TW200914150A - Process for producing laminate - Google Patents
Process for producing laminate Download PDFInfo
- Publication number
- TW200914150A TW200914150A TW97131014A TW97131014A TW200914150A TW 200914150 A TW200914150 A TW 200914150A TW 97131014 A TW97131014 A TW 97131014A TW 97131014 A TW97131014 A TW 97131014A TW 200914150 A TW200914150 A TW 200914150A
- Authority
- TW
- Taiwan
- Prior art keywords
- coating liquid
- coating
- film
- substrate
- liquid crystal
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 15
- 238000000576 coating method Methods 0.000 claims abstract description 154
- 239000011248 coating agent Substances 0.000 claims abstract description 149
- 239000007788 liquid Substances 0.000 claims abstract description 104
- 150000001875 compounds Chemical class 0.000 claims abstract description 47
- 239000000758 substrate Substances 0.000 claims abstract description 42
- 239000004976 Lyotropic liquid crystal Substances 0.000 claims abstract description 32
- 230000009974 thixotropic effect Effects 0.000 claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 claims description 30
- 239000011347 resin Substances 0.000 claims description 20
- 229920005989 resin Polymers 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 17
- 239000011521 glass Substances 0.000 claims description 11
- -1 known Polymers 0.000 claims description 9
- 239000007787 solid Substances 0.000 claims description 8
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000010008 shearing Methods 0.000 claims description 5
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
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- 239000004431 polycarbonate resin Substances 0.000 claims description 3
- 229920005672 polyolefin resin Polymers 0.000 claims description 3
- AFFLGGQVNFXPEV-UHFFFAOYSA-N 1-decene Chemical group CCCCCCCCC=C AFFLGGQVNFXPEV-UHFFFAOYSA-N 0.000 claims description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 2
- 239000012461 cellulose resin Substances 0.000 claims description 2
- 229920001225 polyester resin Polymers 0.000 claims description 2
- 239000004645 polyester resin Substances 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- LDJNYVFOXUBIIF-UHFFFAOYSA-N 1-prop-1-enyl-9H-fluorene Chemical group C(=CC)C1=CC=CC=2C3=CC=CC=C3CC12 LDJNYVFOXUBIIF-UHFFFAOYSA-N 0.000 claims 1
- 239000004973 liquid crystal related substance Substances 0.000 abstract description 21
- 238000002834 transmittance Methods 0.000 abstract description 16
- 230000003287 optical effect Effects 0.000 description 22
- 239000000975 dye Substances 0.000 description 19
- 239000012071 phase Substances 0.000 description 17
- 239000000049 pigment Substances 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 14
- 239000000243 solution Substances 0.000 description 8
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 7
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- 239000004988 Nematic liquid crystal Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
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- 239000010410 layer Substances 0.000 description 5
- 125000001424 substituent group Chemical group 0.000 description 5
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007789 gas Chemical group 0.000 description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 229920002678 cellulose Polymers 0.000 description 3
- 239000001913 cellulose Substances 0.000 description 3
- 239000003086 colorant Substances 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- UHOKSCJSTAHBSO-UHFFFAOYSA-N indanthrone blue Chemical compound C1=CC=C2C(=O)C3=CC=C4NC5=C6C(=O)C7=CC=CC=C7C(=O)C6=CC=C5NC4=C3C(=O)C2=C1 UHOKSCJSTAHBSO-UHFFFAOYSA-N 0.000 description 3
- 239000000463 material Substances 0.000 description 3
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- 150000003839 salts Chemical class 0.000 description 3
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- 239000004094 surface-active agent Substances 0.000 description 3
- 239000002562 thickening agent Substances 0.000 description 3
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 description 2
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- UFWIBTONFRDIAS-UHFFFAOYSA-N Naphthalene Chemical compound C1=CC=CC2=CC=CC=C21 UFWIBTONFRDIAS-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 125000003545 alkoxy group Chemical group 0.000 description 2
- MWPLVEDNUUSJAV-LSMJWXKXSA-N anthracene Chemical group [13CH]1=[13CH][13CH]=[13CH][13C]2=CC3=CC=CC=C3C=[13C]21 MWPLVEDNUUSJAV-LSMJWXKXSA-N 0.000 description 2
- 239000001000 anthraquinone dye Substances 0.000 description 2
- 239000000987 azo dye Substances 0.000 description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 description 2
- 239000012965 benzophenone Substances 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- VLARUOGDXDTHEH-UHFFFAOYSA-L disodium cromoglycate Chemical compound [Na+].[Na+].O1C(C([O-])=O)=CC(=O)C2=C1C=CC=C2OCC(O)COC1=CC=CC2=C1C(=O)C=C(C([O-])=O)O2 VLARUOGDXDTHEH-UHFFFAOYSA-L 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 235000019239 indanthrene blue RS Nutrition 0.000 description 2
- 229910052747 lanthanoid Inorganic materials 0.000 description 2
- 150000002602 lanthanoids Chemical class 0.000 description 2
- 229910052744 lithium Inorganic materials 0.000 description 2
- 230000002535 lyotropic effect Effects 0.000 description 2
- 238000000691 measurement method Methods 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical compound N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 229920001721 polyimide Polymers 0.000 description 2
- 229920006254 polymer film Polymers 0.000 description 2
- 229910052700 potassium Inorganic materials 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- QGKMIGUHVLGJBR-UHFFFAOYSA-M (4z)-1-(3-methylbutyl)-4-[[1-(3-methylbutyl)quinolin-1-ium-4-yl]methylidene]quinoline;iodide Chemical compound [I-].C12=CC=CC=C2N(CCC(C)C)C=CC1=CC1=CC=[N+](CCC(C)C)C2=CC=CC=C12 QGKMIGUHVLGJBR-UHFFFAOYSA-M 0.000 description 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 1
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- WLDHEUZGFKACJH-ZRUFZDNISA-K Amaranth Chemical compound [Na+].[Na+].[Na+].C12=CC=C(S([O-])(=O)=O)C=C2C=C(S([O-])(=O)=O)C(O)=C1\N=N\C1=CC=C(S([O-])(=O)=O)C2=CC=CC=C12 WLDHEUZGFKACJH-ZRUFZDNISA-K 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 108010068370 Glutens Proteins 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000004642 Polyimide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000004990 Smectic liquid crystal Substances 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- 240000006394 Sorghum bicolor Species 0.000 description 1
- 235000011684 Sorghum saccharatum Nutrition 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000006096 absorbing agent Substances 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 239000002535 acidifier Substances 0.000 description 1
- 239000000999 acridine dye Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
- 235000012735 amaranth Nutrition 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 125000006267 biphenyl group Chemical group 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 125000002843 carboxylic acid group Chemical group 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 229960000265 cromoglicic acid Drugs 0.000 description 1
- 210000002858 crystal cell Anatomy 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- SUXCALIDMIIJCK-UHFFFAOYSA-L disodium;4-amino-3-[[4-[4-[(1-amino-4-sulfonatonaphthalen-2-yl)diazenyl]-3-methylphenyl]-2-methylphenyl]diazenyl]naphthalene-1-sulfonate Chemical compound [Na+].[Na+].C1=CC=CC2=C(N)C(N=NC3=CC=C(C=C3C)C=3C=C(C(=CC=3)N=NC=3C(=C4C=CC=CC4=C(C=3)S([O-])(=O)=O)N)C)=CC(S([O-])(=O)=O)=C21 SUXCALIDMIIJCK-UHFFFAOYSA-L 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 125000001301 ethoxy group Chemical group [H]C([H])([H])C([H])([H])O* 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 125000003983 fluorenyl group Chemical group C1(=CC=CC=2C3=CC=CC=C3CC12)* 0.000 description 1
- 235000021312 gluten Nutrition 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 description 1
- COHYTHOBJLSHDF-BUHFOSPRSA-N indigo dye Chemical compound N\1C2=CC=CC=C2C(=O)C/1=C1/C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-BUHFOSPRSA-N 0.000 description 1
- COHYTHOBJLSHDF-UHFFFAOYSA-N indigo powder Natural products N1C2=CC=CC=C2C(=O)C1=C1C(=O)C2=CC=CC=C2N1 COHYTHOBJLSHDF-UHFFFAOYSA-N 0.000 description 1
- 230000009878 intermolecular interaction Effects 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 239000011630 iodine Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 210000003127 knee Anatomy 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- DZVCFNFOPIZQKX-LTHRDKTGSA-M merocyanine Chemical compound [Na+].O=C1N(CCCC)C(=O)N(CCCC)C(=O)C1=C\C=C\C=C/1N(CCCS([O-])(=O)=O)C2=CC=CC=C2O\1 DZVCFNFOPIZQKX-LTHRDKTGSA-M 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 125000000896 monocarboxylic acid group Chemical group 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000001005 nitro dye Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001006 nitroso dye Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 125000000962 organic group Chemical group 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920001690 polydopamine Polymers 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000001008 quinone-imine dye Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 125000000020 sulfo group Chemical group O=S(=O)([*])O[H] 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- 239000001017 thiazole dye Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- SWGJCIMEBVHMTA-UHFFFAOYSA-K trisodium;6-oxido-4-sulfo-5-[(4-sulfonatonaphthalen-1-yl)diazenyl]naphthalene-2-sulfonate Chemical compound [Na+].[Na+].[Na+].C1=CC=C2C(N=NC3=C4C(=CC(=CC4=CC=C3O)S([O-])(=O)=O)S([O-])(=O)=O)=CC=C(S([O-])(=O)=O)C2=C1 SWGJCIMEBVHMTA-UHFFFAOYSA-K 0.000 description 1
- 239000003021 water soluble solvent Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/133528—Polarisers
-
- G—PHYSICS
- G02—OPTICS
- G02F—OPTICAL DEVICES OR ARRANGEMENTS FOR THE CONTROL OF LIGHT BY MODIFICATION OF THE OPTICAL PROPERTIES OF THE MEDIA OF THE ELEMENTS INVOLVED THEREIN; NON-LINEAR OPTICS; FREQUENCY-CHANGING OF LIGHT; OPTICAL LOGIC ELEMENTS; OPTICAL ANALOGUE/DIGITAL CONVERTERS
- G02F1/00—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics
- G02F1/01—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour
- G02F1/13—Devices or arrangements for the control of the intensity, colour, phase, polarisation or direction of light arriving from an independent light source, e.g. switching, gating or modulating; Non-linear optics for the control of the intensity, phase, polarisation or colour based on liquid crystals, e.g. single liquid crystal display cells
- G02F1/133—Constructional arrangements; Operation of liquid crystal cells; Circuit arrangements
- G02F1/1333—Constructional arrangements; Manufacturing methods
- G02F1/1335—Structural association of cells with optical devices, e.g. polarisers or reflectors
- G02F1/13363—Birefringent elements, e.g. for optical compensation
Landscapes
- Physics & Mathematics (AREA)
- Nonlinear Science (AREA)
- Mathematical Physics (AREA)
- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Polarising Elements (AREA)
- Laminated Bodies (AREA)
- Liquid Crystal (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
Abstract
Description
200914150 九、發明說明： 【發明所屬之技術領域】 本發明係關於一種用作偏光膜或相位差膜之具有光學各 向異性之積層體之製造方法。 【先前技術】BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a laminated body having optical anisotropy which is used as a polarizing film or a retardation film. [Prior Art]
於液晶顯示器中’為控制通過液晶之光線之旋光性或雙 折射性而使用偏光板或相位差板。另外，於有機EL (Electrolumineseenee，電致發光）顯示器中，為防止外光 之反射而使用圓偏光板。 先前，該等偏光板中廣泛使用以如下方式獲得之偏光元 件.使碘或二色性有機色素溶解或吸附於聚乙烯醇等之高 分子膜，且藉由向一個方向延伸該膜而使色素等之分子配 向（延伸法）。但藉由延伸法所製造之偏光元件會產生由於 所使用之色素或高分子材料而对熱性或财光性+充分之問 題另外亦產生於製造顯示面板時臈之貼合之良率較低之 問題。進而隨著顯示面板之大型化而需要延伸寬幅之膜， 因此亦產生製膜裝置大型化之問題。 子 已去有如下方法（塗布法）（專利文獻j ):將呈液晶 相之含有—色性色素之塗布液於玻璃板或高分子膜等基板 上邊％加剪切應力—邊進行塗布，藉由剪切應力使塗膜 内之二色性色素配向而製作偏光膜(光學各向異性膜卜相 較於延伸法，塗布法可製造薄且耐熱性優異之偏光板，故 =注：。現今眾所周知歧，若使用於塗布液中由於溶 里夜a曰相之類之分子間相互作用而形成色素聚集體者來 133511.doc 200914150 作為二色性色素’則可獲得光學各向異性良好之偏光板。 但溶致型液晶化合物之塗布液一般黏度較高。因此若將 塗布液較薄地塗布，則存在易產生條紋狀之塗布不均之問 題。若稀釋塗布液而降低黏度，雖可避免塗布不均，但溶 劑之揮發量變多’故會產生如下問題：產生揮發不均而容 易於塗膜之表面產生微小之凹凸。進而因存在經稀釋之塗 布液超出呈液晶相之濃度範圍之情形，故亦產生難以藉由 剪切應力而使溶致型液晶化合物配向之問題。 [專利文獻]曰本專利特開2007-61755號公報 【發明内容】 [發明所欲解決之問題] 本發明之目的在於提供一種可穩定地製造積層體之製造 方法’該積層體具有無揮發不均及塗布不均、透射率偏差 較小（5%以下）、二色比較高（2〇以上）之光學各向異性膜。 [解決問題之技術手段] 本發明者等人為解決先前技術之問題而進行努力研究， 結果發現藉由使用具有於剪切速率較大時黏度變小之性質 (觸變性）之塗布液，可獲得均勻且配向度較高之光學各向 異性膜。即’若為觸變性較大之塗布液，則於基板上塗布 時施加較大之剪切速率而減小塗布液之黏度，可防止塗布 不句°亥方法並非過度稀釋塗布液而減小黏度，故亦難以 產生揮發不均。進而因塗布液處於呈液晶相之濃度範圍， 故可藉由剪切應力而使塗布液中之溶致型液晶化合物配 向。 133511.doc 200914150 本發明之主旨如下所述。 (1) 本發明之積層體之製造方法，其特徵在於：其係製 造具有基板與形成、積層於上述基板上之光學各向異性臈 的積層體者，其包括如下步驟：將塗布液於23C>c、剪切迷 率1 00私時之黏度設為V1GG (23 °c )，將塗布液於23。(：、剪 切速率1〇〇〇秒-丨時之黏度設為Vi_ (以艽），且將v⑽ °c)與v瞻（2rc)之比：v⑽（23〇c)/Vi_ (23。〇設為觸變 指數Ti時，將含有溶致型液晶化合物與溶劑、且上述觸變 指數Τι為1.2以上之上述塗布液塗布於上述基板上，於塗布 時對上述塗布液施加剪切應力而使上述溶致型液晶化合物 配向，於上述基板上形成、積層光學各向異性膜。 (2) 本發明之積層體之製造方法，其特徵在於··其係製 造具有基板與形成、積層於上述基板上之光學各向異性膜 的積層體者，其包括如下步驟：將塗布液於23t、剪切速 率100秒時之黏度設為V1GQ (23°c )，將塗布液於23°c、剪 切速率1000秒·〗時之黏度設為V刚。（23。〇，且將V_ (23 〇crnv_ (23。〇之比：V⑽（2；rc)/v_ (23t)設為觸變 才曰數Τι時’將含有溶致型液晶化合物與溶劑、且上述觸變 才曰數Τι為1.2以上之上述塗布液塗布於上述基板上，於塗布 後對包含上述塗布液之塗膜施加剪切應力而使上述溶致型 液晶化合物配向’於上述基板上形成、積層光學各向異性 臈。 (3) 本發明之積層體之製造方法，其特徵在於··上述塗 布液於23。(：、剪切速率1000秒-丨時之黏度Vi(K)() I33511.doc 200914150 mPa’s〜200 mpa，s。再者「mpa.s」為黏度之單位「毫米帕 斯卡秒」。 (4) 本發明之積層體之製造方法，其特徵在於：上述塗 布液之 V⑽（23。〇與 V]_ (23。〇之差：{v 丨。。（23τ)·ν】〇〇〇 (23 C )}為 1〇 mPa.s以上。 (5) 本發明之積層體之製造方法，其特徵在於：於塗布 上述塗布液後，進一步包括加熱乾燥上述塗膜之步驟。 (6) 本發明之積層體之製造方法，其特徵在於：於上述 加熱乾燥之情形之乾燥溫度為”它〜丨2〇。匚。 (7) 本發明之積層體之製造方法，其特徵在於：上述塗 布液之全固形物濃度為丨2重量〇重量％。 (8) 本發明之積層體之製造方法，其特徵在於：乾燥後 之上述塗膜、即光學各向異性膜之厚度為〇 〇5 μπι〜5 。 (9) 本發明之積層體之製造方法，其特徵在於：上述光 學各向異性膜之二色比於波長550 nm時為20以上。 (1〇)本發明之積層體之製造方法，其特徵在於：上述積 層體之厚度為5 μπι〜500 μΐΏ。 ⑴）本發明之積層體之製造方法，其特徵在於：上述基 板^含無驗玻璃板，或者苯乙稀系樹脂、（甲基）丙烯酸系 樹月曰聚自曰系樹脂、聚烯烴系樹脂、降褚烯系樹脂、聚醯 胺系樹月曰，纖維素系樹脂、聚乙稀醇系樹脂、聚碳酸醋 系樹脂中之任一樹脂臈。 [發明之效果] 本發月提供-種以簡易之操作可穩定地製造積層體之製 133511 ,d〇c 200914150 造方法’該積層體具有無揮發不均及塗布不均、透射率偏 差較小（5%以下）、二色比較高（20以上）之光學各向異性 膜。 【實施方式】 [本發明之製造方法] 本發明之積層體之製造方法，其特徵在於：其係具有基 板與包含形成、積層於基板上之塗膜的光學各向異性膜之 積層體之製造方法，其包括如下步驟：將含有溶致型液晶 化合物與溶劑、且觸變指數Ti為1.2以上之塗布液塗布於基 板上，對塗布時之塗布液或塗布後之塗膜施加剪切應力而 使溶致型液晶化合物配向，於基板上形成.積層光學各向 異性膜。將觸變指數Ti定義為於23t：、剪切速率1〇〇秒時 之黏度(23 °C )與於23 °C、剪切速率1〇〇〇秒-1時之黏度 V10〇〇 (23°c)之比：Ti=v1()() (23。〇。 圖1中針對（a)本發明之塗布液與（b)先前之塗布液，示意 性地表示剪切速率（橫軸）與黏度（縱軸）之關係之圖。縱轴 之黏度為任意刻度。另外塗布液之溫度為23 °C。剪切速率 ΙΟΟί^}、·1之黏度為塗布時之黏度之標準，剪切速率1〇〇秒·! 之黏度為乾燥時之黏度之標準。本發明之塗布液（a)具有觸 變性，故剪切速率越大黏度越小。因此於本發明之塗布液 中Vioo (23°C)>V1000 (23°C) ’且觸變指數Ti大於1。相對於 此’先前之塗布液（b)即使剪切速率發生變化黏度亦基本不 變化，故不具有觸變性，且觸變指數Ti大致為1.0。 本發明之積層體之製造方法除上述步驟以外，亦可包括 133511.doc 10- 200914150 任意步驟。較好的是於將塗布液塗布後進一步包括加熱乾 燥塗膜之步驟。 本發明之光學各向異性膜係於層内正交之2個方向上於 吸收率、折射率等光學性質中具有各向異性之膜，且具有 作為直線偏光膜、圓偏光臈、相位差膜之功能。因此本發 明之積層體較好的是用於偏光膜、相位差膜。 [塗布液之液體物性] 本發明所使用之塗布液具有觸變性。觸變性可藉由觸變 指數丁!定量地進行評價。觸變指數丁冰大觸變性越大，觸 變指數Ti越接近i觸變性越小，而牛頓流動性越大。 本發明所使用之塗布液之觸變指數丁丨為12以上，較好的 疋1.2〜4.0 ’更好的是12〜3 〇。於塗布液之觸變指數乃未滿 之情形’即使施加剪切應力’塗布液之黏度亦不太會 變小’故容易產生塗布不均，若為了防止塗布不均而稀釋 塗布液’使黏度減小’則容易產生揮發不均。反之若觸變 指數Ti超過4.0,則存在乾燥時之塗布液之流動性過於變低 而無法獲得目標厚度之均勻塗膜之情形。 本發明所使用之塗布液之觸變指數Ti，例如可藉由改變 二t液中之溶致型液晶化合物之濃度、導入溶致型液晶化 合物之取代基之種類、溶劑之種餚， +…β 劑之種類而使其適當增加或減 ;數==溶致型液晶化合物之分子量而使觸變 =Tl增加。或者亦可藉由添加聚丙稀酸或纖維素類之化 合物而使觸變指數Ti增加。另一方面 中使用醇類、W酮類等不…| 7藉由於溶劑 類等不良溶劑而使觸變指數Ti減 133511.doc 200914150 少。或者亦可使用市場上出售之黏度計（例如HAAKE公司 製造之Rhe〇Stress600)測定觸變指數Ti，而自多種塗布液 中適當選擇具有特定之觸變指數Ti之塗布液。 本發明所使用之塗布液於23艽、剪切速率…⑽秒·〗時之 黏度(23°C )較好的是1〇 mPa.s〜200 mPa.s，更好的是 20 mPa.s〜150 mPa.s ’ 尤其好的是 1〇〇 mPa.s〜15〇 mpa s。 於塗布液之黏度V⑽〇 (23°C )未滿10 mPa.s之情形，塗布液 之流動性過高，故存在無法獲得目標厚度之塗膜之情形。 另一方面，於塗布液之黏度Vl刪（23。〇超過2〇〇爪〜巧之 情形，塗布液之流動性過低’故存在產生條紋狀之塗布不 均之情形。若塗布液之黏度V|_ (23。〇為1〇 mpas〜2〇〇 mPa.s之範圍，則施加對於溶致型液晶化合物配向適度之 剪切應力’且可獲得均勻之目標厚度之塗膜。 本發明所使用之塗布液之Vl(H) (23。〇與Vi(K)〇 (23。〇之 差· {V丨〇〇 (23 c )-V10。。（23°C )}較好的是 1〇 mpa.s以上，更 好的是20 mPa.s〜200 mpa.s。若為{v⑽（2；rc )·%_ C )}為20 mPa.s〜200 mPa.s之塗布液，則可同時防止塗布 不均與揮發不均兩方面。 本發明所使用之塗布液之全固形物濃度無特別限制，較 好的是12重量❶/。〜50重量％，更好的是12重量％〜3〇重量 若全固形物濃度為上述範圍，則可獲得難產生揮發不均、 且呈穩疋之液晶相之塗布液。 [塗布液之組成] 本發明所使用之塗布液含有溶致型液晶化合物與溶劑。 I33511.doc -12- 200914150 另外塗布液可含有任意之添加劑。作為添加劑，例如可列 舉：界面活性劑、均化劑、抗氧化劑、黏合樹脂、單體： 硬化劑、塑化劑、熱穩定劑、光較劑、潤滑劑、抗酸化 劑、紫外線吸收劑、著色劑、阻燃劑、抗靜電劑、相容 劑、增稠劑、偶合劑等。添加劑之調配量相對於溶致型： 晶化合物100重量份’適當的是〇重量 + 仞以上5重量份以 下。若於溶液中添加界面活性劑，則可使二色性色素對美In a liquid crystal display, a polarizing plate or a phase difference plate is used to control the optical rotation or birefringence of light passing through the liquid crystal. Further, in an organic EL (Electrolumineseenee) display, a circularly polarizing plate is used to prevent reflection of external light. In the polarizing plate, a polarizing element obtained by dissolving or adsorbing iodine or a dichroic organic dye in a polymer film such as polyvinyl alcohol, and a pigment by extending the film in one direction is widely used. Molecular alignment (extension method). However, the polarizing element manufactured by the stretching method causes a problem of sufficient heat or richness due to the dye or polymer material used, and also causes a low yield of the bonding when manufacturing the display panel. problem. Further, as the size of the display panel is increased, it is necessary to extend the wide film, which also causes a problem of an increase in the size of the film forming apparatus. The following method (coating method) has been used (Patent Document j): a coating liquid containing a coloring pigment in a liquid crystal phase is applied to a substrate such as a glass plate or a polymer film with a % shear stress. The polarizing film is prepared by aligning the dichroic dye in the coating film by shear stress (the optically anisotropic film is thinner than the stretching method, and the coating method can produce a polarizing plate which is thin and excellent in heat resistance, so that: It is well known that if it is used in a coating liquid to form a pigment aggregate due to intermolecular interactions such as a lyophilized night phase, 133511.doc 200914150 as a dichroic dye, a polarized light having good optical anisotropy can be obtained. However, the coating liquid of the lyotropic liquid crystal compound generally has a high viscosity. Therefore, if the coating liquid is applied thinly, there is a problem that coating unevenness is likely to occur in a stripe shape. If the coating liquid is diluted to lower the viscosity, coating can be avoided. It is uneven, but the amount of volatilization of the solvent is increased, so that there is a problem that uneven volatilization occurs and it is easy to cause minute irregularities on the surface of the coating film. Further, the presence of the diluted coating liquid exceeds In the case of the concentration range of the liquid crystal phase, there is a problem in that it is difficult to align the lyotropic liquid crystal compound by shear stress. [Patent Document] Japanese Patent Laid-Open Publication No. 2007-61755 [Abstract] [Invention Solution to Problem] An object of the present invention is to provide a method for producing a laminated body which can stably produce a non-volatile unevenness and uneven coating, a small variation in transmittance (less than 5%), and a relatively high two-color ( The optically anisotropic film of 2 or more. [Technical means for solving the problem] The inventors of the present invention have diligently studied to solve the problems of the prior art, and as a result, it has been found that the viscosity is reduced by using a large shear rate. A coating solution of a property (thixotropy) can obtain an optically anisotropic film having a uniform and high degree of alignment. That is, if a coating liquid having a large thixotropic property is applied, a large shear rate is applied when coating on a substrate. Reducing the viscosity of the coating liquid can prevent the coating from being over-diluted and reducing the viscosity, so that it is difficult to cause uneven volatilization. In the range of the degree, the lyotropic liquid crystal compound in the coating liquid can be aligned by the shear stress. 133511.doc 200914150 The gist of the present invention is as follows. (1) The method for producing a laminate according to the present invention is characterized in that The method of manufacturing a laminate having a substrate and an optically anisotropic flaw formed on the substrate, comprising the steps of: setting the viscosity of the coating liquid to 23 C> V1GG (23 °c), the coating liquid is at 23. (:, the shear rate is 1 sec - 丨 when the viscosity is set to Vi_ (to 艽), and v (10) ° c) and v (2rc) Ratio: v(10)(23〇c)/Vi_ (23. When 〇 is set to the thixotropic index Ti, the coating liquid containing the lyotropic liquid crystal compound and the solvent and having the thixotropic index Τι of 1.2 or more is coated on the substrate. At the time of coating, a shear stress is applied to the coating liquid to align the lyotropic liquid crystal compound, and an optically anisotropic film is formed on the substrate. (2) A method for producing a laminate according to the present invention, which is characterized in that a laminate having a substrate and an optically anisotropic film formed on the substrate is formed, and the method includes the steps of: applying a coating liquid The viscosity at 23 t and the shear rate of 100 seconds was set to V1GQ (23°c), and the viscosity of the coating liquid at 23° C. and the shear rate of 1000 sec· was set to V just. (23. 〇, and V_(23 〇crnv_ (23. 〇 ratio: V(10)(2; rc)/v_ (23t) is set to a thixotropic Τ 时ι" will contain a lyotropic liquid crystal compound and a solvent, And applying the coating liquid having a thixotropy of 1.2 or more to the substrate, applying a shear stress to the coating film containing the coating liquid after coating, and aligning the lyotropic liquid crystal compound on the substrate (3) The method for producing a laminated body according to the present invention is characterized in that the coating liquid is at 23. (:, the shear rate is 1000 sec - the viscosity at the time of 丨 Vi (K) ( In the meantime, the "mPa. (23. 〇 and V]_ (23. 〇 difference: {v 丨. (23τ)·ν] 〇〇〇 (23 C )} is 1 〇 mPa.s or more. (5) The laminated body of the present invention The manufacturing method is characterized in that after the application of the coating liquid, the step of heating and drying the coating film is further included. (6) The present invention The method for producing a laminate is characterized in that the drying temperature in the case of the above-described heat drying is "it ~ 丨 2 〇. 7. (7) The method for producing a laminate according to the present invention, characterized in that the coating liquid is (8) The method for producing a laminate according to the present invention, characterized in that the thickness of the coating film, that is, the optically anisotropic film after drying is 〇〇5 μπι 5 (9) The method for producing a laminate according to the present invention, wherein the optically anisotropic film has a dichroic ratio of 20 or more at a wavelength of 550 nm. (1) A method for producing a laminate according to the present invention. The thickness of the laminated body is 5 μm to 500 μΐΏ. (1) The method for producing a laminated body according to the present invention, characterized in that the substrate comprises a glass-free plate, or a styrene resin, (meth) The acrylic tree is polymerized from a lanthanum resin, a polyolefin resin, a decene-based resin, a polyamido-based tree, a cellulose resin, a polyvinyl alcohol resin, or a polycarbonate resin. a resin 臈. [Invention Effect] This month provides a system for producing a laminate with a simple operation. 133511, d〇c 200914150 Manufacturing method 'The laminate has non-volatile unevenness and uneven coating, and the transmittance deviation is small (5%) (Embodiment) The method for producing a laminate according to the present invention is characterized in that it has a substrate and an inclusion formation. A method for producing a laminate of an optically anisotropic film of a coating film laminated on a substrate, comprising the steps of: applying a coating liquid containing a lyotropic liquid crystal compound and a solvent and having a thixotropic index Ti of 1.2 or more on a substrate The coating liquid at the time of coating or the coating film after coating is applied with a shear stress to align the lyotropic liquid crystal compound to form a laminated optical anisotropic film on the substrate. The thixotropic index Ti is defined as the viscosity at 23 t:, the shear rate at 1 sec (23 ° C) and the viscosity at 23 ° C, shear rate 1 〇〇〇 sec -1 V10 〇〇 (23 °c) ratio: Ti = v1 () () (23. 〇. Fig. 1 for (a) the coating liquid of the present invention and (b) the previous coating liquid, schematically showing the shear rate (horizontal axis) The relationship between the viscosity and the vertical axis. The viscosity of the vertical axis is any scale. The temperature of the coating liquid is 23 ° C. The shear rate ΙΟΟί^}, the viscosity of 1 is the standard of viscosity at the time of coating, shearing The viscosity at a rate of 1 〇〇··· is the standard of the viscosity at the time of drying. The coating liquid (a) of the present invention has thixotropic properties, so the higher the shear rate, the smaller the viscosity. Therefore, Vioo (23) is used in the coating liquid of the present invention. °C)>V1000 (23°C)' and the thixotropic index Ti is greater than 1. Compared with the previous coating liquid (b), the viscosity does not change even if the shear rate changes, so there is no thixotropic property, and The thixotropy index Ti is approximately 1.0. The method for producing the laminate of the present invention may include any step of 133511.doc 10-200914150 in addition to the above steps. After coating the coating liquid, the step of heating and drying the coating film is further included. The optically anisotropic film of the present invention is an anisotropic film in optical properties such as absorbance and refractive index in two directions orthogonal to each other in the layer. Further, it has a function as a linear polarizing film, a circularly polarizing film, or a retardation film. Therefore, the laminated body of the present invention is preferably used for a polarizing film or a retardation film. [Liquid physical properties of coating liquid] Coating used in the present invention The thixotropy can be quantitatively evaluated by the thixotropic index. The larger the thixotropic index, the larger the thixotropic thixotropy, the closer the thixotropic index Ti is to i, the smaller the thixotropy, and the greater the fluidity of Newton. The coating liquid used in the present invention has a thixotropic index of 12 or more, preferably 疋1.2 to 4.0', more preferably 12 to 3 Å. The thixotropic index of the coating liquid is not full even if the shearing is applied The shear stress 'the viscosity of the coating liquid is also less likely to be small', so coating unevenness is likely to occur. If the coating liquid is diluted to prevent the coating unevenness, the viscosity is reduced, and the volatilization unevenness is likely to occur. More than 4.0, then save When the fluidity of the coating liquid at the time of drying is too low to obtain a uniform coating film of a target thickness, the thixotropic index Ti of the coating liquid used in the present invention can be changed, for example, by changing the lyotropic liquid crystal in the liquid of the second liquid. The concentration of the compound, the type of the substituent introduced into the lyotropic liquid crystal compound, the species of the solvent, and the type of the ?? agent are appropriately increased or decreased; the number = the molecular weight of the lyotropic liquid crystal compound to cause thixotropic = Tl is increased. Alternatively, the thixotropic index Ti may be increased by adding a compound of polyacrylic acid or cellulose. On the other hand, an alcohol, a ketone, or the like is used instead of | 7 by a poor solvent such as a solvent. Reduce the thixotropic index Ti by 133511.doc 200914150. Alternatively, a thixotropic index Ti may be measured using a commercially available viscometer (e.g., Rhe〇 Stress 600 manufactured by HAAKE Co., Ltd.), and a coating liquid having a specific thixotropic index Ti may be appropriately selected from a plurality of coating liquids. The viscosity of the coating liquid used in the present invention at 23 Torr, the shear rate of (10) sec. (23 ° C) is preferably 1 〇 mPa.s to 200 mPa·s, more preferably 20 mPa·s. ~150 mPa.s ' Especially good is 1〇〇mPa.s~15〇mpa s. When the viscosity of the coating liquid V (10) 〇 (23 ° C) is less than 10 mPa·s, the fluidity of the coating liquid is too high, so that the coating film of the target thickness cannot be obtained. On the other hand, in the case where the viscosity of the coating liquid is V1 (23. 〇 exceeds 2 〇〇 〜 巧 巧 , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , V|_ (23. 〇 is a range of 1 〇 mpas to 2 〇〇 mPa.s, and a suitable coating thickness is applied to the lyotropic liquid crystal compound, and a uniform target thickness of the coating film can be obtained. Vl(H) of the coating liquid used (23. 〇 and Vi(K) 〇 (23. 〇 difference · {V丨〇〇(23 c )-V10 (23 ° C )} is preferably 1 〇mpa.s or more, more preferably 20 mPa.s~200 mpa.s. If {v(10)(2; rc )·%_ C )} is a coating liquid of 20 mPa.s to 200 mPa.s, then The coating unevenness and the volatilization unevenness can be prevented at the same time. The total solid concentration of the coating liquid used in the present invention is not particularly limited, and is preferably 12% by weight/% to 50% by weight, more preferably 12% by weight. When the total solid content is in the above range, a coating liquid having a liquid crystal phase which is less likely to cause volatilization and which is stable can be obtained. [Composition of Coating Liquid] The coating liquid used in the present invention contains The liquid crystal compound and the solvent are used. I33511.doc -12- 200914150 The coating liquid may contain any additives. Examples of the additive include a surfactant, a leveling agent, an antioxidant, a binder resin, and a monomer: a hardener. Plasticizer, heat stabilizer, light comparator, lubricant, acidifier, UV absorber, colorant, flame retardant, antistatic agent, compatibilizer, thickener, coupling agent, etc. Relative to the lyotropic type: 100 parts by weight of the crystalline compound is suitably 〇 weight + 仞 or more and 5 parts by weight or less. If a surfactant is added to the solution, the dichroic pigment can be made beautiful.
板表面之濡濕性、塗布性提高。作為界面活性劑較好的： 非離子界面活性劑。 [溶致型液晶化合物] 本發明所使用之溶致型液晶性化合物係指具有藉由改變 溫度或濃度而引起各向同性相-液晶相之相轉移的性質之 液晶化合物。塗布液藉由該溶致型液晶化合物之作用而呈 液晶相。呈現之液晶相無特別限制，可列舉向列型液晶 相、層列型液晶相'膽固醇型液晶相等。較好的是向列： 液晶相。該等液晶相藉由以偏光顯微鏡所觀察到之光學模 式而進行確認、識別。 本發明所使用之溶致型液晶化合物為了職予對親水性溶 劑之溶解性，較好的是具有親水性取代基。親水性取代基 較好的是選自由-COOM、-S03M、-P〇3m、_〇H、_雇2所 組成之群中之至少一種取代基。作為M,可列舉氫離子2 ' 如Li、Na、K、Cs之第一族金屬之離子、銨離子等。 本發明所使用之溶致型液晶化合物較好的是可吸收於 400 nm〜780 nm之波長區段之任一波長之光之有機化合 1335H.doc •13- 200914150 物。另外’藉由該溶致型液晶化合物之配向而獲得之光學 各向異性膜較好的是於波長5 5 0 nm時顯示吸收二色性。 作為本發明所使用之溶致型液晶化合物，通常使用水溶 性之二色性色素。作為本發明所使用之二色性色素之具體 例，可列舉：偶氮系色素、蒽醌系色素、茈系色素、陰丹 士林系色素、咪唑系色素 '靛藍系色素、呤畊系色素、酞 菁系色素、二苯甲烧系色素、°比唑酮系色素、芪系色素、 二苯甲院系色素、萘酿系色素、部花青系色素、啥駄嗣系 色素、二苯并吡喃系色素、茜素系色素、吖啶系色素、醌 亞胺系色素、噻唑系色素、:欠甲基系色素、硝基系色素、 亞硝基系色素等。Μ等之中較好的是偶氮系色素、蒽醌系 色素茈系色素、陰丹士林系色素及咪唑系色素。該等可 早獨使用或者混合使用兩種以上。為獲得黑色之偏光膜， 較好的是混合使用具有不同吸收光譜之複數種。 另外該等一色性色素較好的是包含磺酸基（_s〇3H)或羧 基（COOH)或該等之鹽之有機化合物、包含氮系取代基 (-NH2、顧R、_NR2、_nr1r2(此處 R、R,、尺2為 i價之有 機基）)之有機化合物，尤其好的是包含績酸基之有機化合 物或Θ —色性色素巾導人確酸基於提高對水之溶解 面有效$入一色性色素中之續酸基之個數越多對水 之溶解度越高。考慮到兼具對水之溶解度與光學各向異性 臈之耐水性而適當選擇該磺酸基之個數。 進而，作為本發明中所使用之二色性色素之具體例，可 列舉以通式（1)所表示之化合物： 133511.doc -14 - 200914150 (色原體）(S03M)n 通式（1) (η為1以上之整數，μ表示陽離子）。 作為通式（1)之M，較好的是氫離子、如Li、Na、K、Cs 之類之第一族金屬之離子、銨離子等。另外，作為色原體 部位，較好的是包含偶氮衍生物單元、蒽醌衍生物單元、 茈衍生物單元、咪唑衍生物單元及/或陰丹士林衍生物 者。 以上述通式(1)所表示之二色性色素於溶液中，偶氮化 Γ 纟物或多環式化合物結構等之色原體成為疏水性部位，績 酸及其鹽成為親水性部位，藉由兩者之平衡而使疏水性部 位彼此及親水性部位彼此聚集，整體呈現溶致型液晶。 作為以通式⑴所表示之二色性色素之具體例，可列舉 以下述之式（2)〜式（8)所表示之化合物等： [化1]The wettability and coating properties of the surface of the board are improved. Preferred as a surfactant: a nonionic surfactant. [Liquidotropic liquid crystal compound] The lyotropic liquid crystal compound used in the present invention means a liquid crystal compound having a property of causing phase transition of an isotropic phase-liquid crystal phase by changing temperature or concentration. The coating liquid is in a liquid crystal phase by the action of the lyotropic liquid crystal compound. The liquid crystal phase to be present is not particularly limited, and examples thereof include a nematic liquid crystal phase and a smectic liquid crystal phase 'cholesterol liquid crystal. Preferred is nematic: liquid crystal phase. These liquid crystal phases are confirmed and recognized by an optical mode observed by a polarizing microscope. The lyotropic liquid crystal compound used in the present invention preferably has a hydrophilic substituent in order to impart solubility to a hydrophilic solvent. The hydrophilic substituent is preferably at least one substituent selected from the group consisting of -COOM, -S03M, -P〇3m, _〇H, and _ employed 2. Examples of M include hydrogen ions 2' such as ions of a first group of metals such as Li, Na, K, and Cs, ammonium ions, and the like. The lyotropic liquid crystal compound used in the present invention is preferably an organic compound which can absorb light of any wavelength in the wavelength range of 400 nm to 780 nm, 1335H.doc • 13-200914150. Further, the optically anisotropic film obtained by the alignment of the lyotropic liquid crystal compound preferably exhibits absorption dichroism at a wavelength of 550 nm. As the lyotropic liquid crystal compound used in the present invention, a water-soluble dichroic dye is usually used. Specific examples of the dichroic dye used in the present invention include an azo dye, an anthraquinone dye, an anthraquinone dye, an indanthrene dye, an imidazole dye, an indigo dye, and a sorghum dye. , phthalocyanine pigment, benzophenone dye, bisazolone dye, ruthenium pigment, benzophenone pigment, naphthalene pigment, merocyanine pigment, lanthanide pigment, diphenyl And a pyranoid pigment, a halogen pigment, an acridine dye, a quinone imine dye, a thiazole dye, an under-methyl dye, a nitro dye, a nitroso dye, or the like. Among the above, azo dyes, lanthanide pigments, indanthrene pigments, and imidazole dyes are preferred. These may be used alone or in combination of two or more. In order to obtain a black polarizing film, it is preferred to use a plurality of kinds having different absorption spectra in combination. Further, the one-color pigment is preferably an organic compound containing a sulfonic acid group (_s〇3H) or a carboxyl group (COOH) or a salt thereof, and includes a nitrogen-based substituent (-NH2, Gu R, _NR2, _nr1r2 (this An organic compound having an organic group of the valence of R, R, and 2 is an organic compound, and particularly preferably an organic compound containing a carboxylic acid group or a phthalocyanine-based pigmented towel, which is effective for improving the dissolution surface of water. The more the number of the acid groups in the one-color pigment, the higher the solubility in water. The number of the sulfonic acid groups is appropriately selected in consideration of the water solubility to water and the optical anisotropy. Further, specific examples of the dichroic dye used in the present invention include a compound represented by the formula (1): 133511.doc -14 - 200914150 (chromogen) (S03M)n formula (1) (η is an integer of 1 or more, and μ represents a cation). As the M of the formula (1), a hydrogen ion, an ion of a first group metal such as Li, Na, K or Cs, an ammonium ion or the like is preferable. Further, as the chromogen moiety, those containing an azo derivative unit, an anthracene derivative unit, an anthracene derivative unit, an imidazole derivative unit and/or an indanthrene derivative are preferred. The dichroic dye represented by the above formula (1) is in a solution, and the chromogen of the arsenazo quinone or the polycyclic compound structure becomes a hydrophobic portion, and the acid and the salt thereof become a hydrophilic portion. By the balance of the two, the hydrophobic portions and the hydrophilic portions are aggregated with each other, and the liquid crystal is lyotropic as a whole. Specific examples of the dichroic dye represented by the formula (1) include compounds represented by the following formulas (2) to (8): [Chemical Formula 1]
1S〇3M)2 式 〇 式（2)中，R1為氫或氣，r2 A7从沉基、ArNH ArCONH ;作為該烷基，較好的 圾数為1〜4之烧基， 中更好的是曱基或者乙基；作為芸 ,作為方基（Ar)，較好的是取/ 或未經取代之苯基，其中更妊 更好的疋未經取代或以氣取代 I33511.doc 200914150 另外Μ與上述通式⑴同樣。1S〇3M) 2 In the formula (2), R1 is hydrogen or gas, r2 A7 is from sinking group, ArNH ArCONH; as the alkyl group, a preferred amount of burning is 1 to 4, preferably better It is a fluorenyl group or an ethyl group; as a hydrazine, as a square group (Ar), it is preferably a phenyl group which is taken or unsubstituted, wherein a more mature hydrazine is unsubstituted or substituted with a gas I33511.doc 200914150 Μ is the same as the above formula (1).
t ’ Α為以式⑷或者式(b)所表示者，η為2〜3。 為氧、燒基、㈣或院氧基，心表示取代或者未經 ^方基；作為烧基，較好的是碳數為卜4之烧基，其 =子的是甲基或者乙基；齒素較好的是填或者氯；另外 坑乳基較好的是碳數^個或2個之燒氧基，其中更好的是 位之苯基 [化2]t ′ Α is expressed by the formula (4) or the formula (b), and η is 2 to 3. Oxygen, alkyl, (iv) or alkoxy, the core represents a substituted or unsubstituted group; as the alkyl group, it is preferred that the carbon number is a burnt group of 4, and the = is a methyl group or an ethyl group; Preferably, the dentate is filled or chlorine; in addition, the pit base is preferably a carbon number of 2 or 2 alkoxy groups, and more preferably a phenyl group [Chemical 2]
作為芳基，較好的是取代或者未經取代之苯基， 其中較好的是未經取代或以甲氧基、乙氧基、氣或丁基取 代4位，或者以$基取代3位之苯基；_上述通式⑴同 133511.doc -16· 200914150 樣。 [化3]As the aryl group, a substituted or unsubstituted phenyl group is preferred, and it is preferred that unsubstituted or substituted 4-position with a methoxy group, ethoxy group, gas or butyl group, or substituted with a base group for 3 positions Phenyl; _ above formula (1) is the same as 133511.doc -16· 200914150. [Chemical 3]
式（6) 式（6)中η為3〜5，Μ與上述通式（1)同樣 [化4]In the formula (6), η is 3 to 5, and Μ is the same as the above formula (1).
-(S03M)2 式（7) 式（7)中Μ與上述通式（1)同樣 [化5]-(S03M)2 Formula (7) The formula (7) is the same as the above formula (1) [Chemical 5]
1S03M)2 式（8) 式（8)中Μ與上述通式（1)同樣。 向上述化合物中之有機化合物中導入磺酸基（磺化），例 133511.doc -17- 200914150 如可列舉於有機化合物中，使硫酸、氣績酸或者發煙硫酸 起作用而以磺基取代核之氫之方法。上述化合物中之鹽係 以例如链離子、卸離子、絶離子、錄離子等1價離子取代 可藉由酸之解離而產生之氫原子者。 作為本發明所使用之二色性色素之其他具體例，可列舉 於曰本專利特開2006-047966號公報、日本專利特開2005-255846號公報、日本專利特開2005-154746號公報、曰本 專利特開2002-090526號公報、日本專利特表平8-511109號 公報、曰本專利特表平2004-528603號公報中記載之二色 性色素。 本發明亦可使用市場上出售之二色性色素。作為其例， 可列舉C.I. DirectB67、DSCG (INTAL)、RU3 1.1 56、Methyl orange、AH6556、Sirius Supra Blown RLL、Benzopurpurin、 Copper-tetoracarboxyphthalocyanine、Acid Red 266、Cyanine Dye ' Violet 20、Perylenebiscarboximides、Benzopurpurin 4B > Methyleneblue (Basic Blue 9) ' Brilliant Yellow ' Acid red 18、Acid red 27 等。 [溶劑] 若本發明所使用之溶劑為均勻地溶解或分散溶致型液晶 化合物者則無特別限制。溶劑較好的是親水性溶劑。作為 親水性溶劑，例如可列舉水、乙醇類、溶纖劑類。亦可於 水中添加乙醇類、醚類、溶纖劑類、二曱亞砜、二甲基甲 醯胺等水溶性溶劑。另外亦可添加甘油、乙二醇等水溶性 化合物。該等添加物可用於調整水溶性液晶化合物之易溶 133511.doc • 18 - 200914150 性及水，谷液之乾燥速度。該等溶劑之調配量相對於水溶液 中之水100重量份’較好的是1〇〇重量份以下。 [基板] 本發明所使用之基板無特別限制，既可為單層者，亦可 為複數層（例如包含配向膜）之積層體。作為具體之基板可 列舉玻璃板及樹脂膜。於基板包含配向膜之情形，配向膜 較好的是已實施配向處理者。作為包含配向膜之基板，例 如可列舉於玻璃板上塗布有聚酿亞胺膜之基板。藉由眾所 周知之方法、例如朝固定方向之摩擦等機械性配向處理或 光配向處理等化學性配向處理，而賦予該聚醯亞胺臈配向 )生。關於基板之配向處理，可利用於「液晶便覽」（丸善 股份有限公司，2000年10月30日發行）226頁〜239頁等中記 載之眾所周知之方法而實施。 基板之玻璃板較好的是用於液晶胞者，例如無鹼玻璃。 作為市場上出售之玻璃板，例如可列舉K〇enig公司製造之 1737、旭硝子公司製造之AN635、NH Techn〇 Giass公 造之NA-35等。 於使用樹脂膜作為基板之情形時基板可具有可撓性，故 適用於要求具有可撓性之用途。樹脂膜之表面亦可藉由摩 擦等進行配向處理。或者亦可於樹脂膜之表面上形成包含 其他素材之配向膜。作為用於基板之樹脂膜之素材，若為 具有成臈性之樹脂則無特別限制，可列舉苯乙烯系樹脂、 (甲基）丙烯酸系樹脂、聚酯系樹脂、聚烯烴系樹脂、 膝么 丨苷伯 碲系樹脂、聚醯亞胺系樹脂、纖維素系樹脂、聚乙烯醇系 1335II.doc 19 200914150 樹脂、聚碳酸酯系樹脂。 基板之厚度可根據用途而確定，此外無特別限制，一般 為1 μηι〜1 000 μηι之範圍。 又 [塗布] 本發明所使用之塗布方法若為將塗布液均勻地塗布者則 無特別限制，可採取使用適當之塗布機之塗布方法。作為 塗布裝置’可列舉斜板式塗布機、槽模塗布機、棒式塗布 機、桿式塗布機、輥式塗布機、柔版印刷機、網版印刷 機、淋幕式塗布機、噴霧塗布機、旋塗機等。其中於可加 大剪切應力及剪切迷率之方面，較好的是斜板式塗布機、 槽模塗布機、刮棒塗布機。 [配向] 本發明所使用之溶致型液晶化合物若於液晶狀態下施加 剪切應力，則可藉由流動使其配向。溶致型液晶化合物於 液ΒΘ狀態下形成超分子聚集體，若對含有超分子聚集體之 塗布液施加剪切應力而使其流動，則超分子聚集體之長軸 方向於流動方向配向。配向方法除剪切應力以外，亦可組 合使用摩擦處理及光配向處理等配向處理、藉由磁場或電 場所進行之配向等。 [剪切應力] 本發明所使用之剪切應力，例如可藉由使用上述塗布機 將塗布液塗布於基板上而產生。或者藉由金屬或塑料之棒 或板朝一個方向摩擦塗布於基板上之塗布液，或以任意之 噴射裝置將塗布液噴射於基板上，以此方式亦可產生剪切 133511.doc -20- 200914150 應力。既可於將塗布液 可於塗⑽板上後對加-應力’亦 [乾無] 本發明所使用之乾燥方法無特 燥、減壓乾燥、加埶 例如使用自然乾 為…上之塗布液塗=广所使用之觸變⑽ =，…到外部之影響(風等)。另心== ”液相較於先前之塗布液難以產生揮發不均，且可 於本發明之製造方法中將塗布液二 進行加熱乾燥。料加熱乾燥方法， :使用利用空氣循環式乾燥供箱或熱親等任意乾燥裝置之 乾餘方法。加熱乾燥之情形之乾燥溫度較好的是5代〜12〇 C更好的疋80C〜100C。若為上述乾燥溫度範圍，則難 以產生揮發不均，且可於短時間内減少塗膜之殘存溶劑。 [積層體及光學各向異性膜] 藉由本發明之製造方法所獲得之積層體具有基板與形成 於基板上之包含溶致型液晶化合物之光學各向異性膜。若 為具有基板與光學各向異性膜之積層體，則其亦可包含其 他層。例如亦可於光學各向異性膜之表面設置包含樹脂之 保護層。或者亦可於基板之正面或背面預先設置平滑層、 脫模層或易黏接層等。本發明之積層體之厚度較好的是5 μηι〜500 μιη 〇 光學各向異性膜較好的是於波長550 nm時顯示吸收二色 性。將如上所述之光學各向異性膜例如用作偏光板。光學 133511.doc -21 - 200914150 各向異性膜之二色比於波長550 nm時較好的是2〇以上更 好的是30以上。光學各向異性膜之厚度較好的是〇〇5 μιη〜5 μιη，更好的是（Μ μηι〜丨μηι。若為上述之厚度範 圍，則可獲得良好之光學特性。再者二色比可藉由下述方 法算出：使用分光光度計，使直線偏光之測定光入射，使 測定光之偏光之電場向量平行及正交於光學各向異性膜之 配向方向而測定透射率。 [積層體及光學各向異性臈之用途] (1S03M) 2 Formula (8) The formula (8) is the same as the above formula (1). A sulfonic acid group (sulfonated) is introduced into the organic compound in the above compound, and 133511.doc -17- 200914150 is exemplified as an organic compound, and sulfuric acid, gas acid or fuming sulfuric acid is acted upon to be substituted with a sulfo group. The method of nuclear hydrogen. The salt in the above compound is a hydrogen atom which can be produced by dissociation of an acid by a monovalent ion such as a chain ion, an unloading ion, an anion ion or a recording ion. Other examples of the dichroic dye used in the present invention include those disclosed in JP-A-2006-047966, JP-A-2005-255846, JP-A-2005-154746, and 曰The dichroic dye described in Japanese Laid-Open Patent Publication No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. No. Hei. Commercially available dichroic pigments can also be used in the present invention. As an example, CI DirectB67, DSCG (INTAL), RU3 1.1 56, Methyl orange, AH6556, Sirius Supra Blown RLL, Benzopurpurin, Copper-tetoracarboxyphthalocyanine, Acid Red 266, Cyanine Dye 'Violet 20, Perylenebiscarboximides, Benzopurpurin 4B > Methyleneblue (Basic Blue 9) 'Brilliant Yellow ' Acid red 18, Acid red 27, etc. [Solvent] The solvent used in the present invention is not particularly limited as long as it uniformly dissolves or disperses the lyotropic liquid crystal compound. The solvent is preferably a hydrophilic solvent. Examples of the hydrophilic solvent include water, ethanol, and cellosolve. A water-soluble solvent such as ethanol, ether, cellosolve, disulfoxide or dimethylformamide may be added to the water. Further, a water-soluble compound such as glycerin or ethylene glycol may be added. These additives can be used to adjust the solubility of water-soluble liquid crystal compounds. 133511.doc • 18 - 200914150 Properties and drying rate of water and gluten. The amount of the solvent to be added is preferably 1 part by weight or less based on 100 parts by weight of water in the aqueous solution. [Substrate] The substrate used in the present invention is not particularly limited, and may be a single layer or a laminate of a plurality of layers (for example, an alignment film). Specific examples of the substrate include a glass plate and a resin film. In the case where the substrate contains an alignment film, it is preferred that the alignment film is subjected to an alignment treatment. The substrate including the alignment film may, for example, be a substrate on which a polyimide film is coated on a glass plate. The polyimine oxime is imparted to the compound by a well-known method such as mechanical alignment treatment such as rubbing in a fixed direction or a chemical alignment treatment such as photo-alignment treatment. The alignment processing of the substrate can be carried out by a well-known method described in "Liquid Crystals" (Maruzen Co., Ltd., issued on October 30, 2000), pages 226 to 239. The glass plate of the substrate is preferably used for liquid crystal cells, such as alkali-free glass. As the glass plate to be sold on the market, for example, 1737 manufactured by K〇enig Co., Ltd., AN635 manufactured by Asahi Glass Co., Ltd., NA-35 manufactured by NH Techn〇 Giass, and the like can be cited. When the resin film is used as the substrate, the substrate can have flexibility, and therefore it is suitable for applications requiring flexibility. The surface of the resin film can also be subjected to alignment treatment by rubbing or the like. Alternatively, an alignment film containing other materials may be formed on the surface of the resin film. The material of the resin film for the substrate is not particularly limited as long as it is a resin having a bismuth property, and examples thereof include a styrene resin, a (meth)acrylic resin, a polyester resin, a polyolefin resin, and a knee. Anthraquinone-based resin, polyimide-based resin, cellulose-based resin, polyvinyl alcohol-based 1335II.doc 19 200914150 resin, polycarbonate resin. The thickness of the substrate can be determined according to the use, and is not particularly limited, and is generally in the range of 1 μηι to 1 000 μηι. Further, the coating method used in the present invention is not particularly limited as long as the coating liquid is uniformly applied, and a coating method using a suitable coater can be employed. Examples of the coating device include a slant plate coater, a slot die coater, a bar coater, a bar coater, a roll coater, a flexographic press, a screen printing machine, a curtain coater, and a spray coater. , spin coating machine, etc. Among them, a slant plate coating machine, a slot die coater, and a bar coater are preferred in terms of increasing shear stress and shear rate. [Alignment] When the lyotropic liquid crystal compound used in the present invention exerts shear stress in a liquid crystal state, it can be aligned by flow. The lyotropic liquid crystal compound forms a supramolecular aggregate in a liquid helium state, and when a shear stress is applied to the coating liquid containing the supramolecular aggregate to flow, the long axis direction of the supramolecular aggregate is aligned in the flow direction. In addition to the shear stress, the alignment method may be combined with an alignment treatment such as a rubbing treatment or a photo-alignment treatment, or an alignment by a magnetic field or an electric field. [Shear Stress] The shear stress used in the present invention can be produced, for example, by applying a coating liquid onto a substrate by using the above coater. Alternatively, the coating liquid applied to the substrate may be rubbed in one direction by a metal or plastic rod or plate, or the coating liquid may be sprayed onto the substrate by any spraying means, thereby producing shearing 133511.doc -20- 200914150 Stress. The coating method can be applied to the coated (10) plate after the addition-stress 'also [dry no]. The drying method used in the present invention is not dried, dried under reduced pressure, and dried, for example, using a natural drying solution. The influence of the thixotropic (10) =, ... to the outside (wind, etc.) used by Tu = Guang. It is difficult to produce volatilization unevenness in the liquid phase compared with the previous coating liquid, and the coating liquid 2 can be heated and dried in the production method of the present invention. The material heating and drying method: using the air circulation type drying tank Or a dry method of any drying device such as a hot parent. The drying temperature in the case of heat drying is preferably 代80C to 100C which is preferably 5 passages to 12 Torr C. If the drying temperature range is above, it is difficult to cause unevenness in volatilization. Further, the residual solvent of the coating film can be reduced in a short time. [Laminate and Optical Anisotropic Film] The laminate obtained by the production method of the present invention has a substrate and an optical containing a lyotropic liquid crystal compound formed on the substrate. An anisotropic film may have another layer if it is a laminate having a substrate and an optically anisotropic film. For example, a protective layer containing a resin may be provided on the surface of the optically anisotropic film. The front side or the back side is provided with a smoothing layer, a release layer or an easy-adhesive layer, etc. The thickness of the laminated body of the present invention is preferably 5 μηι to 500 μηη 〇 optical anisotropic film. It exhibits absorption dichroism at a wavelength of 550 nm. The optically anisotropic film as described above is used, for example, as a polarizing plate. Optics 133511.doc -21 - 200914150 Anisotropic film has a dichroic ratio at a wavelength of 550 nm. Preferably, 2 Å or more is more preferably 30 or more. The thickness of the optically anisotropic film is preferably 〇〇 5 μm to 5 μmη, more preferably (Μ μηι 丨 ηηηι. Further, good optical characteristics can be obtained. Further, the two-color ratio can be calculated by using a spectrophotometer to make the measurement light of the linearly polarized light incident, and the electric field vector of the polarization of the measurement light is parallel and orthogonal to the optical directions. Transmittance is measured by the alignment direction of the opposite film. [Use of laminate and optical anisotropy] (
藉由本發明所獲得之積層體及光學各向異性膜有效利用 光學各向異性而用於各種光學元件，特別是可適合用作偏 光板及相位差板。積層體及光學各向異性膜之用途，例 如：電腦監視器、筆記型電腦、影印機等〇Α (〇ffice Automation ’辦公自動化）設備；行動電話、鐘錶、數位相 機、個人數位助理（PDA，Personal Digital Assistant))、掌 上型遊戲機等可攜式設備；攝影機、電視、電子爐等之家 用設備；後方監視器、汽車導航系統用監視器、汽車音響 等車載用設備；商業店鋪用資訊用監視器等展示設備；監 視用監視器等警備設備；看護用監視器、醫療用監視器等 液晶顯示裝置。 光學各向異性膜既可自基板剝離而使用，亦可以積層體 之狀態使用。於以積層體之狀態用於光學用途之情形時， 基板較好的是於可見光之波長區域為透明者。於自基板剝 離之情形時’較好的是可積層於其他載體或光學元件上而 使用。 133511.doc -22· 200914150 [實施例1] 調整包含料溶致錢晶化合物之下述化學 化t物的溶液（QptW—製造之刪）之濃度，將塗= :製：全固形物濃度為16重量％。藉由偏光顯微鏡進行: 察’、'，σ果該塗布液呈向列型液晶相。 [化6] 、(S〇3H)nThe laminate and the optically anisotropic film obtained by the present invention are effectively used for various optical elements by utilizing optical anisotropy, and are particularly suitable for use as a polarizing plate and a phase difference plate. The use of laminates and optically anisotropic films, such as computer monitors, notebook computers, photocopiers, etc. (〇ffice Automation 'office automation) equipment; mobile phones, clocks, digital cameras, personal digital assistants (PDAs, Personal Digital Assistant)), portable devices such as handheld game consoles; household equipment such as cameras, televisions, and electronic stoves; rear monitors, monitors for car navigation systems, car audio equipment, etc.; Display devices such as monitors; guard devices such as monitors for monitoring; liquid crystal display devices such as monitors for medical care and medical monitors. The optically anisotropic film may be used by being peeled off from the substrate or in the form of a laminate. When it is used for optical use in the state of a laminate, the substrate is preferably transparent in the wavelength region of visible light. In the case of peeling from the substrate, it is preferred to use it on other carriers or optical elements. 133511.doc -22· 200914150 [Example 1] Adjusting the concentration of a solution (QptW-manufactured) of the following chemically-organized t-containing compound containing the lyophthalate compound, the coating =: system: the total solid concentration is 16% by weight. It was carried out by a polarizing microscope: the coating liquid was in the nematic liquid crystal phase. [(6), (S〇3H)n
(S〇3H)n 、(S03H)n 使用斜板式塗布機於破璃板上—邊施加剪切應力塗布上 述塗布液，而製作厚度為0.4μΓη之光學各向異性膜。塗布 液與光學各向異性膜之特性示於表1。塗布液之㈣指數 Μ常大為"9,故光學各向異性臈之二色比非常高為 以’透射率之偏差亦較少為5% ’且幾乎未發現不均(塗布 不均與揮發不均）。 [實施例2] 與實施们同樣於包含溶致型液晶化合物之溶液（〇ρ_ 公司製造之Ν 01 5 )中添加水而使其全固形物濃度達到為i 〇 重量％。向其中添加相對於溶致型液晶化合物為3重量％之 1335H.doc -23· 200914150 聚丙烯系增稠劑（San Nopco公司製造之SN thickener615)而 調整塗布液。藉由偏光顯微鏡進行察，結果該塗布液呈向 列型液晶相。使用斜板式塗布機於玻璃板上一邊施加剪切 應力一邊塗布上述塗布液，而製作厚度為〇5以出之光學 各向異性膜。塗布液與光學各向異性臈之特性示於表i。 塗布液之觸變指數Ti較大為丨.46，故光學各向異性膜之二 色比較高為22，透射率之偏差亦較少為5%，且幾乎未發 現不均（塗布不均與揮發不均 [比較例1] 化合物之溶液（Optiva 固形物濃度達到1 〇重 化合物為1 0重量％之 與實施例1同樣於包含溶致型液晶 公司製造之N015)中添加水而使其全 量0/〇。向其中添加相對於溶致型液晶 經丙基纖維素（日本曹達公司製造之NISS〇 Hpc H)而調整 塗布液。藉由偏光顯微鏡進行觀察，結果該塗布液呈向列 型液晶相。使用斜板式塗布機於玻璃板上—邊施加剪切應 力-邊塗布上述塗布液’而製作厚度為。5响之光學各向 異性膜。塗布液與光學各向異性膜之特性示於丄。塗布液 之觸變指數Ti較小為K〇9,故光學各向異性膜之二色比較 低為12，透射率之偏差亦非常大為15%，亦發現塗布不 均。-般認為塗布不均之原因在於，作為塗布時之黏卢之 標準的於剪切速率咖秒·]時之黏度v_。較大:22〇 mPa.s ° [比較例2] 之〉容液（Optiva 與實施例1同樣於包含溶致型液晶化合物 133511.doc -24- 200914150 公司製造之NO 15)中添加水而將塗布液調整為全固形物濃 度達到10重量％。藉由偏光顯微鏡進行觀察，結果該塗布 液呈向列型液晶相。使用斜板式塗布機於破璃板上一邊施 加剪切應力一邊塗布上述塗布液，而製作厚度為〇4 之 光學各向異性膜。塗布液與光學各向異性臈之特性示於表 1。塗布液之觸變指數Ti較小為丨.08，故光學各向異性膜之 —色比較低為16 ,透射率之偏差亦較大為8%，亦幾乎未 發現揮發*均。—般認為揮發不均之原因係加水導致之過 度稀釋。 [比較例3 ] 對包含作為溶致型液晶化合物之下述化學結構之偶氮系 :合物與水、且全固形物濃度為2重量％之塗布液加以調 。藉由偏光顯微鏡觀察，結果該塗布液呈向列型液晶 t。使料板式塗布機於麵板上-邊施加剪切應力^ 塗布上述塗布液，，厚度為〇2㈣之光學各向異性 :。塗布液與光學各向異性膜之特性示於表i。塗 觸變指數Ti為1.00即|觸 …、觸變性，故光學各向異性膜之二色 比非常低為3，透射率夕推* + 匕 旱之偏差亦較大為10%，亦未發現揮 發不均。一般認為揮 a 釋。 谭發不均之原因係加水導致之過度稀 [化7](S〇3H)n and (S03H)n The above coating liquid was applied by applying a shear stress to a glass plate using a swash plate coater to prepare an optically anisotropic film having a thickness of 0.4 μΓ. The properties of the coating liquid and the optically anisotropic film are shown in Table 1. The (four) index of the coating liquid is often large as "9, so the optical anisotropy 二 has a very high dichroic ratio of less than 5% of the transmittance, and almost no unevenness is found (uneven coating) Uneven volatilization). [Example 2] Water was added to a solution containing a lyotropic liquid crystal compound (Ν 5 01 5 manufactured by 公司ρ_ Company) in the same manner as in the embodiment to have a total solid concentration of i 〇 by weight. To this was added a 1335H.doc -23·200914150 polypropylene thickener (SN thickener 615, manufactured by San Nopco Co., Ltd.) in an amount of 3% by weight based on the lyotropic liquid crystal compound to adjust the coating liquid. The coating liquid was observed by a polarizing microscope, and as a result, the coating liquid was in a nematic liquid crystal phase. The coating liquid was applied while applying a shear stress to a glass plate using a swash plate coater to prepare an optically anisotropic film having a thickness of 〇5. The properties of the coating liquid and optical anisotropy are shown in Table i. The thixotropy index Ti of the coating liquid is as large as 丨46, so the two colors of the optically anisotropic film are relatively high at 22, and the deviation of the transmittance is also less than 5%, and almost no unevenness is found (uneven coating and Uneven volatilization [Comparative Example 1] A solution of a compound (Optiva solid content is 10% by weight of the compound, and 10% by weight of the N015 produced by the lyotropic liquid crystal company in the same manner as in Example 1) 0/〇. The coating liquid was adjusted by adding propyl cellulose (NISS〇Hpc H manufactured by Nippon Soda Co., Ltd.) to the lyotropic liquid crystal. The liquid was observed by a polarizing microscope, and the coating liquid was nematic liquid crystal. The optically anisotropic film having a thickness of 5 Å was prepared by applying a slanting plate coating machine to a glass plate while applying shear stress to the coating liquid. The properties of the coating liquid and the optically anisotropic film are shown in丄 The thixotropic index Ti of the coating liquid is smaller than K〇9, so the two colors of the optically anisotropic film are relatively low at 12, and the deviation of the transmittance is also very large at 15%, and uneven coating is also found. The reason for uneven coating is that, as a coating Viscosity of the standard of the viscosity at the shear rate of coffee. v.. Larger: 22〇mPa.s ° [Comparative Example 2]>Liquid (Optiva is the same as Example 1 containing lyotropic liquid crystal compound) 133511.doc -24- 200914150 The water was added to the NO 15), and the coating liquid was adjusted to have a total solid concentration of 10% by weight. The coating liquid was observed by a polarizing microscope, and the coating liquid was a nematic liquid crystal phase. The swash plate coating machine applied the coating liquid while applying shear stress to the glass plate to prepare an optically anisotropic film having a thickness of 〇 4. The properties of the coating liquid and the optical anisotropy were shown in Table 1. The thixotropy index Ti is smaller than 丨.08, so the optical anisotropic film has a relatively low color of 16 and a deviation of transmittance of 8%, and almost no volatilization* is found. The reason for this is that the water is excessively diluted by the addition of water. [Comparative Example 3] A coating liquid containing an azo-based compound having the following chemical structure as a lyotropic liquid crystal compound and water and having a total solid concentration of 2% by weight Adjusted by a polarizing microscope The coating liquid is a nematic liquid crystal t. The coating plate is coated with a shear stress on the panel to apply the coating liquid to a thickness of 〇2 (4). Anisotropy: coating liquid and optical anisotropy The characteristics of the film are shown in Table i. The coating thixotropic index Ti is 1.00, ie, touch..., thixotropy, so the dichroic ratio of the optically anisotropic film is very low at 3, and the transmittance is higher than the deviation of the +* It is 10%, and no volatilization is found. It is generally considered to be a release. The reason for the unevenness of Tan is due to excessive dilution caused by water addition.
133511.doc 200914150 [表l]133511.doc 200914150 [Table l]
[評價][Evaluation]
由以上說明之實施例與比較例之特性可知，於使用觸變 指數h未滿1.2之塗布液之情形，難以製作無揮發不均或塗 布不均、透射率偏差較小（5%以下）、二色比較高（2〇以上） 之光學各向異性膜。反之於使用觸變指數丁丨為12以上之塗 布液之情形，可製作無不均、透射率偏差較小（5%以下）、 二色比較高（20以上）之光學各向異性膜。 [測定•評價方法] 黏度、觸變指數Ti之測定方法：使用HAAKE公司製造之According to the characteristics of the examples and the comparative examples described above, it is difficult to produce non-volatile unevenness or uneven coating, and the transmittance variation is small (5% or less) when a coating liquid having a thixotropic index h of less than 1.2 is used. An optically anisotropic film having a relatively high two-color (2 Å or more). On the other hand, in the case of using a coating liquid having a thixotropic index of 12 or more, an optically anisotropic film having no unevenness, a small variation in transmittance (5% or less), and a relatively high two-color (20 or more) can be produced. [Measurement and Evaluation Method] Method for Measuring Viscosity and Thixotropy Index Ti: Using HAAKE Co., Ltd.
RheoStress600 ’於以下條件下測定v〗〇〇 (2rc )、v丨〇⑽（23 •圓錐：C35/l(直徑35 mm，傾斜角1。) • Solvent trap :使用 • Gap : 0.050 mm •測定溫度：23°C •剪切速率：10秒-1〜4〇00秒-1 二色比、透射率之測定方法：使用具有葛蘭-湯普生偏 光元件之分光光度計（日本分光公司製造之U_4 1 00)，使波 133511.doc -26- 200914150 長550 nm之直線偏光之測定光人射，求得最大透射率 之直線偏光之透射率kl以及與最大透射率方向正交 ° 之直線偏光之透射率k2，藉由下式算出二色比與透乂射之方向 •二色比 slogCl/kd/IogU/kO 。 •透射率=(]<：, + k2)/2 二色比之平均值，於距離縱8咖橫8⑽之樣 ⑽處，於縱方向上取3點，橫方向上取3點，合 點，而求得其平均值。表1中之二色比為該平均值疋9 率亦針對相同之9點加以測冑’將(最格最小 透射 之透射率之偏差。 〜表1 不均之評價方法：對縱8咖橫8 cm之樣品照射 之光’以目視觀察不均。再者揮發不均係於樣品之表： 見如煙靄彌漫，塗布不均係可見平行於塗布方 ：可 故可區別二者。 條紋’ 【圖式簡單說明】 圖1係針對⑷本發明之塗布液與⑻先前之塗布液 _ 剪切速率（橫轴）與黏度（縱軸）之關係之圖。 不 133511.doc 27-RheoStress600 'measured under the following conditions 〇〇(2rc ), v丨〇(10)(23 • cone: C35/l (diameter 35 mm, tilt angle 1.) • Solvent trap : used • Gap : 0.050 mm • measured temperature : 23 ° C • Shearing rate: 10 sec -1 to 4 〇 00 sec - 1 Two-color ratio, transmittance measurement method: Using a spectrophotometer with a Glan-Thompson polarizing element (U_4 1 manufactured by JASCO Corporation) 00), the wave 133511.doc -26- 200914150 linear 550 nm long polarized light measurement of the light, the maximum transmittance of the linear polarized light transmittance kl and the maximum transmittance direction of the linear polarization transmission The rate k2 is calculated by the following equation: the direction of the dichroic ratio and the direction of the diffracting • the dichroic ratio slogCl/kd/IogU/kO. • Transmittance = (] <:, + k2)/2 The average of the dichroic ratio At the distance (10) of the vertical 8 coffee horizontal 8 (10), take 3 points in the longitudinal direction and 3 points in the horizontal direction, and combine the points to obtain the average value. The two-color ratio in Table 1 is the average value. 9 rate is also measured for the same 9 points 'will (the deviation of the transmission of the minimum transmission of the smallest grid. ~ Table 1 evaluation method of unevenness: for the vertical 8 The light irradiated by the sample of 8 cm in width is visually observed unevenly. The uneven volatilization is attached to the surface of the sample: see, if the smoke is diffuse, the uneven coating is visible parallel to the coated side: it can be distinguished by the difference. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a graph showing the relationship between (4) the coating liquid of the present invention and (8) the previous coating liquid _ shear rate (horizontal axis) and viscosity (vertical axis).
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| RU2047643C1 (en) * | 1993-05-21 | 1995-11-10 | Хан Ир Гвон | Material for polarizing coating |
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| JP2001337225A (en) * | 2000-05-29 | 2001-12-07 | Nitto Denko Corp | Multilayer optical element and liquid crystal display device |
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| JP2005225927A (en) * | 2004-02-12 | 2005-08-25 | Nippon Paint Co Ltd | Aqueous coating composition and coating film forming method using the same |
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