CN101561526A - Composite phase difference board and manufacturing method thereof - Google Patents

Composite phase difference board and manufacturing method thereof Download PDF

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CN101561526A
CN101561526A CNA2009101304785A CN200910130478A CN101561526A CN 101561526 A CN101561526 A CN 101561526A CN A2009101304785 A CNA2009101304785 A CN A2009101304785A CN 200910130478 A CN200910130478 A CN 200910130478A CN 101561526 A CN101561526 A CN 101561526A
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polarizer
phase difference
composite phase
difference board
liquid crystal
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落合钢志郎
小林忠弘
九内雄一朗
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Sumitomo Chemical Co Ltd
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Sumitomo Chemical Co Ltd
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Abstract

The present invention provides a composite phase difference board, including a phase difference board (1) obtained by polymerizing liquid crystal compounds with polymerism groups, and a phase difference board (2) containing an organic decorative clay composite body and an adhesive resin.

Description

Composite phase difference board and manufacture method thereof
Technical field
The present invention relates to a kind of composite phase difference board and manufacture method thereof.
Background technology
Composite phase difference board contains several polarizers of the circular polarization tabula rasa that λ/4 and λ/2 plates engaged and obtain etc., is used for liquid crystal indicator etc.
The Jap.P. spy opens the 2005-338215 communique and discloses a kind of composite phase difference board, is λ/4 plates of constituting of the stretched film of resin and obtaining with cementing agent bonding by cyclic polyolefin on the polarizer that contains organic decoration clay complex and adhesive resin.
Summary of the invention
The invention provides following technical scheme:
＜1〉a kind of composite phase difference board contains polarizer (1) that obtains and the polarizer (2) that contains organic decoration clay complex and adhesive resin by the liquid-crystal compounds polymerization with polymerism base.
＜2〉as＜1〉described composite phase difference board, wherein, polarizer (1) is the polarizer of positive uniaxiality.
＜3〉as＜1〉or＜2〉described composite phase difference board, wherein, polarizer (2) is the polarizer of negative uniaxiality.
＜4〉as＜1 〉～＜3〉each described composite phase difference board, wherein, organic decoration clay complex contains quaternary ammonium salt and belongs to the clay mineral of smectite family, the atomic ratio (Mg/Si of magnesium that these mineral are contained and 4 atom silicon 4) less than 2.73.
＜5〉as＜1 〉～＜4〉each described composite phase difference board, wherein, the liquid-crystal compounds with polymerism base is the liquid-crystal compounds with polymerism base of formula (D-1)～(D-5) expression, in the formula, and R 1～R 5Alkyl or the hydrogen atom of representing carbon number 1～4 respectively independently.
Figure A20091013047800041
＜6〉as＜1 〉～＜5 each described composite phase difference board, wherein, polarizer (1) engages with polarizer (2) and forms.
＜7〉as＜1 〉～＜5 each described composite phase difference board, wherein, also contain undercoat, this undercoat is arranged between polarizer (1) and the polarizer (2).
＜8〉as＜1 〉～＜7 each described composite phase difference board, wherein, the light that sees through composite phase difference board is at the front of wavelength 550nm phase difference value (R 0(550)) be 113～163nm.
＜9〉a kind of polarized light member is characterized in that, contain＜1～＜8 each described composite phase difference board and polarization plate.
＜10〉a kind of liquid crystal indicator is characterized in that, contain＜9〉described polarized light member and liquid crystal cell.
＜11〉a kind of optical component is characterized in that, contain＜1～＜8 each described composite phase difference board and color filter.
＜12〉a kind of manufacture method of composite phase difference board is characterized in that, have following (i)～(operation v), (i) mixing has the operation of the liquid-crystal compounds and the organic solvent of polymerism base; (ii) the solution that is obtained by operation (i) obtains the operation of coat film; (iii) make the contained liquid-crystal compounds polymerization of coat film that obtains in (ii) in operation and obtain the operation of polarizer (1) with polymerism base; The operation of (iv) mixing organic decoration clay complex, adhesive resin and organic solvent; (v) will be coated on the operation that resulting polarizer (1) upward obtains composite phase difference board at the coating liquid that operation (iv) obtains.
＜13〉a kind of manufacture method of composite phase difference board is characterized in that, have following (i)～(iv) reach (vi)～(and operation vii), (i) mixing has the operation of the liquid-crystal compounds and the organic solvent of polymerism base; (ii) the solution that is obtained by operation (i) obtains the operation of coat film; (iii) make the contained liquid-crystal compounds polymerization of coat film that obtains in (ii) in operation and obtain the operation of polarizer (1) with polymerism base; The operation of (iv) mixing organic decoration clay complex, adhesive resin and organic solvent; (vi) go up the operation that is coated with primer and goes up the formation undercoat at polarizer (1) at resulting polarizer (1); (vii) will be coated on the undercoat and obtain the operation of composite phase difference board at the coating liquid that operation obtains in (iv).
Description of drawings
Fig. 1 is the cross section mode chart that composite phase difference board represented in summary;
Fig. 2 is the summary cross section mode chart that contains oriented film and/or support the composite phase difference board of base material;
Fig. 3 is the summary cross section mode chart that contains the polarized light member of composite phase difference board;
Fig. 4 is the summary cross section mode chart that contains the liquid crystal indicator of polarized light member and liquid crystal cell;
Fig. 5 is the summary cross section mode chart that contains the optical component of composite phase difference board and color filter;
Symbol description
11 polarizers (1)
12 polarizers (2)
13 undercoats
14 support base material
15 oriented films
16 adhesive layers
17 polarization plates
18 polarized light members
19 liquid crystal cells
20 color-filter layers
Embodiment
Composite phase difference board of the present invention contains polarizer (1) that obtains and the polarizer (2) that contains organic decoration clay complex and adhesive resin by the liquid-crystal compounds polymerization with polymerism base.
Polarizer (1) is the polarizer that is obtained by the liquid-crystal compounds polymerization with polymerism base, " liquid-crystal compounds with polymerism base " is meant polymerization and gives the monomer of liquid crystal phase, be the compound that dissolves in organic solvent (below, abbreviate liquid crystal monomer as).
Polarizer (1) can be obtained by a kind of liquid crystal monomer polymerization, also can be obtained by two or more liquid crystal monomer polymerizations.
As desirable liquid crystal monomer, have for example and have following formula (D-1)～(D-5) (in the formula, R 1～R 5Alkyl or the hydrogen atom of representing carbon number 1～4 respectively independently) expression polymerism base, liquid crystal base (メ ソ ゲ Application), connect their group and be selected from least one liquid crystal monomer in alkoxy, cyano group, nitro, trifluoromethyl, dimethylamino and the halogen atom of alkyl, carbon number 1～13 of carbon number 1～13 as required.Especially, it is desirable to contain the liquid crystal monomer of the polymerism base of formula (D-1) expression.
As the liquid crystal base, aromatic hydrocarbyl, fluorenes two bases of heterocyclic radical, the divalent of ester ring type alkyl, the divalent of divalent etc. are arranged for example, and these groups can have at least one group in alkoxy, cyano group, nitro, trifluoromethyl, dimethylamino and the halogen atom of the alkyl that is selected from hydrogen atom, carbon number 1～13, carbon number 1～13.
The group that has following formula to represent for example as the ester ring type alkyl.
Figure A20091013047800071
The group that has following formula to represent for example as heterocyclic radical.
Figure A20091013047800072
The group that has following formula to represent for example as aromatic hydrocarbyl.
Figure A20091013047800073
Especially, it is desirable to have the ester ring type alkyl that is selected from divalent, the aromatic hydrocarbyl of divalent and the liquid crystal monomer of at least one group in fluorenes two bases as the liquid crystal base, better is to have 1,4-cyclohexane two bases, 1,4-phenylene, 2,7-naphthalene two bases, 2,7-fluorenes two base and 4,4 '-liquid crystal monomer of at least 2 groups in biphenyl two bases.
As the group that connects polymerism base and liquid crystal base, have for example can with the alkylidene of the carbon number 1～12 of at least one replacement of the alkoxy of the alkyl that is selected from carbon number 1～5, carbon number 1～5 and halogen atom and at least one of this alkylidene terminal with-CR 11R 12-,-C ≡ C-,-CH=CH-,-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-or-O-C (=O)-CH=CH-bonding and the group that obtains.R 11And R 12The alkyl of representing hydrogen atom, fluorine atom or carbon number 1～4 respectively independently, perhaps R 11And R 12Bonding and form the alkylidene of carbon number 5～7 forms ring with its bonding carbon atom.
Especially, it is desirable to carbon number 1～12 alkylidene and at least one of this alkylidene terminal with-C ≡ C-,-CH=CH-,-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-or-O-C (=O)-CH=CH-bonding and the group that obtains.The alkylidene of better is carbon number 1～12 and at least one of this alkylidene terminal with-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-or-O-C (=O)-CH=CH-bonding and the group that obtains, it is desirable to especially carbon number 1～12 alkylidene and two ends of this alkylidene and-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 1 1-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-or-O-C (=O)-CH=CH-bonding and the group that obtains.
As the group that connects liquid crystal base and liquid crystal base, have for example the alkoxy of the alkyl that can be selected from carbon number 1～5, carbon number 1～5 and halogen atom at least one replacement carbon number 1～12 alkylidene ,-CR 11R 12-,-C ≡ C-,-CH=CH-,-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-,-O-C (=O)-CH=CH-, singly-bound etc.R 11And R 12The expression and the above-mentioned same meaning.Especially, it is desirable to-CH 2-CH 2-,-C ≡ C-,-CH=CH-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-,-O-C (=O)-and CH=CH-and singly-bound, better is-CH 2-CH 2-,-C ≡ C-,-CH=CH-,-C (=O)-O-,-O-C (=O)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-and singly-bound.
Object lesson as liquid crystal monomer, the compound that has the polymerism base in " 3.2 achiralitys (the ノ Application キ ラ Le) rod shaped liquid crystal molecule " of " 3 chapter molecular structure and liquid crystal liquid crystal property " of liquid crystal brief guide (liquid crystal brief guide editorial board compiles, and ball kind (strain) is put down into distribution on October 30th, 12) and the compound that " 3.3 chirality rod shaped liquid crystal molecule " put down in writing is arranged for example.
The compound that following formula (I)～formula (V) expression is arranged particularly, for example.
P11-E11-B11-A11-B12-A12-B13-A13-B14-A14-B15-A15-B16-E12-P12 (I)
P11-E11-B11-A11-B12-A12-B13-A13-B14-A14-B15-E12-P12 (II)
P11-E11-B11-A11-B12-A12-B13-A13-B14-E12-P12 (III)
P11-E11-B11-A11-B12-A12-B13-A13-B14-F11 (IV)
P11-E11-B11-A11-B12-A12-B13-F11 (V)
In above-mentioned formula (I)～formula (V), A11, A12, A13, A14 and A15 represent the ester ring type alkyl of divalent, the heterocyclic radical of divalent, the aromatic hydrocarbyl or fluorenes two bases of divalent respectively independently, and these bases can have the group of alkoxy, nitro, cyano group, phenyl, dimethylamino and the halogen atom of at least one alkyl that is selected from carbon number 1～5, carbon number 1～5.
As the aromatic hydrocarbyl of the heterocyclic radical of the ester ring type alkyl of the divalent of A11, A12, A13, A14 and A15, divalent and divalent respectively for example and above-mentioned the same group.Especially, it is desirable to, A11, A12, A13, A14 and A15 are the ester ring type alkyl of divalent, the aromatic hydrocarbyl or fluorenes two bases of divalent independently, and better is, be 1 independently, 4-cyclohexane two bases, 1,4-phenylene, 2,7-naphthalene two bases, 2,7-fluorenes two bases or 4,4 '-biphenyl two bases.
B11, B12, B13, B14, B15 and B16 difference be expression-CR independently 11R 12-,-C ≡ C-,-CH=CH-,-CH 2-CH 2-,-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-,-O-C (=O)-and CH=CH-or singly-bound, R 11And R 12The alkyl of representing hydrogen atom, fluorine atom or carbon number 1～4 respectively independently, perhaps R 11And R 12Bonding and form the alkylidene of carbon number 5～7 forms ring with its bonding carbon atom.
With B11, the B14 of E11 or E12 adjacency, B15 and B16 respectively independently expression-C ≡ C-,-CH=CH-,-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-,-O-C (=O)-CH=CH-or singly-bound, it is desirable to, for-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-,-O-C (=O)-CH=CH-or singly-bound.
With the B12 of A11 and A12 bonding, with the B13 of A12 and A13 bonding, with the B14 of A13 and A14 bonding, with the B15 of A14 and A15 bonding represent the carbon atom 1～12 that can replace with at least one group of the alkoxy of the alkyl that is selected from carbon number 1～5, carbon number 1～5 and halogen atom alkylidene ,-CR 11R 12-,-C ≡ C-,-CH=CH-,-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-,-O-C (=O)-and CH=CH-or singly-bound, it is desirable to, for-CH 2-CH 2-,-C ≡ C-,-CH=CH-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-,-O-C (=O)-CH=CH-or singly-bound, better is, for-CH 2-CH 2-,-C ≡ C-,-CH=CH-,-C (=O)-O-,-O-C (=O)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-or singly-bound.
E11 and E12 be the alkylidene of the expression carbon atom 1～12 that can replace with at least one group of the alkoxy of the alkyl that is selected from carbon number 1～5, carbon number 1～5 and halogen atom, this alkylidene and end P11 or P12 bonding and-CR independently respectively 11R 12-,-C ≡ C-,-CH=CH-,-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-or-O-C (=O)-CH=CH-bonding and the group that obtains, it is desirable to, the alkylidene of carbon atom 1～12, this alkylidene and end P11 or P12 bonding and-C ≡ C-,-CH=CH-,-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-CH=N-,-N=CH-,-N=N-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-or-O-C (=O)-CH=CH-bonding and the group that obtains, better is, the alkylidene of carbon atom 1～12, this alkylidene and end P11 or P12 bonding and-O-,-S-,-C (=O)-,-C (=O)-O-,-O-C (=O)-,-O-C (=O)-O-,-C (=S)-,-C (=S)-O-,-O-C (=S)-,-C (=O)-NR 11-,-NR 11-C (=O)-,-OCH 2-,-OCF 2-,-NR 11-,-CH 2O-,-CF 2O-,-CH=CH-C (=O)-O-or-O-C (=O)-CH=CH-bonding and the group that obtains.
P11 represents the polymerism base of above-mentioned formula (D-1)～(D-5) expression, and P12 represents the polymerism base or the hydrogen atom of above-mentioned formula (D-1)～(D-5) expression.
F11 represents the alkyl of hydrogen atom, carbon number 1～13, alkoxy, cyano group, nitro, trifluoromethyl, dimethylamino or the halogen atom of carbon number 1～13.
Can use the liquid crystal monomer more than 2 kinds.
As liquid crystal monomer, it is desirable at least one in the liquid crystal monomer of the formula that is selected from (I), formula (II) and formula (III) expression.
As the object lesson of liquid crystal monomer, the compound of following formula (I-1)～(I-5), (II-1)～(II-6), (III-1)～(III-19), (IV-1)～(IV-14), (V-1)～(V-5) expression is arranged for example.In the following formula, m represents 1～12 integer respectively independently.
Figure A20091013047800111
Figure A20091013047800121
Figure A20091013047800131
Figure A20091013047800141
Be above-mentioned liquid crystal monomer, owing to make easily or obtaining easily of market sale etc. and desirable.
For example, the solution coat by will containing liquid crystal monomer and organic solvent supporting on base material or the oriented film etc., removes organic solvent then and filmed, and makes the liquid crystal monomer polymerization in resulting the filming, and obtains polarizer (1).
Below, the manufacture method of described polarizer (1) is described.
[(i) preparation contains the operation of the coating liquid of liquid crystal monomer and organic solvent]
At first, be dissolved in the organic solvent by making liquid crystal monomer, preparation contains the coating liquid (below abbreviate coating liquid (1) as) of liquid crystal monomer and organic solvent.As required, coating liquid (1) can contain the adjuvant of polymerization initiator, polymerization inhibitor, photosensitizer, crosslinking chemical, levelling agent etc.Especially, polymerization initiator owing to have makes effect that resulting polarizer solidifies and ideal.Again, for purpose of the optical characteristics of control phase difference plate etc., can be in coating liquid (1) compound outside the mixed liquid crystal monomer.
[organic solvent]
As organic solvent,, particularly, the alcoholic solvent of methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol, propylene glycol, methyl cellosolve, butyl cellosolve, propylene glycol monomethyl ether, phenol etc. is arranged for example so long as the organic solvent of solubilized liquid crystal monomer gets final product; The ester solvent of ethyl acetate, butyl acetate, Ethylene Glycol Methyl ether acetic acid ester, gamma-butyrolacton, methyl proxitol acetate, ethyl lactate etc.; The ketone solvent of acetone, methyl ethyl ketone, cyclopentanone, cyclohexanone, methyl amyl ketone, hexone etc.; The chlorine-free aliphatic hydrocarbon solvent of pentane, hexane, heptane etc.; The chlorine-free aromatic hydrocarbon solvents of toluene, dimethylbenzene etc.; The nitrile solvent of acetonitrile etc.; The ether solvents of tetrahydrofuran, dimethoxy-ethane etc.; The chlorine of chloroform, chlorobenzene etc. is hydrocarbon solvent etc.These organic solvents may be used alone, two or more kinds can also be used in combination.Especially, above-mentioned liquid crystal monomer is because intermiscibility is good, also can be dissolved in alcoholic solvent, ester solvent, ketone solvent, chlorine-free aliphatic hydrocarbon solvent and chlorine-free aromatic hydrocarbon solvents, so, also can dissolve and prepare coating liquid (1) even not using the chlorine of chloroform etc. is hydrocarbon solvent.Described organic solvent can contain water.
[polymerization initiator]
Coating liquid (1) it is desirable to contain the polymerization initiator that the liquid crystal monomer polymerization is used as mentioned above.As polymerization initiator thermal polymerization, Photoepolymerizationinitiater initiater etc. are arranged for example,, it is desirable to Photoepolymerizationinitiater initiater from can be at low temperatures and liquid crystal monomer polymerization this respect is considered.
As thermal polymerization, have 2,2 for example '-azo two (isobutyronotrile), 4,4 '-superoxide of the azo series initiators of azo two (4-cyanopentanoic acid) etc., benzoyl peroxide etc. etc.
As Photoepolymerizationinitiater initiater, benzoin compound, benzophenone cpd, benzyl ketal compound, alpha-hydroxyacetone compounds, alpha-amido ketonic compound, salt compounded of iodine, sulfonium salt etc. are arranged for example.Particularly, Irgacure907 is arranged for example, Irgacure184, Irgacure651, Irgacure819, Irgacure250, Irgacure369 (more than, all be that チ バ ス ペ シ ャ Le テ ィ ケ ミ カ Le ズ company makes), セ ィ Network オ one Le BZ, セ ィ Network オ one Le Z, セ ィ Network オ one Le BEE (more than, all be that Seiko chemical company makes), kayacureBP100 (Japanese chemical drug corporate system is made), kayacureUVI-6992 (manufacturing of ダ ゥ company), ァ デ カ オ プ ト マ one SP-152, ァ デ カ オ プ ト マ one SP-170 (more than, all be that rising sun electrification is made) etc.
The use amount of polymerization initiator is generally 0.1 weight portion～30 weight portions with respect to summation 100 weight portions of liquid crystal monomer, it is desirable to 0.5 weight portion～10 weight portions.In above-mentioned scope, can make it polymerization not upsetting under the direction-sense situation of liquid crystal monomer.
[polymerization inhibitor]
Coating liquid (1) can contain polymerization inhibitor.As polymerization inhibitor, quinhydrones is arranged for example, have substituent catechin compoundses such as alkoxy, the 1,2,3,-thrihydroxy-benzene compound, 2 with methoxyl etc. of the substituent hydroquinone compounds such as alkoxy, butyl catechol etc. of methoxyl etc., 2,6, the free radical scavenger of 6-tetramethyl-1-piperidines oxygen base free radical etc., thiophenol compound, betanaphthyl amines, betanaphthol compound etc.
By using polymerization inhibitor, can easily control the polymerization of liquid crystal monomer, the stability of resulting polarizer and the stability of coating liquid (1) are improved.The use amount of polymerization inhibitor is generally 0.1 weight portion～30 weight portions with respect to summation 100 weight portions of liquid crystal monomer, it is desirable to 0.5 weight portion～10 weight portions.In above-mentioned scope, can make it polymerization not upsetting under the direction-sense situation of liquid crystal monomer.
[photosensitizer]
Coating liquid (1) can contain photosensitizer.As photosensitizer have for example xanthone, thioxanthones etc. xanthone compound, anthracene, have substituent anthracene compound, phenothiazine, the rubrenes etc. such as alkoxy of methoxyl etc.
By using photosensitizer, can carry out the polymerization of liquid crystal monomer with higher sensitivity.The use amount of photosensitizer is generally 0.1 weight portion～30 weight portions with respect to summation 100 weight portions of liquid crystal monomer, it is desirable to 0.5 weight portion～10 weight portions.In above-mentioned scope, can make it polymerization not upsetting under the direction-sense situation of liquid crystal monomer.
[levelling agent]
Coating liquid (1) can contain levelling agent.(PVC ッ Network ケ ミ one ジ ャ パ Application is made: BYK-352 with adjuvant as levelling agent radiation setting coating for example, BYK-353, BYK-361N), (East レ ダ ゥ コ one ニ Application グ company makes coating additive: SH28PA, DC11PA, ST80PA), (polysiloxane company of SHIN-ETSU HANTOTAI makes coating additive: KP321, KP323, X22-161A, KF6001), fluorine be adjuvant (Dainippon Ink Chemicals makes: F-445, F-470, F-479) etc.
By using levelling agent, can obtain more level and smooth polarizer.And, in the manufacture process of polarizer, also can control the flowability of coating liquid (1), perhaps adjust the cross-linking density of polarizer.The use amount of levelling agent is generally 0.1 weight portion～30 weight portions with respect to summation 100 weight portions of liquid crystal monomer, it is desirable to 0.5 weight portion～10 weight portions.In above-mentioned scope, can make it polymerization not upsetting under the direction-sense situation of liquid crystal monomer.
Coating liquid (1) mixes, dissolves after above-mentioned each composition, usually viscosity is adjusted into below the 10Pas, it is desirable to about 0.1～7Pas, so that easily be coated with.
The concentration that solid formation in the coating liquid (1) divides is generally 5～50 weight %.
[the (ii) operation that obtains filming by the resulting solution of operation (i)]
After being coated on the resulting coating liquid of above-mentioned operation (i) (1) on support base material or the oriented film etc.,, filmed by removing organic solvent.It is desirable to, on oriented film, be coated with coating liquid (1) afterwards, remove organic solvent, filmed.
[oriented film]
Oriented film need have not can coated liquid (1) dissolving solvent resistance, have peeling off of causing of the thermotolerance that is used for removing organic solvent or adjusting the direction-sense heat treated of liquid crystal monomer, the friction etc. that can not grind generation etc., contain polymkeric substance.
As above-mentioned polymkeric substance, it is the polymkeric substance of polyamic acid, polyvinyl alcohol (PVA), alkyl-modified polyvinyl alcohol (PVA), polyacrylamide, Ju oxazole, polyethyleneimine, polystyrene, polyvinylpyrrolidone, polyacrylic acid or polyacrylate etc. that the polyimide and the hydrolysate thereof that have imine linkage in the polyamide that has amido link in the molecule or keratin class, the molecule can be arranged for example.These polymkeric substance may be used alone, can also be two or more kinds in combination, and also can be used as multipolymer and use.These polymkeric substance can or take off the polycondensation of amine etc. or the chain polymerization of free radical polymerization, anionic polymerisation, cationic polymerization etc., coordination polymerization, ring-opening polymerization etc. easily obtain by dehydration.
Described polymkeric substance is dissolved in the solvent usually, is coated on to support on the base material again.As solvent without limits, particularly, the alcoholic solvent of water, methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol, propylene glycol, methyl cellosolve, butyl cellosolve etc. is arranged for example; The ester solvent of ethyl acetate, butyl acetate, Ethylene Glycol Methyl ether acetic acid ester, gamma-butyrolacton, methyl proxitol acetate, ethyl lactate etc.; The ketone solvent of acetone, methyl ethyl ketone, cyclopentanone, cyclohexanone, methyl amyl ketone, hexone etc.; The aliphatic hydrocarbon solvent of pentane, hexane, heptane etc.; The aromatic hydrocarbon solvents of toluene, dimethylbenzene, chlorobenzene etc.; The nitrile solvent of acetonitrile etc.; The ether solvents of propylene glycol monomethyl ether, tetrahydrofuran, dimethoxy-ethane etc.; The halogenated hydrocarbon solvent of chloroform etc. etc.These organic solvents may be used alone, two or more kinds can also be used in combination.
In order to form oriented film, can directly use the oriented film material of selling in market.As the oriented film material of selling in market, サ Application ェ バ one (registered trademark, daily output chemical company makes), オ プ ト マ one (registered trademark, JSR makes) etc. are arranged for example.
Use such oriented film, because the orientation of liquid crystal monomer becomes easily, so disperse in birefracting (ば ら っ I) diminishes.Therefore, play such effect: the also adaptable bigger polarizer of maximization that FPD can be provided.Again, utilize the material of oriented film or grinding condition etc., the orientation easier control that also becomes can obtain the various orientations of horizontal orientation, vertical orientation, mixing orientation, inclined orientation etc., can be used to field angle of improving various liquid crystal panels etc.
For example, the solution by at the compound of the material of supporting to be coated on the oriented film material of selling in market on the base material or to become oriented film by annealing, can form oriented film then.
The thickness of oriented film is generally 10nm～10000nm, it is desirable to 10nm～1000nm.In above-mentioned scope, during coating coating liquid (1), can make liquid crystal monomer direction or angle orientation with hope on this oriented film.
Usually these oriented films are ground or the polarized ultraviolet irradiation.By using oriented film, can make direction or the angle orientation of liquid crystal monomer with hope through these processing.
As the method for grinding oriented film, have for example on making the mixing roll that is rotating that is wound with abrasive cloth and being placed on objective table and the method that the oriented film on the support base material that is transported contacts.
As the method for preparing oriented film supporting coating oriented film material on the base material, extrude cladding process, direct intaglio plate cladding process, reverse intaglio plate cladding process (reverse gravure coating), CAP cladding process, metal mold cladding process (ダ ィ コ one テ ィ Application グ) etc. for example.The method that also has coaters such as using dipping coater, bar type coater, spinner to be coated with again for example.
Above-mentioned support base material is to support to form on the base material getting final product of oriented film at this.For example glass, plastic tab, plastic foil, light transmissive film etc. are arranged for example.As light transmissive film, polyene film, polyvinyl alcohol film, polyethylene terephthalate film, polymethacrylate film, polyacrylate film, cellulose ester membrane, poly (ethylene naphthalate) film, polycarbonate membrane, polysulfone membrane, poly (ether sulfone) film, polyetherketone film, polyphenylene sulfides film, polyphenylene oxide film of tygon, polypropylene, the rare based polymer of norborneol etc. etc. are arranged for example.
Polarizer of the present invention (1) is generally film, even but when needing film strength with composite phase difference board of the present invention and other member engages or carrying, keeping polarizer (1) time etc., also can support base material by using, and operation easily under not damaged situation.
As the method that on oriented film, is coated with coating liquid (1), have for example with above-mentioned oriented film material is coated on and support the same method on the base material.
The coating weight by suitably adjusting coating liquid (1) or the amount of the organic solvent in the coating liquid (1), thickness that can modulation phase potential difference plate (1) is to give the phase differential with hope.Owing to determine phase difference value (length of delay (retardation), the R of the frontal in the polarizer (1) as the formula (3) 0(λ)), so R in order to obtain wishing 0(λ), as long as adjust thickness d.
R 0(λ)＝d×Δn(λ)(3)
(in the formula, R 0(λ) be illustrated in phase difference value among the wavelength X nm, d represents thickness, and Δ n (λ) is illustrated in the refractive index anisotropy among the wavelength X nm.)
The phase difference value of resulting polarizer (1) is suitably selected to get final product according to the purposes of the composite phase difference board scope from about 30～300nm.For example, when using composite phase difference board in the more small-sized liquid crystal indicator as mobile phone or portable information terminal, polarizer (1) is favourable for λ/4 plates.
For example, for polarizer (1) is used as broadband λ/4 plates or λ/2 plates, suitably select the content from the structural unit of liquid crystal monomer, the thickness of adjusting polarizer (1) according to formula (3) gets final product.It is desirable to, the thickness of polarizer (1) is 0.1～10 μ m, and from making the photoelasticity this point that diminishes, further it is desirable to is 0.5～3 μ m.
Particularly, λ/4 plates is with the R of resulting polarizer (1) 0(550) be adjusted into 113～163nm, it is desirable to be adjusted into 130～150nm and get final product, λ/2 plates is with the R of resulting polarizer 0(550) be adjusted into 250～300nm, it is desirable to be adjusted into 265～285nm and get final product.Therefore, for the phase difference value that obtains wishing, also can adjust thickness.
In the time of coating coating liquid (1) or after the coating, remove organic solvent.The method of removing organic solvent has the method for air dry, aeration-drying, drying under reduced pressure etc. for example.Removing that temperature it is desirable to is 10～150 ℃, and better is to be 25～120 ℃.The time of removing it is desirable to 10 second～60 minute, better is 30 second～30 minute.Remove temperature and the time of removing in above-mentioned scope, even supporting that the thermotolerance of base material and oriented film is relatively lower also can use, therefore desirable.
Remove organic solvent and filming of obtaining is made of unpolymerized liquid crystal monomer.Usually because liquid crystal monomer gives the phase of the demonstration liquid crystal liquid crystal property of nematic phase etc., the double refraction that (domain) orientation that has single domain causes so this is filmed.It is desirable to, this is filmed usually about 0～150 ℃, preferably carry out orientation under 25～120 ℃ low temperature.
Remove after the organic solvent, can heat again, adjust the directed state of liquid crystal monomer.
[(iii) make the liquid crystal monomer polymerization and obtain the operation of polarizer (1)]
Contain unpolymerized liquid crystal monomer filming of obtaining in (ii) of operation,, obtain polarizer (1) by making its polymerization.Particularly, filming of obtaining carried out rayed, perhaps heat, perhaps carry out rayed and heating, make the liquid crystal monomer polymerization filming to filming.
The polymerism base that liquid crystal monomer contained is an optical polymerism, makes it to solidify by the light that shines visible light, ultraviolet light, laser etc. and implements polymerization, and this polymerism base is thermal polymerization, implements polymerization by heating.From the film forming viewpoint, it is desirable to photopolymerization, and from the operability viewpoint, better is to carry out polymerization by ultraviolet light.
It is desirable to, resulting polarizer (1) shows positive uniaxiality.Make polarizer (1) show positive uniaxiality, using molecular shape usually is that bar-shaped liquid crystal monomer gets final product.
The molecular shape of liquid crystal monomer is the bar-shaped liquid crystal base that is meant the divalent that has more than 2, have the compound of the group that connects liquid crystal base and liquid crystal base.The compound that above-listed formula (I)～formula (IV) expression is arranged particularly, for example.
[polarizer (2)]
Polarizer used in the present invention (2) contains organic decoration clay complex and adhesive resin, can remove organic solvent from the coating liquid that contains organic decoration clay complex, adhesive resin and organic solvent (below abbreviate coating liquid (2) as) usually and obtains.
Organic decoration clay complex is the complex of organism and clay mineral, specifically is compound and obtain complex with having the clay mineral of layer structure and organic compound, and it can be scattered in the organic solvent.
As clay mineral with layer structure, smectite family or swelling property mica etc. are arranged for example, can be compound by its cation exchange energy with organic compound.Especially, belong to the clay mineral of smectite family because the transparency is also good and desirable.The clay mineral that belongs to smectite family has hectorite, polynite, bentonitic clay etc. for example.Especially, chemosynthesis considers more satisfactory from few, the transparent good this respect of impurity.Especially, the synthetic li-montmorillonite of controlling particle diameter less preferably uses owing to suppress the scattering of luminous ray.
Especially, it is desirable to belong to the magnesium of smectite family and the atomic ratio (Mg/Si of 4 atom silicon 4) organic decoration clay complex less than 2.73.
As and organism that obtain compound with clay mineral, have for example can with the compound of the oxygen atom of clay mineral or hydroxyl reaction or can be with the ionic compound of exchangeable cation exchange etc.Particularly, the alkyl of 1～4 carbon number 1～30 and nitrogen atom bonding are arranged for example and the alkyl of the nitrogen-containing compound that obtains, 4 carbon numbers 1～30 and phosphorus atoms bonding and obtain the alkyl of De phosphonium salt, 3 carbon numbers 1～30 and sulfur atom linkage and sulfonium salt of obtaining etc.As above-mentioned nitrogen-containing compound primary amine, secondary amine, tertiary amine, quaternary ammonium salt etc. are arranged for example.
The alkyl of carbon number 1～30 has the alkyl of carbon number 1～30, the alkylidene of carbon number 1～30, the aralkyl of carbon number 7～30 etc. for example.It is desirable to, at least 1 is the alkyl of carbon number 4～20, and better is that at least 1 is the alkyl of carbon number 6～10.
It is desirable to quaternary ammonium salt.
Organic decoration clay complex also can be used in combination more than 2 kinds.The commercially available product of suitable organic decoration clay complex has the synthetic li-montmorillonite of selling with " Le one セ Application ィ ト STN " " Le one セ Application ィ ト SPN " trade name of コ one プ ケ ミ カ Le Co., Ltd. and the complex of quaternary ammonium salt etc.
Organic decoration clay complex contains with the form of chlorion etc. according to its chlorine sometimes of originating, and it is desirable to water and cleans organic decoration clay complex, makes described chlorinity in the coating liquid (2) 2, below the 000ppm.
Adhesive resin is to make organic decoration clay complex disperse, be dissolved in the material of the organic solvent of toluene, dimethylbenzene, acetone, ethyl acetate etc., especially, it is desirable to glass transition temperature (about below 20 ℃) below the room temperature.As desirable adhesive resin, acrylic resin, urethane resin, metha crylic resin, epoxy resin, vibrin of the cellulose-based resin, butyl acrylate etc. of the polyvinyl acetal resin, cellulose acetate butyrate etc. of polyvinyl butyral or polyvinyl formal etc. etc. are arranged for example.
As the commercially available product of adhesive resin, the acrylic resin of selling with " ァ ロ Application S1601 " trade name of aldehyde modified resin, the Toagosei Co., Ltd of the polyvinyl alcohol (PVA) of selling with " デ Application カ Block チ ラ one Le #3000-K " trade name of electrochemical industry Co., Ltd. is arranged for example, firmly change the urethane resin etc. of the isophorone diisocyanate matrix of selling with " SBU ラ ッ カ 1 " trade name of バ ィ ェ Le ゥ レ Application Co., Ltd..
The organic decoration clay complex in the polarizer (2) and the weight ratio of adhesive resin (organic decoration clay complex: adhesive resin) be generally 1: 2～10: 1, it is desirable to 1: 1～2: 1.
As the organic solvent in the coating liquid (2), it is the organic solvent that can disperse organic decoration clay complex, dissolving adhesive resin, the alcoholic solvent that methyl alcohol, ethanol, ethylene glycol, isopropyl alcohol, propylene glycol, methyl cellosolve, butyl cellosolve, propylene glycol monomethyl ether, phenol etc. are arranged particularly, for example; The ester solvent of ethyl acetate, butyl acetate, Ethylene Glycol Methyl ether acetic acid ester, gamma-butyrolacton, methyl proxitol acetate, ethyl lactate etc.; The ketone solvent of acetone, methyl ethyl ketone, cyclopentanone, cyclohexanone, methyl amyl ketone, hexone etc.; The chlorine-free aliphatic hydrocarbon solvent of pentane, hexane, heptane etc.; The chlorine-free aromatic hydrocarbon solvents of toluene, dimethylbenzene etc.; The nitrile solvent of acetonitrile etc.; The ether solvents of tetrahydrofuran, dimethoxy-ethane etc.; The chlorine of chloroform, chlorobenzene etc. is hydrocarbon solvent etc.These organic solvents may be used alone, two or more kinds can also be used in combination.
The polarizer that so obtains (2) shows negative uniaxiality usually.
[composite phase difference board]
Composite phase difference board of the present invention can engage polarizer (1) and polarizer (2), also can between polarizer (1) and polarizer (2) undercoat be set.
The composite phase difference board that engages polarizer (1) and polarizer (2) for example can be made by method as follows.
[operation that (iv) prepares coating liquid (2)]
Prepare coating liquid (2) by mixing organic decoration clay complex, adhesive resin and organic solvent.Usually, adhesive resin is dissolved in the organic solvent, and organic decoration clay complex is dispersed in the organic solvent.With the total concentration of organic decoration clay complex in the coating liquid (2) and adhesive resin be diluted to coating liquid in practicality no problem scope and can gelation or the degree of gonorrhoea get final product, be generally about 3～15 weight %.Optium concentration is according to organic decoration clay complex, adhesive resin kind and the difference of both ratio of componentss and difference separately, gets final product so set according to each composition.The various adjuvants such as crosslinking chemical that are used to improve the viscosity modifier of coating or are used for further improving hydrophobicity and/or permanance in the time of also can adding the system film.
Chlorinity in the coating liquid (2) it is desirable to 2, below the 000ppm.Chlorinity in the coating liquid (2) is 2, and 000ppm is following, tends to make liquid crystal cell glass to be situated between and is engaged forcefully by the surface of adhesive layer with resulting polarizer (2), so desirable.Chlorinity in the coating liquid (2) to be adjusted to 2, below the 000ppm, the method for aforesaid water cleaning organic decoration clay complex etc. be arranged for example.
It is desirable to, the water cut of usefulness Ka Er-coating liquid (2) that the Fei Xier moisture meter is measured is in the scope of 0.15～0.35 weight %.Water cut is below 0.35 weight %, and coating liquid (2) tends to water and organic phase is not easily separated, and water cut tends to suppress the haze value of polarizer (2) more than 0.15 weight %, and is therefore desirable.
[(v) coating liquid (2) is coated on the operation that polarizer (1) upward obtains composite phase difference board]
As the method that coating liquid (2) is coated on the polarizer (1), the rubbing method of direct intagliotype, reverse intagliotype, metal mold coating (ダ ィ コ one ト) method, comma coating (カ Application マ コ one ト) method, bar type rubbing method etc. is arranged for example.
The refractive index anisotropy of the thickness direction of polarizer (2) the phase difference value R of the thickness direction of through type (7) definition ThValue representation, this value can be by phase difference value R 40With the phase difference value R in the face 0Calculate phase difference value R 40Be meant the hysteresis axle in the face is made it 40 degree and the value of mensuration as sloping shaft.Just, the phase difference value R in the use face 0, the axle that will lag behind is as the sloping shaft phase difference value R that 40 degree measure that tilt 40, the thickness of film and the mean refractive index n of film 0, utilize following formula (4)～(6) to carry out numerical evaluation and obtain n x, n yAnd n z,, can calculate the phase difference value R of the thickness direction of through type (7) definition with they substitution formulas (7) Th
R th＝[(n x+n y)/2-n z]×d (7)
R 0＝(n x-n y)×d (4)
R 40＝(n x-n y’)×d/cos(φ)?(5)
(n x+n y+n z)/3＝n 0 (6)
Here,
φ＝sin -1〔sin(40°)/n 0〕
n y’＝n y×n z/〔n y 2×sin 2(φ)+n z 2×cos 2(φ)〕 1/2
The thickness direction phase difference value R of polarizer (2) ThIt is desirable to according to the characteristic of its purposes, especially liquid crystal cell suitably the scope from about 40～300nm select.This thickness direction phase difference value R ThAdvantageously more than 50nm, again advantageously below 200nm.
Then, resulting coat film heated remove organic solvent, can obtain the composite phase difference board that polarizer (1) and polarizer (2) have engaged.
Heating-up temperature is generally 0～150 ℃, it is desirable to 25～120 ℃.
Composite phase difference board of the present invention contains polarizer (1) and polarizer (2), also can contain oriented film, support base material, undercoat etc.For example, can be shown in Fig. 1 (a), Fig. 2 (a), Fig. 2 (c) and Fig. 2 (e), be that polarizer (1) and polarizer (2) engage the composite phase difference board that forms, also can shown in Fig. 1 (b), Fig. 2 (b), Fig. 2 (d) and Fig. 2 (f), between polarizer (1) and polarizer (2), undercoat 13 be set.
Can be shown in Fig. 2 (a), composite phase difference board of the present invention is that polarizer (1) and polarizer (2) engage, and engages support base material 14 on the face of the opposition side of the face that engages with polarizer (2) of polarizer (1).Can be as Fig. 2 (c) and (e), polarizer (1) and polarizer (2) engage, joint oriented film 15 on the face of the opposition side of the face that engages with polarizer (2) of polarizer (1).Can be shown in Fig. 2 (c), on the face of the opposition side of the face that engages with polarizer (1) of oriented film, engage and support base material 14.
Can be shown in Fig. 2 (b), composite phase difference board of the present invention is to form undercoat 13 between polarizer (1) and the polarizer (2), engages support base material 14 on the face of the opposition side of the face that engages with undercoat 13 of polarizer (1).Can be as Fig. 2 (d) and (f), form undercoat 13 between polarizer (1) and the polarizer (2), joint oriented film 15 on the face of the opposition side of the face that engages with undercoat 13 of polarizer (1).Can be shown in Fig. 2 (d), on the face of the opposition side of the face that engages with polarizer (1) of oriented film 15, engage and support base material 14.
Composite phase difference board shown in Fig. 2 (a)～Fig. 2 (f) can directly use, also can peel off support base material or peel off support that base material and oriented film duplicate after, re-use.
Support base material or support the method that base material and oriented film duplicate as peeling off, have for example at the support layers on substrates of thinking lamination composite phase difference board of the present invention and press adhesive layer described later, then peel off simultaneously and support base material and oriented film, perhaps only peel off the support base material, be bonded on the method for adhesive layer etc.
Composite phase difference board of the present invention can be with the numerical value that is called as the Nz coefficient, and the shape of the indicatrix of this polarizer is discussed.In addition, the Nz coefficient is calculated by following formula (8).
Nz＝(n x-n z)/(n x-n y)(8)
The Nz coefficient shows 1.1～2.0, it is desirable to 1.2～1.8 composite phase difference board is the circularly polarized light pattern, engages with the liquid crystal cell of vertical orientation (VA) pattern, is suitable for the liquid crystal panel that middle-size and small-size liquid crystal indicator is used.The Nz coefficient shows 2.0～5.0, it is desirable to 2.5～4.5 composite phase difference board is the rectilinearly polarized light pattern, engages with the liquid crystal cell of vertical orientation (VA) pattern, is suitable for the liquid crystal panel that large-scale liquid crystal indicator is used.
Owing to adjust the Nz coefficient, so can make the composite phase difference board of Nz coefficient with the thickness of the thickness of only adjusting polarizer (1) and polarizer (2) with hope for each liquid crystal panel.
Composite phase difference board of the present invention is the composite phase difference board of the remarkable thin-walled property of the polarizer of the polarizer of the positive uniaxiality of lamination and negative uniaxiality normally.Again, owing to be thin-walled, therefore by light-weighted composite phase difference board.
[undercoat]
Undercoat is formed by the primer as transparent resin usually.Defective during polarizer (2) film forming that undercoat owing to can suppress forms by coating or coating spot and ideal.Again, though the organic solvent from prevent coating liquid (2) this respect that influences of polarizer (1) is considered, it is desirable to be provided with undercoat.
It is desirable to the transparency and the good primer of cohesiveness after coating is good, especially layer forms as primer.
Primer can be dissolved in the solvent, again, in order to adjust thickness, also can be with this resin of solvent dilution.According to dissolving resin, also can use aromatic hydrocarbon solvents such as benzene,toluene,xylene; The ketone solvent of acetone, methyl ethyl ketone, hexone etc.; Ester solvent such as ethyl acetate, isobutyl acetate; The chlorinated hydrocarbon solvent of methylene chloride, triclene, chloroform etc.; The general organic solvents such as alcoholic solvent of ethanol, 1-propyl alcohol, 2-propyl alcohol, 1-butanols etc., but owing to use the solution that contains organic solvent to form the words of undercoat, sometimes influence the optical characteristics of polarizer (1), so it is desirable to use solvent to form undercoat as the solution of water.
Suitable example as primer can have epoxy resin for example.Epoxy resin can use the single component curing type, also can use the bi-component curing type.It is desirable to water miscible epoxy resin especially.Water miscible epoxy resin has the daiamid epoxy resin that polyamide polyamine and chloropropylene oxide reaction are obtained for example, and this polyamide polyamine is obtained by diethylene triamine or such polyalkylene polyamine and the such dicarboxylic acid reaction of hexane diacid of trien.The commercially available product of described daiamid epoxy resin has for example firmly changes " ス ミ レ one ズ レ ジ Application (registered trademark) 650 (30) " or the ス ミ レ one ズ レ ジ Application (registered trademark) 675 that ケ system テ ッ Network ス Co., Ltd. sells " (registered trademark) etc.
When using water miscible epoxy resin as primer, in order further to improve coating, it is desirable to polyvinyl alcohol resin etc. other water soluble resin and use.Polyvinyl alcohol resin can be partly-hydrolysed polyvinyl alcohol (PVA), fully saponified polyvinyl alcohol (PVA), carboxy-modified polyvinyl alcohol (PVA), acetoacetyl modified polyvinylalcohol, methylol modified polyvinylalcohol, amino modified polyvinyl alcohol (PVA) such be resin through modified polyethylene alcohol.The commercially available product of suitable polyvinyl alcohol resin has the polyvinyl alcohol (PVA) that contains the anionic property base " KL-318 " (trade name) of the Network ラ レ of Co., Ltd. sale etc. for example.
When forming undercoat by the solution that contains water miscible epoxy resin, it is desirable to epoxy resin is scope about 0.2～1.5 weight portion with respect to 100 weight parts waters.Again, when this solution mixing pva was resin, it is desirable to this amount was about 1～6 weight portion with respect to 100 weight parts waters.It is desirable to, the thickness of undercoat is the scope about 0.1～10 μ m.
For the formation method of undercoat without limits, can use direct intagliotype, reverse known various cladding processes such as intagliotype (リ バ one ス グ ラ PVC ァ), metal mold rubbing method (ダ ィ コ one ト), comma coating (カ Application マ コ one ト) method, bar type rubbing method.
[(vi) go up the operation that forms undercoat at polarizer (1)]
For example, can carry out drying, obtain undercoat by going up the solution that coating is dissolved in the primer in water or the organic solvent at polarizer (1).Baking temperature is generally 0～150 ℃, it is desirable to 25～120 ℃.
[(vii) on undercoat, form the operation of polarizer (2)]
Can make it dry by on resulting undercoat, being coated with coating liquid (2), can obtain composite phase difference board.
[polarized light member]
Polarized light member of the present invention contains composite phase difference board of the present invention and polarization plate.The polarized light member carries out lamination by the order of composite phase difference board, adhesive layer and polarization plate usually, and its concrete example has the polarized light member shown in Fig. 3 (a)～(f) for example.
The polarized light member of Fig. 3 (a) is the polarized light member that carries out lamination by the order of composite phase difference board, adhesive layer and the polarization plate of Fig. 1 (a).The polarized light member of Fig. 3 (b) is the polarized light member that carries out lamination by the order of composite phase difference board, adhesive layer and the polarization plate of Fig. 1 (b).The polarized light member of Fig. 3 (c) is the polarized light member that carries out lamination by the order of composite phase difference board, adhesive layer and the polarization plate of Fig. 2 (e).The polarized light member of Fig. 3 (d) is the polarized light member that carries out lamination by the order of composite phase difference board, adhesive layer and the polarization plate of Fig. 2 (f).The polarized light member of Fig. 3 (e) is the polarized light member that carries out lamination by the order of composite phase difference board, adhesive layer and the polarization plate of Fig. 2 (c).The polarized light member of Fig. 3 (f) is the polarized light member that carries out lamination by the order of composite phase difference board, adhesive layer and the polarization plate of Fig. 2 (d).
Polarization plate gets final product and be absorbed in the member that the direction of at right angles intersecting with above-mentioned direction in the face has the rectilinearly polarized light of vibration plane so long as the rectilinearly polarized light that makes a direction in face have vibration plane sees through.For example, have for example have make polyvinyl alcohol (PVA) mesentery absorption iodine or dichroism pigment extend the polariscope that obtains film, have the polyvinyl alcohol (PVA) mesentery extended and makes the film etc. of the polariscope of iodine or the absorption of dichroism pigment.Again, such polariscope can utilize as polarization plate separately, but it is desirable to, and can use the polariscope behind the stickup of one side (one or both sides) at least diaphragm of polariscope.It is resin etc. as the cyclic polyolefin of the rare such polycycle ring-type alkene of norborneol that this diaphragm can use the so cellulose-based resin of tri acetyl cellulose or monomer.
The employed cementing agent of adhesive layer can be made of the material that with acrylic acid series polymeric compounds, polysiloxane based polymer, polyester, polyurethane, polyethers etc. is base polymer.Especially, it is desirable to select the cementing agent as the acrylic acid series cementing agent to use, this cementing agent optical transparence is good, the wettability or the cohesiveness that keep appropriateness, also good with the cohesiveness of base material, and have against weather or thermotolerance etc., the problem of peeling off that under the heating or the condition of humidification, can not float or peel off etc.In the acrylic acid series cementing agent, weight-average molecular weight is useful as base polymer at the acrylic acid series copolymer more than 100,000, described weight-average molecular weight obtains like this at the acrylic acid series copolymer more than 100,000: mix acrylic acid Arrcostab of the alkyl of carbon number below 20 and by the acrylic monomer that contains functional group of formations such as (methyl) acrylic acid or (methyl) Hydroxyethyl Acrylate with methyl or ethyl, butyl etc., make glass transition temperature it is desirable to below 25 ℃, better be below 0 ℃.
[optical component]
Optical component of the present invention contains composite phase difference board of the present invention and color filter.
Particularly, for example just like the optical component shown in Fig. 5 (a), it is supporting to form color-filter layer 20 on the base material, forms polarizer (1) and polarizer (2) thereon as mentioned above successively again and obtains.Also for example just like the optical component shown in Fig. 5 (b), it is to support to form color-filter layer 20 on the base material 14, forms polarizer (1), undercoat 13 and polarizer (2) thereon as mentioned above successively again and obtains.Also for example just like the optical component shown in Fig. 5 (c), it is by supporting base material 14, color-filter layer 20, the order of oriented film 15, polarizer (1) and polarizer (2) is carried out lamination and is formed, also for example just like the optical component shown in Fig. 5 (d) etc., it is by supporting base material 14, color-filter layer 20, and the order of oriented film 15, polarizer (1), undercoat 13 and polarizer (2) is carried out lamination and formed.
Also for example just like the optical component shown in Fig. 5 (e), it is containing support base material 14, the composite phase difference board upper strata of polarizer (1) and polarizer (2) is pressed color-filter layer 20 and is constituted, also for example just like the optical component shown in Fig. 5 (f), it is by supporting base material 14, polarizer (1), undercoat 13, the order of polarizer (2) and color-filter layer 20 is carried out lamination and is constituted, also for example just like the optical component shown in Fig. 5 (g) etc., it is by supporting base material 14, oriented film 15, polarizer (1), the order of polarizer (2) and color-filter layer 20 is carried out lamination and is constituted, also for example just like the optical component shown in Fig. 5 (h) etc., it is by supporting base material 14, oriented film 15, polarizer (1), undercoat 13, the order of polarizer (2) and color-filter layer 20 is carried out lamination and is constituted.
Use optical component of the present invention, can make liquid crystal cell by general way.Again, the liquid crystal cell of use also can be made liquid crystal indicator (LCD) by general way.
The liquid crystal cell that contains optical component of the present invention, its field angle or color reproduction are enhanced.
[liquid crystal indicator]
Liquid crystal indicator of the present invention (following note do LCD) sometimes have for example the LCD that contains polarized light member of the present invention and liquid crystal cell, specifically at the LCD of the one side configuration polarized light member of liquid crystal cell, at the LCD of the two sides of liquid crystal cell configuration polarized light member.
As shown in Figure 4, polarized light member 18 and 19 common Jie of liquid crystal cell are carried out lamination by adhesive layer 16.
Can dispose polarized light member of the present invention in the one side of liquid crystal cell, being situated between at the another side of liquid crystal cell is provided with polarized light member (for example polarization plate) outside the polarized light member of the present invention by adhesive layer same as described above.Again, polarized light member of the present invention be can dispose, composite phase difference board outside composite phase difference board of the present invention, the present invention or common polarizer engaged at the another side of liquid crystal cell in the one side of liquid crystal cell.According to above-mentioned formation, the electrode by use figure does not show is applied to voltage on the liquid crystal panel, drives liquid crystal molecule, plays the effect of optical shutter (シ ャ ッ one).
Liquid crystal cell has TN (Twisted Nematic) mode, STN (Super Twisted Nematic) mode, VA (Vertical Alignmen) mode, IPS (In plane Switching) mode, ECB (ElectricallyControlled Bireviringence) mode etc. for example, it is desirable to VA mode and ECB mode, it is desirable to the VA mode especially.
Embodiment
Below, by embodiment, the present invention will be described in more detail, but the present invention is not limited to these examples.In the example, the part of expression content or use amount is a weight basis as long as there is not special record.The coating liquid (A) that uses in the following example and the composition of coating liquid (B) are as follows respectively.
[coating liquid (A)]
Mix following each composition, under 80 ℃,, be cooled to room temperature, preparation coating liquid (A) after the resulting solution stirring 1 hour.
Liquid crystal monomer: contain following formula
30 parts of the Poliocolor of shown compound (BASF AG's registered trademark) LC242
0.9 part of Photoepolymerizationinitiater initiater: ィ Le ガ キ ュ ァ 907 (manufacturing of チ バ ス ペ シ ャ リ テ ィ one ケ ミ カ Le ズ company)
0.1 part of levelling agent: BYK 361 N (manufacturing of PVC ッ Network ケ ミ one ジ ャ パ Application company)
Organic solvent: 69 parts of cyclopentanone
[coating liquid (B)]
Mix following each composition, stir after the resulting potpourri, with the filtrator filtration of aperture 1 μ m, preparation coating liquid (B).
Organic decoration clay complex: the complex of synthetic li-montmorillonite and tricaprylmethylammonium ion is " Le one セ Application ィ ト STN " (trade name) 7.2 parts that コ one プ ケ ミ カ Le Co., Ltd. makes
Adhesive resin: the solid formation branch concentration in the urethane resin of isophorone diisocyanate matrix is 30% resin varnish, promptly firmly changes " SBU ラ ッ カ 1 " (trade name) 16.0 parts that バ ィ ェ Le ゥ レ Application Co., Ltd. makes
Organic solvent: 76.8 parts of toluene
Other: 0.3 part in water
Chlorinity in " Le one セ Application ィ ト STN " (trade name) used is 1,111ppm.
Water percentage through measuring in the coating liquid (B) with Ka Er-Fei Xier moisture meter is 0.25%.Again, the weight ratio of organic decoration clay complex in the coating liquid (B) and adhesive resin is 6/4.
The Production Example of embodiment 1＜blooming 〉
Go up at glass substrate (support base material) after the 2 weight % aqueous solution of pva coating (polyvinyl alcohol (PVA) 1000 fully saponified types, Wako Pure Chemical Industries, Ltd. makes), carry out heat drying, on glass substrate, obtain the polyvinyl alcohol film of thickness 89nm.Then, milled processed is implemented on the surface of polyvinyl alcohol film, obtained the layered product of oriented film and support base material.On the face of the enforcement milled processed of resulting layered product by spin-coating method coating coating liquid (A).On 45 ℃ hot plate, will be coated with after dry 1 minute of the layered product of coating liquid (A), at room temperature shine 1200mJ/cm 2Ultraviolet ray, making layer is pressed with the layered product of polarizer (1).Then, by spin-coating method coating liquid (B) is coated on the polarizer (1).The layered product that has been coated with coating liquid (B) is carried out heat drying, obtain composite phase difference board by the order lamination of glass substrate (support base material), oriented film, polarizer (1) and polarizer (2).
The mensuration of＜optical characteristics 〉
Use mensuration machine (KOBRA-WR, prince's instrumentation machines corporation is made) to measure the incident angle dependency of the phase difference value under the wavelength of 550nm of the above-mentioned composite phase difference board that obtains.On the other hand, the incident angle dependency of the layered product of oriented film and support base material is also measured by same method.The front phase difference value of this layered product and the phase difference value that supporter inclination 40 degree mensuration are obtained all are 0nm respectively, confirm that thus this layered product does not have phase differential, the phase difference value of the composite phase difference board that obtains with the mensuration machine is that the phase differential by composite phase difference board causes.Again, peel off the polarizer (1) and the polarizer (2) of a part, only measure the thickness of the composite phase difference board that constitutes by polarizer (1) and polarizer (2) with laser microscope (LEXT, Olympus Corp make) from composite phase difference board.Measurement result, as can be known: the front phase difference value R of composite phase difference board 0Be 113nm, with the phase difference value Rs of axle that lag behind as sloping shaft inclination 40 degree mensuration 40Be 139nm, the pitch angle is 1.0 degree, and the thickness of polarizer (1) is 0.87 μ m, and the thickness of polarizer (2) is 3.87 μ m, and only the thickness of the composite phase difference board that is made of polarizer (1) and polarizer (2) is 4.82 μ m.Mean refractive index (n with polarizer 0) as 1.6, obtain n according to above-mentioned formula (4)～formula (6) x, n yAnd n z, according to following formula (8)
Nz＝(n x-n z)/(n x-n y)(8)
Calculating the Nz coefficient, is 1.74, and the result is shown in the table 1.
Embodiment 2
Except the thickness that changes polarizer (2), other carry out with embodiment 1 the samely.The result is shown in the table 1.
Embodiment 3
Going up coating daiamid epoxy resin aqueous solution i.e. " ス ミ レ one ズ レ ジ Application (registered trademark) 650 (30) " with the embodiment 1 the same polarizer that obtains (1), carry out drying, form undercoat.On resulting undercoat,, carry out heat drying, can obtain the composite phase difference board that the order lamination by glass substrate (support base material), oriented film, polarizer (1), undercoat and polarizer (2) forms by spin-coating method coating coating liquid (B).
Comparative example 1
At phase retardation film (horizontal stretching ェ ス シ one Na (norborneol is rare to be resin), phase difference value 140nm, thickness 40 μ m, the manufacturing of ponding chemistry) goes up pva coating (polyvinyl alcohol (PVA) 1000 fully saponified types, Wako Pure Chemical Industries, Ltd.'s manufacturing) after the 2 weight % aqueous solution, carry out heat drying, on phase retardation film, obtain the polyvinyl alcohol film of thickness 79nm.Then, after the surface enforcement milled processed to polyvinyl alcohol film, this film is bonded on the glass substrate (support base material) with cementing agent.Then, implementing on the face of milled processed by spin-coating method coating coating liquid (B), carry out heat drying, can obtain the composite phase difference board that the order lamination by glass substrate (support base material), adhesive layer, phase retardation film, oriented film and polarizer (2) forms.
The mensuration of＜optical characteristics 〉
Use mensuration machine (KOBRA-WR, prince's instrumentation machines corporation is made) to measure the incident angle dependency of the above-mentioned phase difference value under the wavelength of 550nm that contains the composite phase difference board of supporting base material that obtains.
On the other hand, support the incident angle dependency of base material (glass substrate) also to measure by same method.Making the front phase difference value of supporting base material and making the phase difference value of supporting base material inclination 40 degree mensuration to obtain all is 0nm respectively, confirm to support that thus base material does not have phase differential, the phase difference value that contains the composite phase difference board of supporting base material that obtains with the mensuration machine be with by an identical value of phase differential by the composite phase difference board of phase retardation film, oriented film and polarizer (2) formation.
The front phase difference value R of composite phase difference board as can be known 0Be 139nm, with the phase difference value Rs of axle that lag behind as sloping shaft inclination 40 degree mensuration 40Be 170nm, the pitch angle is 0.6 degree, and the thickness of polarizer (2) is 2.27 μ m, and the thickness of whole composite phase difference board is 42.35 μ m.
Mean refractive index (n with phase retardation film 0) as 1.6, calculate with embodiment 1, the Nz coefficient is 1.71 as can be known. the samelyThe result is shown in the table 1.
Comparative example 2
Except the thickness of polarizer (2) is the 0.64 μ m, other carry out with comparative example 1 the samely.The result is shown in the table 1.
[table 1]
Figure A20091013047800321
According to table 1, the Nz coefficient of composite phase difference board of the present invention and the optical characteristics at pitch angle demonstrate the composite phase difference board equal extent good optical characteristics with comparative example, and the little one digit number of while thickness is by thin-walled property.
Utilizability on the industry
Composite phase difference board of the present invention uses filming to be easy to be obtained by the liquid-crystal compounds polymerization with polymerism base Polarizer (1), can obtain thinner composite phase difference board.

Claims (13)

1. a composite phase difference board contains polarizer (1) that obtains and the polarizer (2) that contains organic decoration clay complex and adhesive resin by the liquid-crystal compounds polymerization with polymerism base.
2. composite phase difference board as claimed in claim 1, wherein, polarizer (1) is the polarizer of positive uniaxiality.
3. composite phase difference board as claimed in claim 1 or 2, wherein, polarizer (2) is the polarizer of negative uniaxiality.
4. composite phase difference board as claimed in claim 1, wherein, organic decoration clay complex contains quaternary ammonium salt and belongs to the clay mineral of smectite family, the atomic ratio (Mg/Si of magnesium that these mineral are contained and 4 atom silicon 4) less than 2.73.
5. composite phase difference board as claimed in claim 1, wherein, the liquid-crystal compounds with polymerism base is the liquid-crystal compounds with polymerism base of formula (D-1)～(D-5) expression, in the formula, R 1～R 5Alkyl or the hydrogen atom of representing carbon number 1～4 respectively independently.
Figure A2009101304780002C1
6. composite phase difference board as claimed in claim 1, wherein, polarizer (1) engages with polarizer (2) and forms.
7. composite phase difference board as claimed in claim 1 wherein, also contains undercoat, and this undercoat is arranged between polarizer (1) and the polarizer (2).
8. composite phase difference board as claimed in claim 1, wherein, the light that sees through composite phase difference board is at the front of wavelength 550nm phase difference value R 0(550) be 113～163nm.
9. a polarized light member is characterized in that, contains each described composite phase difference board and polarization plate in the claim 1～8.
10. a liquid crystal indicator is characterized in that, contains described polarized light member of claim 9 and liquid crystal cell.
11. an optical component is characterized in that, contains each described composite phase difference board and color filter in the claim 1～8.
12. the manufacture method of a composite phase difference board is characterized in that, have following (i)～(operation v):
(i) mixing has the operation of the liquid-crystal compounds and the organic solvent of polymerism base;
(ii) the solution that is obtained by operation (i) obtains the operation of coat film;
(iii) make contained liquid-crystal compounds polymerization in the coat film that operation obtains in (ii) and obtain the operation of polarizer (1) with polymerism base;
The operation of (iv) mixing organic decoration clay complex, adhesive resin and organic solvent;
(v) will be coated on the operation that resulting polarizer (1) upward obtains composite phase difference board at the coating liquid that operation (iv) obtains.
13. the manufacture method of a composite phase difference board is characterized in that, have following (i)～(iv) reach (vi)～(operation vii):
(i) mixing has the operation of the liquid-crystal compounds and the organic solvent of polymerism base;
(ii) the solution that is obtained by operation (i) obtains the operation of coat film;
(iii) make contained liquid-crystal compounds polymerization in the coat film that operation obtains in (ii) and obtain the operation of polarizer (1) with polymerism base;
The operation of (iv) mixing organic decoration clay complex, adhesive resin and organic solvent;
(vi) go up the operation that is coated with primer and goes up the formation undercoat at polarizer (1) at resulting polarizer (1);
(vii) will be coated on the undercoat and obtain the operation of composite phase difference board at the coating liquid that operation obtains in (iv).
CNA2009101304785A 2008-04-17 2009-04-15 Composite phase difference board and manufacturing method thereof Pending CN101561526A (en)

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Application publication date: 20091021