofferdam), can carry out in the same manner as the formation method of above-mentioned light shield layer.
And; after forming the black matrix as next door (cofferdam); repeatedly carry out in the peristome of this black matrix, being coated with the operation of painted black liquid with ink-jetting style and making the operation of this painted ink liquid-solidization; form dyed layer; and then form transparent protective film as required, can color filter be manufactured thus.The method utilizing ink-jetting style to form dyed layer can use known method.
According to the present invention, can form the black matrix used as next door (partition) in ink-jetting style using thick film, the painted black liquid that therefore can prevent the peristome for black matrix from giving exceedes next door spilling and between pixel, produces the situation of colour mixture.
In addition, compared with the situation of thin with black matrix (next door is low), low viscous painted black liquid can be used.
In addition, photoetching process also can be utilized as in the past to form color filter.
Embodiment
Below, further illustrate the present invention by embodiment, but the present invention is not defined as following embodiment.
< embodiment 1 ~ 3, reference example 1 ~ 6 and comparative example 1 ~ 10>
[synthesis of (A) alkali soluble resin]
First, bisphenol fluorene type epoxy resin (epoxide equivalent 235) 235g, tetramethyl ammonium chloride 110mg, 2 is dropped in 500ml four-hole boiling flask, 6-di-tert-butyl-4-methy phenol 100mg and acrylic acid 72.0g, be blown into air with the speed of 25ml/ minute wherein on one side, carry out heating for dissolving at 90 ~ 100 DEG C.Then, slowly heat up under the state that solution is gonorrhoea, be heated to 120 DEG C and make it dissolve completely.At this moment, solution becomes clear viscous gradually, but still continues to stir.Measure acid number during this, continue to add thermal agitation until be less than 1.0mgKOH/g.Until acid number reaches desired value need 12 hours.Then be cooled to room temperature, obtain water white transparency and solid shape, bisphenol fluorene type acrylic acid epoxy ester represented by following formula (a4).
Next, acetic acid 3-methoxybutyl 600g is added in the above-mentioned bisphenol fluorene type acrylic acid epoxy ester 307.0g of gained thus, after dissolving, mixing benzophenone tetracarboxylic dianhydride 80.5g and tetraethylammonium bromide 1g, slow intensification, makes it react 4 hours at 110 ~ 115 DEG C.After confirming the disappearance of anhydride group, mixing 1,2,3,6-tetrabydrophthalic anhydride 38.0g, makes it react 6 hours at 90 DEG C, obtains resin (A-1).The disappearance of anhydride group utilizes IR spectrum to confirm.Weight-average molecular weight is 3400.
[light shield layer forms the preparation with photonasty substrate composition]
Shown in table 1 described as follows, (S) solvent is added in (A) alkali soluble resin, (E) photopolymerization monomer, (H) surfactant and (D) colorant, solid component concentration is adjusted to 15 quality % or 17 quality %, carry out mixing in 2 hours with stirring machine, prepare light shield layer formation photonasty substrate composition.In addition, the use level of each composition in table 1 is " mass parts ".
[table 1]
The details of (A) alkali soluble resin used in table 1, (E) photopolymerization monomer, (B) emulsion, (D) colorant and (S) organic solvent is as follows.
(A)-1: in resin (A-1), add acetic acid 3-methoxybutyl and be adjusted to solid component concentration be 50 quality % prepare liquid
(E)-1: dipentaerythritol acrylate
(B)-1:IRGACUREOXE02 (Ciba Specialty Chemicals's system)
(B)-2:IRGACURE369 (Ciba Specialty Chemicals's system)
(D)-1: carbon black (Yu Guo pigment Inc., concentration of carbon: 55%, solvent: acetic acid 3-methoxybutyl)
(S)-1: acetic acid 3-methoxybutyl/cyclohexanone/propylene glycol monomethyl ether=60/20/20 (mass ratio)
In addition, shown in the details table 2 described as follows of (H) surfactant used in table 1.In table 2, the ratio of the inventory of each monomer when monomer total amount during synthetic copolymer is set to 100 mass parts by the numeral in the parantheses in the multipolymer of (H)-1 ~ (H)-7.
[table 2]
[uneven width evaluation]
Use spin coater (MIKASA Inc.), the light shield layer formation photonasty substrate composition of the reference example 1 ~ 6 of above-mentioned gained, comparative example 1 ~ 4 is coated on the glass substrate (1737 glass) of 100mm × 100mm respectively, then, be positioned on the wide glass sheet of the 5mm that arranges on hot plate, 90 DEG C carry out 120 second prebake.Use surface roughness measurement machine SurfcorderSE-2300 (research of (strain) little slope is made) mensuration uneven width now.It the results are shown in table 1.
In addition, so-called uneven width, refers to that mensuration position is as shown in Figure 1 as uneven width (nm).Owing to becoming the heat transfer of glass substrate only from glass sheet heat transfer, therefore cause convection current from by the position of heating, light-blocking resin composition is upspring, this thing of upspringing is pearl.This upspring thing less, namely thickness to become very thin part fewer, then its coating homogeneity, flatness are better.
As shown in Table 1, employ in the reference example 1 ~ 6 of the specific surfactant of molecular weight more than 10000, can obtain that uneven width is little, coating homogeneity and the excellent light shield layer formation photonasty substrate composition of flatness.On the other hand, employ molecular weight and be less than in the comparative example 1 ~ 4 of other surfactants of 10000, uneven width is large, coating homogeneity and flatness poor.
(embodiment 1)
When the preparation of the composition of reference example 1, with acetic acid 3-methoxybutyl, (H) composition ((H)-2) is diluted to after concentration is 10 quality % from stoste (40 quality %), aperture is utilized to be that the PTFE film (PALL Inc.) of 0.05 μm is filtered, in addition, the method same with reference example 1 is adopted to obtain light shield layer formation photonasty substrate composition.
The glass substrate with clean surface of thickness 1mm uses spin coater (TR25000: chemical industry Inc. is answered in Tokyo), the mode being 1.2 μm with dry film thickness is coated with the light shield layer formation photonasty substrate composition of gained, carry out drying in 2 minutes at 90 DEG C, define the film (photographic layer) of light shield layer formation photonasty substrate composition.
Next, exposure machine (EXM-1066-E01:ORC Inc.) is utilized to expose.After exposure, 0.04% potassium hydroxide developer solution is utilized to carry out development in 60 seconds by spray pattern.And then, cure after carrying out 30 minutes at 200 DEG C, form the black matrix of the matrix pattern of 20 μm of thickness 1.0 μm, dot pattern, isolated patterns.
The presence or absence of the pin hole of the black matrix of visual confirmation gained, result does not confirm pin hole, can obtain good black matrix.
(comparative example 5)
(H) composition is not filtered, in addition, adopt method similarly to Example 1 to obtain light shield layer formation photonasty substrate composition.And then, use the light shield layer of gained to be formed and use photonasty substrate composition, adopt method similarly to Example 1, define photographic layer, black matrix.The presence or absence of the pin hole of the black matrix of visual confirmation, results verification is to tens pin holes.
(comparative example 6)
(H) composition do not diluted and filtered, in addition, adopting method similarly to Example 1 to obtain light shield layer formation photonasty substrate composition.But, add solvent separately, with make (H) composition identical with embodiment 1 relative to the ultimate density of light shield layer formation photonasty substrate composition become 10 quality %.And then, use the light shield layer of gained to be formed and use photonasty substrate composition, adopt method similarly to Example 1, define photographic layer, black matrix.The presence or absence of the pin hole of the black matrix of visual confirmation, results verification is to tens pin holes.
(embodiment 2)
Composition is changed to the composition of reference example 2, in addition, adopt method similarly to Example 1 to obtain light shield layer formation photonasty substrate composition.And then, use the light shield layer of gained to be formed and use photonasty substrate composition, adopt method similarly to Example 1, define photographic layer, black matrix.
The presence or absence of the pin hole of the black matrix of visual confirmation gained, result does not confirm pin hole, can obtain good black matrix.
(comparative example 7)
(H) composition is not filtered, in addition, adopt method similarly to Example 2 to obtain light shield layer formation photonasty substrate composition.And then, use the light shield layer of gained to be formed and use photonasty substrate composition, adopt method similarly to Example 2, define photographic layer, black matrix.The presence or absence of the pin hole of the black matrix of visual confirmation, results verification is to tens pin holes.
(comparative example 8)
(H) composition do not diluted and filtered, in addition, adopting method similarly to Example 2 to obtain light shield layer formation photonasty substrate composition.But, add solvent separately, with make (H) composition identical with embodiment 2 relative to the ultimate density of light shield layer formation photonasty substrate composition become 10 quality %.And then, use the light shield layer of gained to be formed and use photonasty substrate composition, adopt method similarly to Example 2, define photographic layer, black matrix.The presence or absence of the pin hole of the black matrix of visual confirmation, results verification is to tens pin holes.
(embodiment 3)
Composition is changed to the composition of reference example 6, in addition, adopt method similarly to Example 1 to obtain light shield layer formation photonasty substrate composition.And then, use the light shield layer of gained to be formed and use photonasty substrate composition, adopt method similarly to Example 1, define photographic layer, black matrix.
The presence or absence of the pin hole of the black matrix of visual confirmation gained, result does not confirm pin hole, can obtain good black matrix.
(comparative example 9)
(H) composition is not filtered, in addition, adopt method similarly to Example 3 to obtain light shield layer formation photonasty substrate composition.And then, use the light shield layer of gained to be formed and use photonasty substrate composition, adopt method similarly to Example 3, define photographic layer, black matrix.The presence or absence of the pin hole of the black matrix of visual confirmation, results verification is to tens pin holes.
(comparative example 10)
(H) composition do not diluted and filtered, in addition, adopting method similarly to Example 3 to obtain light shield layer formation photonasty substrate composition.But, add solvent separately, with make (H) composition identical with embodiment 3 relative to the ultimate density of light shield layer formation photonasty substrate composition become 10 quality %.And then, use the light shield layer of gained to be formed and use photonasty substrate composition, adopt method similarly to Example 3, define photographic layer, black matrix.The presence or absence of the pin hole of the black matrix of visual confirmation, results verification is to tens pin holes.
From the result of embodiment 1 ~ 3 and comparative example 5 ~ comparative example 10, by filtering after (H) component diluent, even if when the molecular weight of (H) composition be more than 10000 large like this, also can not be produced the black matrix of the high-quality of pin hole.
According to the display of above-mentioned result, the manufacture method of light shield layer formation photonasty substrate composition of the present invention can not be produced the black matrix of the high-quality of pin hole.
Claims (5)
1. light shield layer forms the manufacture method with photonasty substrate composition, it is characterized in that,
Filter after the surfactant component (H) as weight-average molecular weight being the polymkeric substance of 10000 ~ 50000 is diluted to 2.5 ~ 10 quality %,
This surfactant component (H) after filtration, photonasty base material component (A), pigment composition (G) and Elements in Organic Solvents (S) are disperseed,
The polymkeric substance that described surfactant component (H) is the fluoro-alkyl and lyophily group side chain with carbon number 1 ~ 20.
2. the manufacture method of light shield layer formation photonasty substrate composition according to claim 1, wherein,
Described filtration aperture is that the PTFE film of less than 1 μm is carried out.
3. the manufacture method of light shield layer formation photonasty substrate composition according to claim 1 and 2, wherein,
Described photonasty base material component (A) is containing alkali-soluble base material (A1).
4. the manufacture method of light shield layer formation photonasty substrate composition according to claim 1 and 2, wherein,
Described photonasty base material component (A) is containing photopolymerizable compound (A2).
5. the manufacture method of light shield layer formation photonasty substrate composition according to claim 4, wherein,
Described photonasty base material component (A) is containing Photoepolymerizationinitiater initiater (A3).
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| CN101799627A (en) * | 2009-02-09 | 2010-08-11 | 日油株式会社 | Positive type photosensitive organic compound |
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| JP3550248B2 (en) * | 1996-03-28 | 2004-08-04 | ライオン株式会社 | Purification method of nonionic surfactant |
| JPH1033983A (en) * | 1996-07-24 | 1998-02-10 | Lion Corp | Purification of nonionic surface-active agent |
| JP2002049161A (en) * | 2000-08-04 | 2002-02-15 | Clariant (Japan) Kk | Aqueous surfactant solution for developing coating layer |
| US20020081520A1 (en) * | 2000-12-21 | 2002-06-27 | Ratnam Sooriyakumaran | Substantially transparent aqueous base soluble polymer system for use in 157 nm resist applications |
| JP2003330202A (en) * | 2002-05-09 | 2003-11-19 | Fuji Photo Film Co Ltd | Method for manufacturing positive resist composition |
| KR101176101B1 (en) * | 2004-06-18 | 2012-08-22 | 후지필름 가부시키가이샤 | Colored photosensitive resin composition, coating film of colored photosensitive resin composition, photosensitive resin transfer material, method for forming photosensitive resin layer, color filter, method for manufacturing color filter and liquid crystal display |
| EP1690551A3 (en) * | 2005-02-10 | 2006-10-18 | Sindan Pharma Srl | Method of purifying a surfactant by ultrafiltration |
| JP5507938B2 (en) * | 2008-10-01 | 2014-05-28 | 東京応化工業株式会社 | Photosensitive resin composition for color filter, color filter, and liquid crystal display |
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