TWI807200B - Solvent-free type curable composition, cured film using the same, color filter, and display device - Google Patents
Solvent-free type curable composition, cured film using the same, color filter, and display device Download PDFInfo
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- TWI807200B TWI807200B TW109124379A TW109124379A TWI807200B TW I807200 B TWI807200 B TW I807200B TW 109124379 A TW109124379 A TW 109124379A TW 109124379 A TW109124379 A TW 109124379A TW I807200 B TWI807200 B TW I807200B
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- solvent
- curable composition
- diffusing agent
- particle diameter
- light
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- JIGUICYYOYEXFS-UHFFFAOYSA-N 3-tert-butylbenzene-1,2-diol Chemical compound CC(C)(C)C1=CC=CC(O)=C1O JIGUICYYOYEXFS-UHFFFAOYSA-N 0.000 description 1
- OKISUZLXOYGIFP-UHFFFAOYSA-N 4,4'-dichlorobenzophenone Chemical compound C1=CC(Cl)=CC=C1C(=O)C1=CC=C(Cl)C=C1 OKISUZLXOYGIFP-UHFFFAOYSA-N 0.000 description 1
- 239000004342 Benzoyl peroxide Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- NLZUEZXRPGMBCV-UHFFFAOYSA-N Butylhydroxytoluene Chemical compound CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 NLZUEZXRPGMBCV-UHFFFAOYSA-N 0.000 description 1
- YYLLIJHXUHJATK-UHFFFAOYSA-N Cyclohexyl acetate Chemical compound CC(=O)OC1CCCCC1 YYLLIJHXUHJATK-UHFFFAOYSA-N 0.000 description 1
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 description 1
- ZMDDERVSCYEKPQ-UHFFFAOYSA-N Ethyl (mesitylcarbonyl)phenylphosphinate Chemical compound C=1C=CC=CC=1P(=O)(OCC)C(=O)C1=C(C)C=C(C)C=C1C ZMDDERVSCYEKPQ-UHFFFAOYSA-N 0.000 description 1
- 229910002601 GaN Inorganic materials 0.000 description 1
- 229910005540 GaP Inorganic materials 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- QMXOFBXZEKTJIK-UHFFFAOYSA-N Glycinol Natural products C1=C(O)C=C2OCC3(O)C4=CC=C(O)C=C4OC3C2=C1 QMXOFBXZEKTJIK-UHFFFAOYSA-N 0.000 description 1
- 229910004262 HgTe Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000673 Indium arsenide Inorganic materials 0.000 description 1
- PSBPNWBGNOWCCU-UHFFFAOYSA-N OB(O)O.S.S.S Chemical compound OB(O)O.S.S.S PSBPNWBGNOWCCU-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000002202 Polyethylene glycol Substances 0.000 description 1
- BGNXCDMCOKJUMV-UHFFFAOYSA-N Tert-Butylhydroquinone Chemical compound CC(C)(C)C1=CC(O)=CC=C1O BGNXCDMCOKJUMV-UHFFFAOYSA-N 0.000 description 1
- 229910010413 TiO 2 Inorganic materials 0.000 description 1
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 1
- 239000007983 Tris buffer Substances 0.000 description 1
- NOZAQBYNLKNDRT-UHFFFAOYSA-N [diacetyloxy(ethenyl)silyl] acetate Chemical compound CC(=O)O[Si](OC(C)=O)(OC(C)=O)C=C NOZAQBYNLKNDRT-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000003342 alkenyl group Chemical group 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 125000002877 alkyl aryl group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- ANVURUAGPDCRFI-UHFFFAOYSA-N amino(nitro)cyanamide Chemical compound N#CN(N)[N+]([O-])=O ANVURUAGPDCRFI-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 125000000852 azido group Chemical group *N=[N+]=[N-] 0.000 description 1
- CHIHQLCVLOXUJW-UHFFFAOYSA-N benzoic anhydride Chemical compound C=1C=CC=CC=1C(=O)OC(=O)C1=CC=CC=C1 CHIHQLCVLOXUJW-UHFFFAOYSA-N 0.000 description 1
- 229950011260 betanaphthol Drugs 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 125000006269 biphenyl-2-yl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C1=C(*)C([H])=C([H])C([H])=C1[H] 0.000 description 1
- VYHBFRJRBHMIQZ-UHFFFAOYSA-N bis[4-(diethylamino)phenyl]methanone Chemical compound C1=CC(N(CC)CC)=CC=C1C(=O)C1=CC=C(N(CC)CC)C=C1 VYHBFRJRBHMIQZ-UHFFFAOYSA-N 0.000 description 1
- HXTBYXIZCDULQI-UHFFFAOYSA-N bis[4-(methylamino)phenyl]methanone Chemical compound C1=CC(NC)=CC=C1C(=O)C1=CC=C(NC)C=C1 HXTBYXIZCDULQI-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 235000010354 butylated hydroxytoluene Nutrition 0.000 description 1
- 150000001716 carbazoles Chemical class 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- MGNCLNQXLYJVJD-UHFFFAOYSA-N cyanuric chloride Chemical compound ClC1=NC(Cl)=NC(Cl)=N1 MGNCLNQXLYJVJD-UHFFFAOYSA-N 0.000 description 1
- 125000000392 cycloalkenyl group Chemical group 0.000 description 1
- BLCKNMAZFRMCJJ-UHFFFAOYSA-N cyclohexyl cyclohexyloxycarbonyloxy carbonate Chemical compound C1CCCCC1OC(=O)OOC(=O)OC1CCCCC1 BLCKNMAZFRMCJJ-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 150000008049 diazo compounds Chemical class 0.000 description 1
- 125000005594 diketone group Chemical group 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- 230000005281 excited state Effects 0.000 description 1
- 229910052949 galena Inorganic materials 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 125000001072 heteroaryl group Chemical group 0.000 description 1
- 125000004366 heterocycloalkenyl group Chemical group 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- RPQDHPTXJYYUPQ-UHFFFAOYSA-N indium arsenide Chemical compound [In]#[As] RPQDHPTXJYYUPQ-UHFFFAOYSA-N 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 229910052740 iodine Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- WXVQVZBJMWDACQ-UHFFFAOYSA-N isocyanato 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)ON=C=O WXVQVZBJMWDACQ-UHFFFAOYSA-N 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 150000002921 oxetanes Chemical class 0.000 description 1
- MPQXHAGKBWFSNV-UHFFFAOYSA-N oxidophosphanium Chemical class [PH3]=O MPQXHAGKBWFSNV-UHFFFAOYSA-N 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- LYXOWKPVTCPORE-UHFFFAOYSA-N phenyl-(4-phenylphenyl)methanone Chemical compound C=1C=C(C=2C=CC=CC=2)C=CC=1C(=O)C1=CC=CC=C1 LYXOWKPVTCPORE-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000000206 photolithography Methods 0.000 description 1
- 229920001515 polyalkylene glycol Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000007261 regionalization Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000011257 shell material Substances 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 229910052950 sphalerite Inorganic materials 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000004250 tert-Butylhydroquinone Substances 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- 235000019281 tert-butylhydroquinone Nutrition 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 150000003573 thiols Chemical class 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- FRGPKMWIYVTFIQ-UHFFFAOYSA-N triethoxy(3-isocyanatopropyl)silane Chemical compound CCO[Si](OCC)(OCC)CCCN=C=O FRGPKMWIYVTFIQ-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- MZIGEXAGOVUGIC-UHFFFAOYSA-N trimethyl (5-methyl-4-oxohex-5-enyl) silicate Chemical compound CO[Si](OC)(OC)OCCCC(=O)C(C)=C MZIGEXAGOVUGIC-UHFFFAOYSA-N 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/0005—Production of optical devices or components in so far as characterised by the lithographic processes or materials used therefor
- G03F7/0007—Filters, e.g. additive colour filters; Components for display devices
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
- G03F7/027—Non-macromolecular photopolymerisable compounds having carbon-to-carbon double bonds, e.g. ethylenic compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/30—Inkjet printing inks
- C09D11/38—Inkjet printing inks characterised by non-macromolecular additives other than solvents, pigments or dyes
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B5/00—Optical elements other than lenses
- G02B5/20—Filters
-
- 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
- G02F1/015—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 semiconductor elements having potential barriers, e.g. having a PN or PIN junction
- G02F1/017—Structures with periodic or quasi periodic potential variation, e.g. superlattices, quantum wells
- G02F1/01791—Quantum boxes or quantum dots
-
- 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
- G02F1/133509—Filters, e.g. light shielding masks
- G02F1/133514—Colour filters
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03F—PHOTOMECHANICAL PRODUCTION OF TEXTURED OR PATTERNED SURFACES, e.g. FOR PRINTING, FOR PROCESSING OF SEMICONDUCTOR DEVICES; MATERIALS THEREFOR; ORIGINALS THEREFOR; APPARATUS SPECIALLY ADAPTED THEREFOR
- G03F7/00—Photomechanical, e.g. photolithographic, production of textured or patterned surfaces, e.g. printing surfaces; Materials therefor, e.g. comprising photoresists; Apparatus specially adapted therefor
- G03F7/004—Photosensitive materials
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- General Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Nonlinear Science (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Optics & Photonics (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Mathematical Physics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Materials For Photolithography (AREA)
- Optical Filters (AREA)
- Polymerisation Methods In General (AREA)
Abstract
Description
本申請案主張於2019年7月22日在韓國智慧財產局提出申請的韓國專利申請案第10-2019-0088405號的優先權及權利，所述韓國專利申請的全部內容併入本案供參考。 This application claims priority and rights to Korean Patent Application No. 10-2019-0088405 filed with the Korea Intellectual Property Office on July 22, 2019, the entire content of which is incorporated herein by reference.
本發明是有關於一種無溶劑型可固化組合物、使用其製造的固化膜、包含固化膜的濾色器以及包含濾色器的顯示裝置。 The present invention relates to a solvent-free curable composition, a cured film manufactured using the same, a color filter including the cured film, and a display device including the color filter.
一般來說，應用於顯示器的濾色器透過如下步驟來形成：使用感光性抗蝕劑組合物，透過使用光罩經由曝光製程形成所需圖案且接著經由顯影製程溶解並去除非曝光區域。濾色器的材料可能需要鹼可溶性、高靈敏度、與基板的黏附、耐化學性、耐熱性等。對於色彩材料，通常使用顏料或染料。 Generally, a color filter applied to a display is formed by using a photoresist composition, forming a desired pattern through an exposure process using a photomask and then dissolving and removing non-exposed regions through a developing process. The material of the color filter may require alkali solubility, high sensitivity, adhesion to a substrate, chemical resistance, heat resistance, and the like. For coloring materials, pigments or dyes are usually used.
然而，顏料具有極好的耐熱性或耐化學性但不能良好地分散於溶劑中，且因此不具有例如亮度的極好的色彩特性，而染料 具有極好的色彩特性但耐久性劣化，且因此不具有極好的耐熱性或耐化學性。 However, pigments have excellent heat resistance or chemical resistance but cannot be dispersed well in solvents, and thus do not have excellent color characteristics such as brightness, while dyes Has excellent color characteristics but deteriorates in durability, and thus does not have excellent heat resistance or chemical resistance.
因此，正持續開發能夠克服使用顏料或染料作為色彩材料的當前使用的感光性樹脂組合物的技術限制的新型光致發光型感光性樹脂組合物及應用這種新型光致發光型感光性樹脂組合物(即，使用量子點的組合物)的濾色材料。 Therefore, new photoluminescent photosensitive resin compositions capable of overcoming technical limitations of currently used photosensitive resin compositions using pigments or dyes as color materials and color filter materials using such new photoluminescent photosensitive resin compositions (i.e., compositions using quantum dots) are being continuously developed.
這種含有量子點的組合物可視製程方法分為用光刻方法製備的負型光刻膠類型及用噴墨方法製備的油墨類型，且油墨型含有量子點的組合物又可分為包含溶劑的溶劑型組合物及完全不包含溶劑的無溶劑型組合物。 The composition containing quantum dots can be divided into negative photoresist type prepared by photolithography method and ink type prepared by inkjet method according to the process method, and the ink type composition containing quantum dots can be further divided into solvent type composition containing solvent and solvent-free composition containing no solvent at all.
然而，由於溶劑型油墨組合物不僅具有由於在噴墨期間的溶劑揮發而導致噴嘴變乾且因此噴嘴堵塞、在噴墨之後隨時間流逝單層膜縮減等問題，而且還具有在固化之後存在嚴重的厚度偏差的缺點且因此難以適用於實際製程，因此最近，已優選不包含任何溶劑的無溶劑型油墨組合物。另外，由於將量子點本身應用於溶劑型組合物的技術當前已被評估為達到某一極限，因此對於無溶劑型油墨組合物的開發需求持續增加。 However, since solvent-type ink compositions not only have problems such as drying of the nozzle due to volatilization of the solvent during ink-jet and thus nozzle clogging, shrinkage of a monolayer film over time after ink-jet, and the like, but also have a disadvantage of severe thickness deviation after curing and thus are difficult to apply to actual processes, recently, solvent-free ink compositions that do not contain any solvent have been preferred. In addition, since the technology of applying quantum dots themselves to solvent-based compositions has currently been evaluated to a certain limit, the demand for development of solvent-free ink compositions continues to increase.
本發明實施例提供一種當透過控制光漫射劑的初級顆粒直徑及次級顆粒直徑來使光吸收率及光轉換最大化時沉澱所需的無溶劑型可固化組合物。 Embodiments of the present invention provide a solventless curable composition required for precipitation when maximizing light absorption and light conversion by controlling the primary particle diameter and secondary particle diameter of the light diffusing agent.
另一實施例提供一種使用無溶劑型可固化組合物製造的固化膜。 Another embodiment provides a cured film produced using the solvent-free curable composition.
另一實施例提供一種包含固化膜的濾色器。 Another embodiment provides a color filter including a cured film.
另一實施例提供一種包含濾色器的顯示裝置。 Another embodiment provides a display device including a color filter.
實施例提供一種無溶劑型可固化組合物，所述無溶劑型可固化組合物包含(A)量子點；(B)可聚合單體；以及(C)光漫射劑，所述光漫射劑具有50奈米(nm)至200奈米的初級顆粒直徑及120奈米至250奈米的次級顆粒直徑。 Embodiments provide a solvent-free curable composition comprising (A) quantum dots; (B) a polymerizable monomer; and (C) a light diffusing agent having a primary particle diameter of 50 nanometers (nm) to 200 nm and a secondary particle diameter of 120 nm to 250 nm.
光漫射劑可具有80奈米至180奈米的初級顆粒直徑及140奈米至230奈米的次級顆粒直徑。 The light diffusing agent may have a primary particle diameter of 80 nm to 180 nm and a secondary particle diameter of 140 nm to 230 nm.
光漫射劑的次級顆粒尺寸可具有光漫射劑的初級顆粒尺寸的1.5倍至2.5倍的尺寸。 The secondary particle size of the light diffusing agent may have a size of 1.5 times to 2.5 times the primary particle size of the light diffusing agent.
光漫射劑可為金紅石型光漫射劑與銳鈦礦型光漫射劑的混合物。 The light diffusing agent may be a mixture of a rutile type light diffusing agent and an anatase type light diffusing agent.
可以1：3至3：1的重量比包含混合物中的金紅石型光漫射劑及銳鈦礦型光漫射劑。 The rutile-type light-diffusing agent and the anatase-type light-diffusing agent in the mixture may be included in a weight ratio of 1:3 to 3:1.
光漫射劑可包含硫酸鋇、碳酸鈣、二氧化鈦、氧化鋯或其組合。 The light diffusing agent may include barium sulfate, calcium carbonate, titanium dioxide, zirconium oxide, or combinations thereof.
量子點可包含具有處於450奈米至580奈米的最大熒光發射波長(熒光λem)的量子點、具有處於580奈米至700奈米的最大熒光發射波長(熒光λem)的量子點或其組合。 The quantum dots may comprise quantum dots having a maximum fluorescence emission wavelength (fluorescence λ em ) between 450 nm and 580 nm, quantum dots having a maximum fluorescence emission wavelength (fluorescence λ em ) between 580 nm and 700 nm, or a combination thereof.
無溶劑型可固化組合物可更包含聚合起始劑。 The non-solvent curable composition may further include a polymerization initiator.
無溶劑型可固化組合物可更包含聚合抑製劑；丙二酸；3-胺基-1,2-丙二醇；矽烷類偶合劑；調平劑；氟類表面活性劑；或其組合。 The solvent-free curable composition may further include a polymerization inhibitor; malonic acid; 3-amino-1,2-propanediol; a silane coupling agent; a leveling agent; a fluorosurfactant; or a combination thereof.
另一實施例提供一種使用無溶劑型可固化組合物製造的固化膜。 Another embodiment provides a cured film produced using the solvent-free curable composition.
另一實施例提供一種包含固化膜的濾色器。 Another embodiment provides a color filter including a cured film.
另一實施例提供一種包含濾色器的顯示裝置。 Another embodiment provides a display device including a color filter.
本發明的其它實施例包含於以下詳細描述中。 Other embodiments of the invention are included in the following detailed description.
根據實施例的含有量子點的無溶劑型可固化組合物包含具有受控初級顆粒直徑及次級顆粒直徑的光漫射劑，且因此以降低的密度在短時間內再分散同時使量子點的散射效果最大化是可能的。因此，可實現包含使用組合物製造的固化膜的濾色器的高亮度及高色彩。 The quantum dot-containing solventless curable composition according to the embodiment includes a light diffusing agent having a controlled primary particle diameter and a secondary particle diameter, and thus it is possible to redisperse at a reduced density in a short time while maximizing the scattering effect of the quantum dots. Therefore, high brightness and high color of a color filter including a cured film produced using the composition can be realized.
圖1是繪示光漫射劑的初級顆粒直徑及次級顆粒直徑的示意圖。 FIG. 1 is a schematic diagram illustrating primary particle diameters and secondary particle diameters of a light diffusing agent.
圖2是實例5中使用的光漫射劑的結晶相的X射線分析的曲線圖。 FIG. 2 is a graph of X-ray analysis of the crystal phase of the light diffusing agent used in Example 5. FIG.
圖3是實例4中使用的光漫射劑的結晶相的X射線分析的曲線圖。 3 is a graph of X-ray analysis of the crystal phase of the light diffusing agent used in Example 4. FIG.
在下文中，詳細地描述本發明的實施例。然而，這些實施例是示例性的，本發明不限於此且本發明是由權利要求的範圍定義。 Hereinafter, embodiments of the present invention are described in detail. However, these embodiments are exemplary, the present invention is not limited thereto and the present invention is defined by the scope of the claims.
在本說明書中，當未另外提供具體定義時，「烷基」是指C1至C20烷基，「烯基」是指C2至C20烯基，「環烯基」是指C3至C20環烯基，「雜環烯基」是指C3至C20雜環烯基，「芳基」是指C6至C20芳基，「芳烷基」是指C6至C20芳烷基，「伸烷基」是指C1至C20伸烷基，「伸芳基」是指C6至C20伸芳基，「烷基伸芳基」是指C6至C20烷基伸芳基，「伸雜芳基」是指C3至C20伸雜芳基，且「伸烷氧基」是指C1至C20伸烷氧基。 In this specification, when no specific definition is provided, "alkyl" refers to C1 to C20 alkyl, "alkenyl" refers to C2 to C20 alkenyl, "cycloalkenyl" refers to C3 to C20 cycloalkenyl, "heterocycloalkenyl" refers to C3 to C20 heterocycloalkenyl, "aryl" refers to C6 to C20 aryl, "aralkyl" refers to C6 to C20 aralkyl, "alkylene" refers to C1 to C20 alkylene, "aryl" refers to C 6 to C20 aryl, "alkylaryl" refers to C6 to C20 alkylaryl, "heteroaryl" refers to C3 to C20 heteroaryl, and "alkylene" refers to C1 to C20 alkoxyl.
在本說明書中，當未另外提供具體定義時，「經取代」是指透過以下各物置換至少一個氫：鹵素原子(F、Cl、Br或I)、羥基、C1至C20烷氧基、硝基、氰基、胺基、伸胺基、疊氮基、甲脒基、肼基、伸肼基、羰基、胺甲醯基、硫醇基、酯基、醚基、羧基或其鹽、磺酸基或其鹽、磷酸或其鹽、C1至C20烷基、C2至C20烯基、C2至C20炔基、C6至C20芳基、C3至C20環烷基、C3至C20環烯基、C3至C20環炔基、C2至C20雜環烷基、C2至C20雜環烯基、C2至C20雜環炔基、C3至C20雜芳基或其組合。 In this specification, when no specific definition is otherwise provided, "substituted" refers to the replacement of at least one hydrogen by the following: halogen atom (F, Cl, Br or I), hydroxyl, C1 to C20 alkoxy, nitro, cyano, amino, amine, azido, carboxamidino, hydrazino, hydrazino, carbonyl, carbamido, thiol, ester, ether, carboxyl or its salt, sulfonic acid or its salt, phosphoric acid or its salt, C1 to C20 alkyl , C2 to C20 alkenyl, C2 to C20 alkynyl, C6 to C20 aryl, C3 to C20 cycloalkyl, C3 to C20 cycloalkenyl, C3 to C20 cycloalkynyl, C2 to C20 heterocycloalkyl, C2 to C20 heterocycloalkenyl, C2 to C20 heterocycloalkynyl, C3 to C20 heteroaryl, or combinations thereof.
在本說明書中，當未另外提供具體定義時，「雜」在化學式中可指被N、O、S以及P中的至少一個雜原子取代的一者。 In this specification, when no specific definition is otherwise provided, "hetero" in a chemical formula may refer to one substituted with at least one heteroatom of N, O, S, and P.
在本說明書中，當未另外提供具體定義時，「(甲基)丙烯酸酯」是指「丙烯酸酯」及「甲基丙烯酸酯」，且「(甲基)丙烯酸」是指「丙烯酸」及「甲基丙烯酸」。 In this specification, when no specific definition is provided otherwise, "(meth)acrylate" means "acrylate" and "methacrylate", and "(meth)acryl" means "acryl" and "methacryl".
在本說明書中，當未另外提供具體定義時，「組合」是指混合或共聚合。 In this specification, when no specific definition is otherwise provided, "combination" means mixing or copolymerization.
在本說明書中，除非另外提供具體定義，否則當未繪出化學鍵時，氫原子在推測給出的位置處鍵結。 In this specification, unless a specific definition is provided otherwise, when a chemical bond is not drawn, a hydrogen atom is bonded at a presumably given position.
在本說明書中，當未另外提供具體定義時，「*」指示連接相同或不同原子或化學式的點。 In this specification, when no specific definition is otherwise provided, "*" indicates a point of linking the same or different atoms or chemical formulas.
根據實施例的無溶劑型可固化組合物包含(A)量子點；(B)可聚合單體；以及(C)光漫射劑，且不包含溶劑，其中光漫射劑具有50奈米至200奈米的初級顆粒直徑及120奈米至250奈米的次級顆粒直徑。 A solventless curable composition according to an embodiment includes (A) quantum dots; (B) a polymerizable monomer; and (C) a light diffusing agent, and does not include a solvent, wherein the light diffusing agent has a primary particle diameter of 50 nm to 200 nm and a secondary particle diameter of 120 nm to 250 nm.
一般來說，可固化組合物由顏料或染料、光可聚合單體、黏合劑樹脂、光聚合起始劑、溶劑、添加劑等構成，但根據實施例的可固化組合物使用無機量子點(而不使用顏料或染料)來賦予色彩特性，且因此，由於使用根據實施例的無溶劑型可固化組合物製造的濾色器具有光致發光且相較使用常規可固化組合物製造的濾色器具有更高亮度、針對降低功耗的更高效率、更寬可視角度以及更高色彩再現性，且因此最終可促成具有以上性質的LCD的開發。 In general, curable compositions are composed of pigments or dyes, photopolymerizable monomers, binder resins, photopolymerization initiators, solvents, additives, etc., but the curable compositions according to the embodiments impart color characteristics using inorganic quantum dots instead of using pigments or dyes, and therefore, since the color filters manufactured using the solvent-free curable compositions according to the embodiments have photoluminescence and have higher brightness, higher efficiency for reducing power consumption, wider viewing angles, and higher color reproducibility than color filters manufactured using conventional curable compositions, and thus can finally promote into the development of LCDs with the above properties.
另一方面，根據實施例的可固化組合物為完全不包含溶劑的無溶劑型組合物。由於作為通常且廣泛用於含有量子點的可 固化組合物的可聚合單體的烯類單體(均包含單官能到多官能的乙烯基類單體、丙烯酸酯類單體、甲基丙烯酸酯類單體等)具有關於高度濃縮量子點的不足分散度，因此含有量子點的可固化組合物已被開發為包含大量(大於或等於50重量%(wt%))溶劑，但當溶劑的量增加時，存在噴墨可加工性劣化的問題。因此，為了滿足噴墨可加工性，增加了對無溶劑型可固化組合物的需求，且因此，實施例涉及滿足此增加需求的含有量子點的無溶劑型可固化組合物。換句話說，根據實施例的組合物包含量子點但完全不包含溶劑，且因此可防止噴墨可加工性的劣化，且同時實現具有極好的光效率的濾色器。 On the other hand, the curable composition according to the examples is a solvent-free composition containing no solvent at all. As a common and widely used quantum dot containing Vinyl monomers (all containing monofunctional to polyfunctional vinyl monomers, acrylate monomers, methacrylate monomers, etc.) of the polymerizable monomers of the cured composition have insufficient dispersibility with respect to highly concentrated quantum dots, so curable compositions containing quantum dots have been developed to contain a large amount (greater than or equal to 50 weight percent (wt %)) of solvent, but when the amount of solvent increases, there is a problem of deterioration in inkjet processability. Therefore, in order to satisfy inkjet processability, the demand for a solventless curable composition has increased, and thus, the embodiments relate to a solventless curable composition containing quantum dots satisfying this increased demand. In other words, the composition according to the embodiment includes quantum dots but does not include a solvent at all, and thus can prevent deterioration of inkjet processability while realizing a color filter having excellent light efficiency.
此外，對於含有量子點的無溶劑型可固化組合物，存儲穩定性以及噴墨特性也非常重要。為了實現噴墨特性，組合物需要小於或等於30cPs的極低黏度，但含有量子點的無溶劑型可固化組合物中包含的光漫射劑具有高密度且可易於沉澱，且因此對於長產品存儲穩定性具有負面影響。 In addition, storage stability and inkjet characteristics are also very important for solvent-free curable compositions containing quantum dots. In order to achieve inkjet characteristics, the composition requires an extremely low viscosity of less than or equal to 30 cPs, but the light diffusing agent contained in the quantum dot-containing solvent-free curable composition has a high density and can be easily precipitated, and thus has a negative impact on long-term product storage stability.
光漫射劑可起更高效地使用量子點的光致發光性質的作用，但尚未引進同時改進含有量子點的無溶劑型可固化組合物中的光漫射劑的光學特性及沉澱特性的技術。目前為止已知的改進技術不涉及光漫射劑而是涉及具有高極性的單體與透過量子點的表面改性的量子點之間的增加相容性。 Light diffusing agents can function to more efficiently use the photoluminescent properties of quantum dots, but techniques to simultaneously improve the optical properties and precipitation characteristics of light diffusing agents in solvent-free curable compositions containing quantum dots have not been introduced. The improvement techniques known so far do not involve light diffusing agents but rather the increased compatibility between monomers with high polarity and surface-modified quantum dots permeating the quantum dots.
根據實施例，連同量子點使用的光漫射劑限於具有各自在50奈米至200奈米及120奈米至250奈米的範圍內的初級顆粒 直徑及次級顆粒直徑以減小密度，且因此解決沉澱問題，也同時使量子點上的散射效果最大化(參見圖1)。 According to an embodiment, light diffusers used in conjunction with quantum dots are limited to having primary particles each in the range of 50 nm to 200 nm and 120 nm to 250 nm diameter and secondary particle diameter to reduce the density, and thus resolve the precipitation problem, while also maximizing the scattering effect on the quantum dots (see Figure 1).
具體來說，當光漫射劑限於具有在50奈米至200奈米的範圍內的初級顆粒直徑，且同時具有在120奈米至250奈米的範圍內的次級顆粒直徑時，可解決沉澱問題。換句話說，當限於具有在所述範圍內的初級顆粒直徑的光漫射劑使分散於可聚合單體中的無溶劑型組合物再分散時，組合物在短時間內快速再分散且因此減緩沉澱率。當光漫射劑具有小於50奈米的初級顆粒直徑時，可改進沉澱特性，但可使光吸收率及光轉換率劣化(不管控制次級顆粒直徑與否)。另外，當光漫射劑具有大於250奈米的次級顆粒直徑時，可改進光學特性，但顆粒尺寸太大，且因此加速沉澱率，且因而對光漫射劑顆粒表面的粗糙度具有負面影響。 In particular, when the light diffusing agent is limited to have a primary particle diameter in the range of 50nm to 200nm while having a secondary particle diameter in the range of 120nm to 250nm, the problem of precipitation can be solved. In other words, when a solvent-free composition dispersed in a polymerizable monomer is redispersed limited to a light-diffusing agent having a primary particle diameter within the range, the composition redisperses rapidly in a short time and thus slows down the sedimentation rate. When the light diffusing agent has a primary particle diameter of less than 50 nm, precipitation characteristics may be improved, but light absorption rate and light conversion rate may be deteriorated (regardless of controlling the secondary particle diameter or not). In addition, when the light diffusing agent has a secondary particle diameter greater than 250 nm, optical characteristics can be improved, but the particle size is too large, and thus accelerates the precipitation rate, and thus has a negative impact on the roughness of the surface of the light diffusing agent particles.
另外，當控制光漫射劑以具有在上述範圍內的初級顆粒直徑且同時具有在120奈米至250奈米的範圍內的次級顆粒直徑時，可減緩沉澱率且使光學特性且具體地藍光吸收率及藍光轉換率最大化。 In addition, when the light-diffusing agent is controlled to have a primary particle diameter in the above-mentioned range while having a secondary particle diameter in the range of 120 nm to 250 nm, the precipitation rate can be slowed down and the optical properties, specifically, the blue light absorption rate and the blue light conversion rate can be maximized.
在下文中，具體地描述每種組分。 Hereinafter, each component is specifically described.
(C)光漫射劑(C) light diffuser
如上文所描述，基於D50參考，光漫射劑具有50奈米至200奈米的初級顆粒直徑及120奈米至250奈米的次級顆粒直徑。舉例來說，光漫射劑可具有80奈米至180奈米的初級顆粒直徑及140奈米至230奈米的次級顆粒直徑。根據實施例的無溶劑型可固 化組合物可透過控制光漫射劑的初級顆粒直徑及次級顆粒直徑實現最優光學特性及沉澱特性。 As described above, based on the D50 reference, the light diffusing agent has a primary particle diameter of 50 nm to 200 nm and a secondary particle diameter of 120 nm to 250 nm. For example, the light diffusing agent may have a primary particle diameter of 80 nm to 180 nm and a secondary particle diameter of 140 nm to 230 nm. Solvent-free curable according to the embodiment The optimized composition can achieve optimal optical characteristics and precipitation characteristics by controlling the primary particle diameter and secondary particle diameter of the light diffusing agent.
次級顆粒直徑表示透過適當地分散具有初級顆粒直徑的光漫射劑粉末的成團顆粒的直徑，且可控制初級顆粒直徑及次級顆粒直徑以同時改進含有量子點的無溶劑型可固化組合物的光學特性及沉澱特性。 The secondary particle diameter means the diameter of agglomerated particles by properly dispersing the light-diffusing agent powder having the primary particle diameter, and the primary particle diameter and the secondary particle diameter can be controlled to simultaneously improve the optical characteristics and precipitation characteristics of the solventless curable composition containing quantum dots.
當光漫射劑具有各自在小於50奈米(例如80奈米)及小於120奈米(例如140奈米)的範圍內的初級顆粒直徑及次級顆粒直徑時，光學特性可能急劇劣化，且當光漫射劑具有各自在大於200奈米(例如180奈米)及大於250奈米(例如230奈米)的範圍內的初級顆粒直徑及次級顆粒直徑時，沉澱特性可能急劇劣化。 When the light-diffusing agent has a primary particle diameter and a secondary particle diameter each in a range of less than 50 nm (eg, 80 nm) and less than 120 nm (eg, 140 nm), the optical properties may be sharply deteriorated, and when the light-diffusing agent has a primary particle diameter and a secondary particle diameter each in a range of greater than 200 nm (eg, 180 nm) and greater than 250 nm (eg, 230 nm), the precipitation properties may be drastically deteriorated.
舉例來說，光漫射劑的次級顆粒直徑可比光漫射劑的初級顆粒直徑大1.5倍至2.5倍(例如1.5倍至兩倍)。當光漫射劑具有在所述範圍內的初級顆粒直徑及次級顆粒直徑時，可非常有效地改進光學特性及沉澱特性兩者。 For example, the secondary particle diameter of the light diffusing agent may be 1.5 to 2.5 times (eg, 1.5 to 2 times) larger than the primary particle diameter of the light diffusing agent. When the light-diffusing agent has a primary particle diameter and a secondary particle diameter within the range, it is very effective to improve both optical characteristics and precipitation characteristics.
另外，光漫射劑的不同結晶相且因此其不同密度可用於控制沉澱特性。 Additionally, different crystalline phases of the light diffuser, and thus their different densities, can be used to control the precipitation properties.
一般來說，用作光漫射劑的TiO2具有兩種不同結晶相。一種為銳鈦礦類型，且另一種為金紅石類型，且銳鈦礦類型具有3.8克/毫升(g/ml)的密度，且金紅石類型具有4.2克/毫升的相對較高密度。 Generally, TiO2 used as a light diffuser has two different crystalline phases. One is anatase type and the other is rutile type, and the anatase type has a density of 3.8 grams per milliliter (g/ml) and the rutile type has a relatively high density of 4.2 g/ml.
關於密度，結晶相具有折射率差異且因此散射強度差異，且具有更高折射率且因此更強散射強度的材料可不充當散射體。 With respect to density, the crystalline phase has a difference in refractive index and thus a difference in scattering intensity, and materials with a higher refractive index and therefore stronger scattering intensity may not act as scatterers.
換句話說，當銳鈦礦類型具有2.5的折射率，金紅石類型具有2.7的折射率且因此這兩者俱有相同顆粒分佈時，金紅石類型展現比散射體更高的吸收率但比銳鈦礦類型具有更高密度，且因此，金紅石類型的沉澱特性可比銳鈦礦類型的沉澱特性劣化更多。 In other words, when the anatase type has a refractive index of 2.5 and the rutile type has a refractive index of 2.7 and thus both have the same particle distribution, the rutile type exhibits a higher absorption rate than the scatterer but has a higher density than the anatase type, and thus the precipitation properties of the rutile type may be more degraded than those of the anatase type.
因此，當用作混合物以及當單獨使用時，具有前述初級顆粒直徑範圍及次級顆粒直徑範圍的銳鈦礦類型或金紅石類型可實現改進的沉澱特性。 Therefore, the anatase type or rutile type having the aforementioned primary particle diameter range and secondary particle diameter range can achieve improved precipitation characteristics when used as a mixture as well as when used alone.
舉例來說，光漫射劑可為金紅石型光漫射劑與銳鈦礦型光漫射劑的混合物。在本文中，可以1：3至3：1(例如1：1至1：3)的重量比使用金紅石型光漫射劑及銳鈦礦型光漫射劑。舉例來說，可以比金紅石型光漫射劑的量更多的量包含混合物中的銳鈦礦型光漫射劑。在本文中，可更有效地實現光學特性及沉澱特性兩者。 For example, the light-diffusing agent can be a mixture of rutile-type light-diffusing agent and anatase-type light-diffusing agent. Herein, the rutile-type light-diffusing agent and the anatase-type light-diffusing agent may be used in a weight ratio of 1:3 to 3:1 (for example, 1:1 to 1:3). For example, the anatase-type light-diffusing agent in the mixture may be included in a larger amount than the rutile-type light-diffusing agent. Herein, both optical properties and precipitation properties can be more effectively achieved.
舉例來說，光漫射劑可包含硫酸鋇(BaSO4)、碳酸鈣(CaCO3)、二氧化鈦(TiO2)、氧化鋯(ZrO2)或其組合。 For example, the light diffusing agent may include barium sulfate (BaSO 4 ), calcium carbonate (CaCO 3 ), titanium dioxide (TiO 2 ), zirconium oxide (ZrO 2 ), or combinations thereof.
舉例來說，光漫射劑可為二氧化鈦(TiO2)，例如金紅石型二氧化鈦、銳鈦礦型二氧化鈦或金紅石型二氧化鈦與銳鈦礦型二氧化鈦的混合物。二氧化鈦具有相對較高折射率，且因此可增加無溶劑型可固化組合物中的量子點的光致發光效率。 For example, the light diffusing agent can be titanium dioxide (TiO 2 ), such as rutile titanium dioxide, anatase titanium dioxide or a mixture of rutile titanium dioxide and anatase titanium dioxide. Titanium dioxide has a relatively high refractive index, and thus can increase the photoluminescence efficiency of quantum dots in the solvent-free curable composition.
光漫射劑可反射量子點中未吸收的光，且使所反射光在量子點中再次吸收。換句話說，光漫射劑可增加量子點中吸收的光 量，且因此增加無溶劑型可固化組合物中的量子點的光轉換率。換句話說，由於濾色器製程繼續，因此可防止藍光轉換率的劣化。 The light diffuser can reflect unabsorbed light in the quantum dots and cause the reflected light to be reabsorbed in the quantum dots. In other words, light diffusers increase the amount of light absorbed in the quantum dots amount, and thus increase the light conversion rate of the quantum dots in the solvent-free curable composition. In other words, since the color filter process continues, deterioration of blue light conversion rate can be prevented.
按無溶劑型可固化組合物的總量計，可包含1重量%至20重量%(例如5重量%至10重量%)的量的光漫射劑。按無溶劑型可固化組合物的總量計，當包含小於1重量%的量的光漫射劑時，由於光漫射劑的使用而難以預期光轉換效率改進效果，然而當包含大於20重量%的量的光漫射劑時，存在可沉澱量子點的可能性。 The light diffusing agent may be included in an amount of 1% to 20% by weight (eg, 5% to 10% by weight) based on the total amount of the solvent-free curable composition. When the light-diffusing agent is included in an amount of less than 1% by weight based on the total amount of the solvent-free curable composition, it is difficult to expect a light conversion efficiency improvement effect due to the use of the light-diffusing agent, but when the light-diffusing agent is included in an amount greater than 20% by weight, there is a possibility that quantum dots may be precipitated.
(A)量子點(A) quantum dots
量子點可吸收在360奈米至780奈米的波長范圍(例如400奈米至780奈米的波長范圍)內的光，且發射在450奈米至700奈米的波長范圍內的熒光。即，量子點可具有處於450奈米至700奈米的最大熒光發射波長(熒光λem)。 Quantum dots can absorb light within a wavelength range of 360 nm to 780 nm (eg, a wavelength range of 400 nm to 780 nm) and emit fluorescence within a wavelength range of 450 nm to 700 nm. That is, the quantum dots may have a maximum fluorescence emission wavelength (fluorescence λ em ) at 450 nm to 700 nm.
具體來說，量子點可為具有處於450奈米至580奈米的最大熒光發射波長(熒光λem)的量子點(例如綠光量子點)且具有處於580奈米至700奈米的最大熒光發射波長(熒光λem)的量子點(例如紅光量子點)或其組合。 Specifically, the quantum dots may be quantum dots (such as green light quantum dots) having a maximum fluorescence emission wavelength (fluorescence λ em ) between 450 nm and 580 nm and quantum dots (such as red light quantum dots) having a maximum fluorescence emission wavelength (fluorescence λ em ) between 580 nm and 700 nm, or a combination thereof.
綠光量子點可具有5奈米至10奈米的平均顆粒直徑，且紅光量子點可具有7奈米至15奈米的平均顆粒直徑。 The green light quantum dots may have an average particle diameter of 5 nm to 10 nm, and the red light quantum dots may have an average particle diameter of 7 nm to 15 nm.
量子點可具有20奈米至100奈米(例如20奈米至80奈米，例如40奈米至60奈米)的半高全寬(full width at half maximum，FWHM)。當量子點具有所述範圍的半高全寬(FWHM)時，由於 高色彩純度而在用作濾色器中的材料時增加色彩再現性。 The quantum dots may have a full width at half maximum (FWHM) of 20 nm to 100 nm (eg, 20 nm to 80 nm, eg, 40 nm to 60 nm). When the quantum dot has a full width at half maximum (FWHM) of the stated range, due to High color purity increases color reproducibility when used as a material in color filters.
量子點可為有機材料、無機材料或有機材料與無機材料的雜合物(混合物)。 Quantum dots can be organic materials, inorganic materials, or hybrids (mixtures) of organic and inorganic materials.
量子點可由核心及圍繞核心的殼層構成，且核心及殼層可各自獨立地具有由第II族至第IV族、第III族至第V族等構成的核心、核心/殼層、核心/第一殼層/第二殼層、合金、合金/殼層等的結構，但不限於此。 Quantum dots can be composed of a core and a shell surrounding the core, and the core and the shell can each independently have a structure of core, core/shell, core/first shell/second shell, alloy, alloy/shell, etc., composed of Group II to Group IV, Group III to Group V, etc., but are not limited thereto.
舉例來說，核心可至少包含選自以下的至少一種材料：CdS、CdSe、CdTe、ZnS、ZnSe、ZnTe、HgS、HgSe、HgTe、GaN、GaP、GaAs、InP、InAs以及其合金，但不必限於此。圍繞核心的殼層可至少包含選自以下的至少一種材料：CdSe、ZnSe、ZnS、ZnTe、CdTe、PbS、TiO、SrSe、HgSe以及其合金，但不必限於此。 For example, the core may at least include at least one material selected from the group consisting of CdS, CdSe, CdTe, ZnS, ZnSe, ZnTe, HgS, HgSe, HgTe, GaN, GaP, GaAs, InP, InAs, and alloys thereof, but not necessarily limited thereto. The shell surrounding the core may at least include at least one material selected from the group consisting of CdSe, ZnSe, ZnS, ZnTe, CdTe, PbS, TiO, SrSe, HgSe, and alloys thereof, but is not necessarily limited thereto.
量子點的結構不受特別限制，但具有核心/殼層結構的量子點可具有在1奈米至15奈米(例如5奈米至10奈米)的範圍內的包含殼層的整體尺寸(平均顆粒直徑)。 The structure of quantum dots is not particularly limited, but quantum dots having a core/shell structure may have an overall size including the shell (average particle diameter) in the range of 1 nm to 15 nm (eg, 5 nm to 10 nm).
為了改進量子點的穩定性及分散度，可透過取代殼層表面上的有機材料來使量子點穩定，且有機材料可包含硫醇類化合物、胺類化合物、膦氧化物類化合物、丙烯類化合物、矽類化合物等，但不限於此。 In order to improve the stability and dispersion of quantum dots, the quantum dots can be stabilized by substituting organic materials on the surface of the shell, and the organic materials can include thiol compounds, amine compounds, phosphine oxide compounds, propylene compounds, silicon compounds, etc., but are not limited thereto.
在實施例中，由於當前在全世界範圍內對環境的關注大大增加且對有毒材料的限制也已加強，因此使用量子效率(量子產率)極低但環保的不含鎘的發光材料(例如InP/ZnS核心/殼層型 量子點、InP/ZnSe/ZnS核心/第一殼層/第二殼層型量子點)而不使用具有鎘類核心的發光材料，但不必使用不含鎘的發光材料。 In the embodiment, since environmental concerns are greatly increased worldwide and restrictions on toxic materials have been strengthened at present, a cadmium-free light-emitting material (such as InP/ZnS core/shell type) with extremely low quantum efficiency (quantum yield) but environmentally friendly is used. Quantum dots, InP/ZnSe/ZnS core/first shell/second shell type quantum dots) do not use luminescent materials with cadmium-based cores, but do not need to use luminescent materials without cadmium.
另一方面，針對量子點的分散穩定性，根據實施例的無溶劑型可固化組合物可更包含分散劑。分散劑有助於例如無溶劑型可固化組合物中的量子點的光轉換材料的均一分散性，且可包含非離子、陰離子或陽離子分散劑。具體來說，分散劑可為聚伸烷基二醇或其酯、聚氧化伸烷基(polyoxy alkylene)、多元醇酯環氧烷加成產物、醇環氧烷加成產物、磺酸酯、磺酸鹽、羧酸酯、羧酸鹽、烷基醯胺環氧烷加成產物、烷基胺等，且其可單獨使用或以兩種或大於兩種的混合物形式使用。相對於例如量子點的光轉換材料的固體含量，可使用0.1重量%至100重量%(例如10重量%至20重量%)的量的分散劑。 On the other hand, for the dispersion stability of quantum dots, the solvent-free curable composition according to the embodiment may further include a dispersant. Dispersants contribute to the uniform dispersion of light converting materials such as quantum dots in the solventless curable composition, and may include nonionic, anionic, or cationic dispersants. Specifically, the dispersant may be polyalkylene glycol or its ester, polyoxyalkylene, polyol ester alkylene oxide addition product, alcohol alkylene oxide addition product, sulfonate, sulfonate, carboxylate, carboxylate, alkylamide alkylene oxide addition product, alkylamine, etc., and it may be used alone or in a mixture of two or more. The dispersant may be used in an amount of 0.1 wt % to 100 wt % (eg, 10 wt % to 20 wt %) relative to the solid content of the light conversion material such as quantum dots.
按無溶劑型可固化組合物的總量計，可包含1重量%至40重量%(例如3重量%至30重量%)的量的量子點。當表面改性量子點包含在範圍內時，可提高光轉換率，且不干擾圖案特性及顯影特性，以使得其可具有極好的可加工性。 The quantum dots may be included in an amount of 1% to 40% by weight, such as 3% to 30% by weight, based on the total amount of the solvent-free curable composition. When the surface-modified quantum dot is included in the range, the light conversion rate can be improved without interfering with pattern characteristics and development characteristics, so that it can have excellent processability.
(B)可聚合單體(B) Polymerizable monomer
可聚合單體可為包含至少一個乙烯係不飽和雙鍵的(甲基)丙烯酸的單官能酯或多官能酯。 The polymerizable monomer may be a monofunctional or polyfunctional ester of (meth)acrylic acid containing at least one ethylenically unsaturated double bond.
可聚合單體具有乙烯係不飽和雙鍵，且因此可在圖案形成製程中的曝光期間引起足夠聚合，且形成具有極好的耐熱性、耐光性以及耐化學性的圖案。 The polymerizable monomer has an ethylenically unsaturated double bond, and thus can cause sufficient polymerization during exposure in a pattern forming process, and form a pattern having excellent heat resistance, light resistance, and chemical resistance.
可聚合單體的具體實例可為乙二醇二(甲基)丙烯酸酯、二乙二醇二(甲基)丙烯酸酯、三乙二醇二(甲基)丙烯酸酯、丙二醇二(甲基)丙烯酸酯、新戊二醇二(甲基)丙烯酸酯、1,4-丁二醇二(甲基)丙烯酸酯、1,6-己二醇二(甲基)丙烯酸酯、雙酚A二(甲基)丙烯酸酯、季戊四醇二(甲基)丙烯酸酯、季戊四醇三(甲基)丙烯酸酯、季戊四醇四(甲基)丙烯酸酯、季戊四醇六(甲基)丙烯酸酯、二季戊四醇二(甲基)丙烯酸酯、二季戊四醇三(甲基)丙烯酸酯、二季戊四醇五(甲基)丙烯酸酯、二季戊四醇六(甲基)丙烯酸酯、雙酚A環氧基(甲基)丙烯酸酯、乙二醇單甲醚(甲基)丙烯酸酯、三羥甲基丙烷三(甲基)丙烯酸酯、磷酸三(甲基)丙烯醯氧基乙酯、酚醛環氧(甲基)丙烯酸酯等。 Specific examples of the polymerizable monomer may be ethylene glycol di(meth)acrylate, diethylene glycol di(meth)acrylate, triethylene glycol di(meth)acrylate, propylene glycol di(meth)acrylate, neopentyl glycol di(meth)acrylate, 1,4-butanediol di(meth)acrylate, 1,6-hexanediol di(meth)acrylate, bisphenol A di(meth)acrylate, pentaerythritol di(meth)acrylate, pentaerythritol tri(meth)acrylate, quaternary Pentaerythritol tetra(meth)acrylate, pentaerythritol hexa(meth)acrylate, dipentaerythritol di(meth)acrylate, dipentaerythritol tri(meth)acrylate, dipentaerythritol penta(meth)acrylate, dipentaerythritol hexa(meth)acrylate, bisphenol A epoxy(meth)acrylate, ethylene glycol monomethyl ether(meth)acrylate, trimethylolpropane tri(meth)acrylate, tri(meth)acryloxyethyl phosphate, novolac epoxy(meth)acrylate Acrylic etc.
可聚合單體的市售實例如下。單官能(甲基)丙烯酸酯可包含阿尼克斯(Aronix)M-101®、阿尼克斯M-111®、阿尼克斯M-114®(東亞合成化學工業株式會社(Toagosei Chemistry Industry Co.,Ltd.))；卡亞拉德(KAYARAD)TC-110S®、卡亞拉德TC-120S®(日本化藥株式會社(Nippon Kayaku Co.,Ltd.))；V-158®、V-2311®(大阪有機化學工業株式會社(Osaka Organic Chemical Ind.,Ltd.))等。雙官能(甲基)丙烯酸酯的實例可包含阿尼克斯M-210®、阿尼克斯M-240®、阿尼克斯M-6200®(東亞合成化學工業株式會社)；卡亞拉德HDDA®、卡亞拉德HX-220®、卡亞拉德R-604®(日本化藥株式會社)；V-260®、V-312®、V-335 HP®(大阪有機化學工業株式會社)等。三官能(甲基)丙烯酸酯的實例可包含阿尼克斯M-309®、 阿尼克斯M-400®、阿尼克斯M-405®、阿尼克斯M-450®、阿尼克斯M-7100®、阿尼克斯M-8030®、阿尼克斯M-8060®(東亞合成化學工業株式會社)；卡亞拉德TMPTA®、卡亞拉德DPCA-20®、卡亞拉德DPCA-30®、卡亞拉德DPCA-60®、卡亞拉德DPCA-120®(日本化藥株式會社)；V-295®、V-300®、V-360®、V-GPT®、V-3PA®、V-400®(大阪由岐化藥工業株式會社(Osaka Yuki Kayaku Kogyo Co.Ltd.))等。這些可單獨使用或以兩種或大於兩種的混合物形式使用。 Commercially available examples of polymerizable monomers are as follows. Monofunctional (meth)acrylates may include Aronix M- 101® , Anix M- 111® , Anix M- 114® (Toagosei Chemistry Industry Co., Ltd.); Kayarad (KAYARAD) TC- 110S® , Kayarad TC- 120S® (Nippon Kayaku (Nippon Kayaku Co., Ltd.)); V-158®, V-2311 ® (Osaka Organic Chemical Ind., Ltd.), etc. Examples of difunctional (meth)acrylates may include Anix M- 210® , Anix M- 240® , Anix M- 6200® (Toagosei Chemical Industry Co., Ltd.); Cayallade HDDA® , Cayallade HX- 220® , Cayallade R-604® (Nippon Kayaku Corporation); V- 260® , V- 312® , V-335 HP ® (Osaka Organic Chemical Industry Co., Ltd.), etc. Examples of trifunctional (meth)acrylates may include Anix M -309 ® , Anix M-400 ® , Anix M-405 ® , Anix M-450 ® , Anix M - 7100 ® , Anix M-8030 ® , Anix M-8060 ® (Toagosei Chemical Industry Co., Ltd.); Rad DPCA -20 ® , Cayalad DPCA-30 ® , Kayalad DPCA-60 ® , Kayalad DPCA - 120 ® (Nippon Kayaku Co., Ltd.); saka Yuki Kayaku Kogyo Co. Ltd.) ) etc. These may be used alone or in admixture of two or more.
此外，除可聚合單體之外，可進一步使用通常用於常規熱固或光可固化組合物中的單體。舉例來說，另外使用的單體可為氧雜環丁烷類化合物，例如雙[1-乙基(3-氧雜環丁烷基)]甲基醚。 In addition, monomers generally used in conventional thermosetting or photocurable compositions may be further used in addition to the polymerizable monomer. For example, additionally used monomers may be oxetane compounds such as bis[1-ethyl(3-oxetanyl)]methyl ether.
可聚合單體可用酸酐處理以改進顯影性。 Polymerizable monomers may be treated with anhydrides to improve developability.
按無溶劑型可固化組合物的總量計，可包含40重量%至80重量%(例如50重量%至80重量%)的量的可聚合單體。當可聚合單體包含在所述範圍內時，可製備能夠噴墨的具有黏度的的無溶劑型可固化組合物，且所製備的無溶劑型可固化組合物中的量子點可具有改進的分散性，從而改進光學特性。 The polymerizable monomer may be included in an amount of 40% to 80% by weight (eg, 50% to 80% by weight) based on the total amount of the solvent-free curable composition. When the polymerizable monomer is included within the range, a solvent-free curable composition having a viscosity capable of inkjet can be prepared, and quantum dots in the prepared solvent-free curable composition can have improved dispersibility, thereby improving optical characteristics.
另外，可聚合單體可具有220克/莫耳(g/mol)至1,000克/莫耳的重量平均分子量。當可聚合單體具有所述範圍內的分子量時，可有利於噴墨，這是因為其在不妨礙量子點的光學特性的情況下不會增加組合物的黏度。 In addition, the polymerizable monomer may have a weight average molecular weight of 220 grams per mole (g/mol) to 1,000 g/mol. When the polymerizable monomer has a molecular weight within the range, it may be advantageous for inkjet because it does not increase the viscosity of the composition without hindering the optical characteristics of the quantum dots.
聚合起始劑polymerization initiator
根據實施例的無溶劑型可固化組合物可更包含聚合起始劑，例如光聚合起始劑、熱聚合起始劑或其組合。 The solventless curable composition according to an embodiment may further include a polymerization initiator, such as a photopolymerization initiator, a thermal polymerization initiator, or a combination thereof.
光聚合起始劑為感光性樹脂組合物的常用起始劑，例如苯乙酮類化合物、苯甲酮類化合物、噻噸酮類化合物、安息香類化合物、三嗪類化合物、肟類化合物、胺基酮類化合物等，但不必限於此。 The photopolymerization initiator is a common initiator for photosensitive resin compositions, such as acetophenone compounds, benzophenone compounds, thioxanthone compounds, benzoin compounds, triazine compounds, oxime compounds, aminoketone compounds, etc., but not necessarily limited thereto.
苯乙酮類化合物的實例可為2,2'-二乙氧基苯乙酮、2,2'-二丁氧基苯乙酮、2-羥基-2-甲基苯丙酮、對第三丁基三氯苯乙酮、對第三丁基二氯苯乙酮、4-氯苯乙酮、2,2'-二氯-4-苯氧基苯乙酮、2-甲基-1-(4-(甲硫基)苯基)-2-嗎啉基丙烷-1-酮、2-苯甲基-2-二甲胺基-1-(4-嗎啉基苯基)-丁-1-酮等。 Examples of acetophenones may be 2,2'-diethoxyacetophenone, 2,2'-dibutoxyacetophenone, 2-hydroxy-2-methylpropiophenone, p-tert-butyltrichloroacetophenone, p-tert-butyldichloroacetophenone, 4-chloroacetophenone, 2,2'-dichloro-4-phenoxyacetophenone, 2-methyl-1-(4-(methylthio)phenyl)-2-morpholinopropan-1-one, 2-benzyl-2 -Dimethylamino-1-(4-morpholinylphenyl)-butan-1-one and the like.
二苯甲酮類化合物的實例可為二苯甲酮、苯甲醯基苯甲酸酯、苯甲醯基苯甲酸甲酯、4-苯基二苯甲酮、羥基二苯甲酮、丙烯酸化二苯甲酮、4,4'-雙(二甲胺基)二苯甲酮、4,4'-雙(二乙胺基)二苯甲酮、4,4'-二甲胺基二苯甲酮、4,4'-二氯二苯甲酮、3,3'-二甲基-2-甲氧基二苯甲酮等。 Examples of benzophenone compounds may be benzophenone, benzoyl benzoate, methyl benzoyl benzoate, 4-phenylbenzophenone, hydroxybenzophenone, acrylated benzophenone, 4,4'-bis(dimethylamino)benzophenone, 4,4'-bis(diethylamino)benzophenone, 4,4'-dimethylaminobenzophenone, 4,4'-dichlorobenzophenone, 3,3'- Dimethyl-2-methoxybenzophenone, etc.
噻噸酮類化合物的實例可為噻噸酮、2-甲基噻噸酮、異丙基噻噸酮、2,4-二乙基噻噸酮、2,4-二異丙基噻噸酮、2-氯噻噸酮等。 Examples of thioxanthone-based compounds may be thioxanthone, 2-methylthioxanthone, isopropylthioxanthone, 2,4-diethylthioxanthone, 2,4-diisopropylthioxanthone, 2-chlorothioxanthone, and the like.
安息香類化合物的實例可為安息香、安息香甲醚、安息香***、安息香異丙醚、安息香異丁醚、苯甲基二甲基縮酮等。 Examples of benzoin-based compounds may be benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzoin isobutyl ether, benzyl dimethyl ketal, and the like.
三嗪類化合物的實例可為2,4,6-三氯-均三嗪、2-苯基-4,6- 雙(三氯甲基)-均三嗪、2-(3',4'-二甲氧基苯乙烯基)-4,6-雙(三氯甲基)-均三嗪、2-(4'-甲氧基萘基)-4,6-雙(三氯甲基)-均三嗪、2-(對甲氧苯基)-4,6-雙(三氯甲基)-均三嗪、2-(對甲苯基)-4,6-雙(三氯甲基)-均三嗪、2-聯苯-4,6-雙(三氯甲基)-均三嗪、雙(三氯甲基)-6-苯乙烯基-均三嗪、2-(萘酚-基)-4,6-雙(三氯甲基)-均三嗪、2-(4-甲氧基萘酚-基)-4,6-雙(三氯甲基)-均三嗪、2-4-雙(三氯甲基)-6-胡椒基(piperonyl)-均三嗪、2-4-雙(三氯甲基)-6-(4-甲氧基苯乙烯基)-均三嗪等。 Examples of triazine compounds can be 2,4,6-trichloro-s-triazine, 2-phenyl-4,6- Bis(trichloromethyl)-s-triazine, 2-(3',4'-dimethoxystyryl)-4,6-bis(trichloromethyl)-s-triazine, 2-(4'-methoxynaphthyl)-4,6-bis(trichloromethyl)-s-triazine, 2-(p-methoxyphenyl)-4,6-bis(trichloromethyl)-s-triazine, 2-(p-tolyl)-4,6-bis(trichloromethyl)-s-triazine, 2-biphenyl -4,6-bis(trichloromethyl)-s-triazine, bis(trichloromethyl)-6-styryl-s-triazine, 2-(naphthol-yl)-4,6-bis(trichloromethyl)-s-triazine, 2-(4-methoxynaphthol-yl)-4,6-bis(trichloromethyl)-s-triazine, 2-4-bis(trichloromethyl)-6-piperonyl-s-triazine, 2-4-bis(trichloromethyl)- 6-(4-methoxystyryl)-s-triazine, etc.
肟類化合物的實例可為O-醯基肟類化合物(O-acyloxime-based compound)、2-(O-苯甲醯基肟)-1-[4-(苯硫基)苯基]-1,2-辛二酮、1-(O-乙醯基肟)-1-[9-乙基-6-(2-甲基苯甲醯基)-9H-咔唑-3-基]乙酮、O-乙氧羰基-α-氧胺基-1-苯基丙-1-酮等。O-醯基肟類化合物的具體實施例可為1,2-辛二酮、2-二甲胺基-2-(4-甲基苯甲基)-1-(4-嗎啉-4-基-苯基)-丁-1-酮、1-(4-苯硫基苯基)-丁烷-1,2-二酮2-肟-O-苯甲酸酯、1-(4-苯硫基苯基)-辛烷-1,2-二酮2-肟-O-苯甲酸酯、1-(4-苯硫基苯基)-辛-1-酮肟-O-乙酸酯、1-(4-苯硫基苯基)-丁-1-酮肟-O-乙酸酯等。 Examples of oxime compounds can be O-acyl oxime-based compound (O-acyloxime-based compound), 2-(O-benzoyl oxime)-1-[4-(phenylthio)phenyl]-1,2-octanedione, 1-(O-acetyl oxime)-1-[9-ethyl-6-(2-methylbenzoyl)-9H-carbazol-3-yl]ethanone, O-ethoxycarbonyl- α-Oxyamino-1-phenylpropan-1-one, etc. Specific examples of O-acyl oxime compounds can be 1,2-octanedione, 2-dimethylamino-2-(4-methylbenzyl)-1-(4-morpholin-4-yl-phenyl)-butan-1-one, 1-(4-phenylthiophenyl)-butane-1,2-dione 2-oxime-O-benzoate, 1-(4-phenylthiophenyl)-octane-1,2-dione 2-oxime-O-benzoate, 1- (4-Phenylthiophenyl)-oct-1-one oxime-O-acetate, 1-(4-phenylthiophenyl)-butan-1-one oxime-O-acetate, etc.
胺基酮類化合物的實例可為2-苯甲基-2-二甲胺基-1-(4-嗎啉基苯基)-丁酮-1等。 Examples of aminoketone compounds may be 2-benzyl-2-dimethylamino-1-(4-morpholinophenyl)-butanone-1 and the like.
除所述化合物之外，光聚合起始劑還可更包含咔唑類化合物、二酮類化合物、硼酸鋶類化合物(sulfonium borate-based compound)、重氮類化合物、咪唑類化合物、聯咪唑類化合物等。 In addition to the aforementioned compounds, the photopolymerization initiator may further include carbazole compounds, diketone compounds, sulfonium borate-based compounds, diazo compounds, imidazole compounds, biimidazole compounds, and the like.
光聚合起始劑可與感光劑一起使用，所述感光劑能夠透過吸收光且變成激發態且接著轉移其能量而引起化學反應。 The photopolymerization initiator may be used together with a sensitizer capable of causing a chemical reaction by absorbing light and becoming an excited state and then transferring its energy.
感光劑的實例可為四乙二醇雙-3-巰基丙酸酯、季戊四醇四-3-巰基丙酸酯、二季戊四醇四-3-巰基丙酸酯等。 Examples of the sensitizer may be tetraethylene glycol bis-3-mercaptopropionate, pentaerythritol tetra-3-mercaptopropionate, dipentaerythritol tetra-3-mercaptopropionate, and the like.
熱聚合起始劑的實例可為過氧化物，具體地為過氧化苯甲醯、過氧化二苯甲醯、過氧化月桂醯(lauryl peroxide)、過氧化二月桂醯(dilauryl peroxide)、過氧化二第三丁基(di-tert-butyl peroxide)、過氧化環己烷、過氧化甲基乙基酮、氫過氧化物(例如，第三丁基氫過氧化物(tert-butyl hydroperoxide)、氫過氧化枯烯)、過氧化二碳酸二環己酯(dicyclohexyl peroxydicarbonate)、2,2-偶氮-雙(異丁腈)、過苯甲酸第三丁酯以及例如2,2'-偶氮雙-2-甲基丙腈(2,2'-azobis-2-methylpropinonitrile)的類似物，但不必限於此且可使用所屬領域中熟知的過氧化物中的任一種。 Examples of the thermal polymerization initiator may be peroxides, specifically benzoyl peroxide, dibenzoyl peroxide, lauryl peroxide, dilauryl peroxide, di-tert-butyl peroxide, cyclohexane peroxide, methyl ethyl ketone peroxide, hydroperoxides (for example, tert-butyl hydroperoxide) oxide), cumene hydroperoxide), dicyclohexyl peroxydicarbonate, 2,2-azo-bis(isobutyronitrile), tert-butyl perbenzoate, and analogs such as 2,2'-azobis-2-methylpropinonitrile (2,2'-azobis-2-methylpropinonitrile), but not necessarily limited thereto and any one of peroxides well known in the art may be used.
按無溶劑型可固化組合物的總量計，可包含0.1重量%至5重量%(例如1重量%至4重量%)的量的聚合起始劑。當聚合起始劑包含在所述範圍中時，有可能由於在曝光或熱固化期間充分固化而獲得極好的可靠性，且有可能防止由於非反應起始劑而使透射比劣化，從而防止量子點的光學特性劣化。 The polymerization initiator may be included in an amount of 0.1% to 5% by weight (for example, 1% to 4% by weight) based on the total amount of the non-solvent type curable composition. When the polymerization initiator is included in the range, it is possible to obtain excellent reliability due to sufficient curing during exposure or thermal curing, and it is possible to prevent deterioration of transmittance due to non-reaction initiator, thereby preventing deterioration of optical characteristics of quantum dots.
其它添加劑other additives
針對量子點的穩定性及分散改進，根據實施例的無溶劑型可固化組合物可更包含聚合抑製劑。 For improving the stability and dispersion of quantum dots, the solvent-free curable composition according to the embodiments may further include a polymerization inhibitor.
聚合抑製劑可包含對苯二酚類化合物、兒茶酚類化合物 或其組合，但不必限於此。當根據實施例的無溶劑型可固化組合物更包含對苯二酚類化合物、兒茶酚類化合物或其組合時，可防止在塗佈無溶劑型可固化組合物之後的曝光期間的室溫交聯。 Polymerization inhibitors may contain hydroquinones, catechols or a combination thereof, but not necessarily limited thereto. When the solventless curable composition according to the embodiment further includes a hydroquinone compound, a catechol compound, or a combination thereof, room temperature crosslinking during exposure after coating the solventless curable composition may be prevented.
舉例來說，對苯二酚類化合物、兒茶酚類化合物或其組合可為對苯二酚、甲基對苯二酚、甲氧基對苯二酚、第三丁基對苯二酚、2,5-二-第三丁基對苯二酚、2,5-雙(1,1-二甲基丁基)對苯二酚、2,5-雙(1,1,3,3-四甲基丁基)對苯二酚、兒茶酚、第三丁基兒茶酚、4-甲氧基苯酚、鄰苯三酚、2,6-二-第三丁基-4-甲基苯酚、2-萘酚、三(N-羥基-N-伸硝基苯基胺-O,O')鋁或其組合，但不必限於此。 For example, the hydroquinone compound, the catechol compound, or a combination thereof can be hydroquinone, methylhydroquinone, methoxyhydroquinone, tert-butylhydroquinone, 2,5-di-tert-butylhydroquinone, 2,5-bis(1,1-dimethylbutyl)hydroquinone, 2,5-bis(1,1,3,3-tetramethylbutyl)hydroquinone, catechol, tert-butylcatechol, 4-methoxyphenol, Glycinol, 2,6-di-tert-butyl-4-methylphenol, 2-naphthol, tris(N-hydroxy-N-nitrophenylamine-O,O')aluminum or combinations thereof, but not necessarily limited thereto.
對苯二酚類化合物、兒茶酚類化合物或其組合可以分散液(dispersion)形式使用。按無溶劑型可固化組合物的總量計，可包含0.001重量%至3重量%(例如0.1重量%至2重量%)的量的呈分散液形式的聚合抑製劑。當聚合抑製劑包含在所述範圍中時，可解決室溫下的時間推移問題且同時可防止靈敏度劣化及表面分層現象。 The hydroquinone compound, the catechol compound, or a combination thereof may be used in the form of a dispersion. The polymerization inhibitor in the form of a dispersion liquid may be included in an amount of 0.001% to 3% by weight (for example, 0.1% to 2% by weight) based on the total amount of the non-solvent type curable composition. When the polymerization inhibitor is included in the range, the problem of time lapse at room temperature can be solved and at the same time, sensitivity deterioration and surface delamination phenomenon can be prevented.
另外，根據實施例的無溶劑型可固化組合物可更包含丙二酸；3-胺基-1,2-丙二醇；矽烷類偶合劑；調平劑；氟類表面活性劑；或其組合以改進耐熱性及可靠性。 In addition, the solventless curable composition according to the embodiment may further include malonic acid; 3-amino-1,2-propanediol; a silane coupling agent; a leveling agent; a fluorosurfactant; or a combination thereof to improve heat resistance and reliability.
舉例來說，根據實施例的無溶劑型可固化組合物可更包含具有反應性取代基(例如乙烯基、羧基、甲基丙烯醯氧基、異氰酸酯基團、環氧基等)的矽烷類偶合劑以改進與基板的緊密接觸性質。 For example, the solventless curable composition according to the embodiment may further include a silane-based coupling agent with reactive substituents (such as vinyl, carboxyl, methacryloxy, isocyanate, epoxy, etc.) to improve the close contact property with the substrate.
矽烷類偶合劑的實例可為三甲氧基甲矽烷基苯甲酸、γ-甲基丙烯基丙氧基三甲氧基矽烷、乙烯基三乙醯氧基矽烷、乙烯基三甲氧基矽烷、γ-異氰酸酯丙基三乙氧基矽烷、γ-縮水甘油氧基丙基三甲氧基矽烷、β-環氧環己基)乙基三甲氧基矽烷等，且這些可單獨使用或以兩種或大於兩種的混合物形式使用。 Examples of silane-based coupling agents may be trimethoxysilylbenzoic acid, γ-methacrylpropoxytrimethoxysilane, vinyltriacetoxysilane, vinyltrimethoxysilane, γ-isocyanatopropyltriethoxysilane, γ-glycidoxypropyltrimethoxysilane, β-epoxycyclohexyl)ethyltrimethoxysilane, etc., and these may be used alone or as a mixture of two or more.
按100重量份無溶劑型可固化組合物計，可使用0.01重量份至10重量份的量的矽烷類偶合劑。當矽烷類偶合劑包含在所述範圍內時，緊密接觸性質、存儲能力等得以改進。 Based on 100 parts by weight of the solvent-free curable composition, the silane coupling agent may be used in an amount of 0.01 to 10 parts by weight. When the silane-based coupling agent is contained within the range, close contact properties, storage ability, and the like are improved.
另外，無溶劑型可固化組合物可更包含表面活性劑，例如視需要的氟類表面活性劑以改進塗佈性質且抑制斑點產生，即，改進調平性能。 In addition, the solventless curable composition may further include a surfactant, such as a fluorine-based surfactant, if necessary, to improve coating properties and suppress generation of spots, that is, to improve leveling performance.
氟類表面活性劑可具有4,000克/莫耳至10,000克/莫耳，且具體地6,000克/莫耳至10,000克/莫耳的低重量平均分子量。另外，氟類表面活性劑可具有18毫牛/米(mN/m)至23毫牛/米的表面張力(用0.1%聚乙二醇單甲醚乙酸酯(polyethylene glycol monomethylether acetate，PGMEA)溶液測量)。當氟類表面活性劑具有所述範圍內的重量平均分子量及表面張力時，可進一步改進調平性能且可在應用作為高速塗佈的狹縫塗佈時提供極好的特性，這是由於可透過防止在高速塗佈期間產生斑點且抑制蒸氣產生來較少地產生膜缺陷。 The fluorosurfactant may have a low weight average molecular weight of 4,000 g/mol to 10,000 g/mol, and specifically 6,000 g/mol to 10,000 g/mol. In addition, the fluorosurfactant may have a surface tension of 18mN/m to 23mN/m (measured with a 0.1% polyethylene glycol monomethylether acetate (PGMEA) solution). When the fluorine-based surfactant has a weight-average molecular weight and surface tension within the range, leveling performance can be further improved and excellent characteristics can be provided when applying slit coating as high-speed coating, since film defects can be less generated by preventing occurrence of spots during high-speed coating and suppressing vapor generation.
氟類表面活性劑的實例可為BM-1000®及BM-1100®(BM化學公司(BM Chemie Inc.))；麥格菲斯(MEGAFACE)F 142D®、 麥格菲斯F 172®、麥格菲斯F 173®以及麥格菲斯F 183®(大日本油墨化學工業株式會社(Dainippon Ink Kagaku Kogyo Co.,Ltd.))；福勒拉德(FULORAD)FC-135®、福勒拉德FC-170C®、福勒拉德FC-430®以及福勒拉德FC-431®(住友3M株式會社(Sumitomo 3M Co.,Ltd.))；索龍(SURFLON)S-112®、索龍S-113®、索龍S-131®、索龍S-141®以及索龍S-145®(旭硝子株式會社(ASAHI Glass Co.,Ltd.))；以及SH-28PA®、SH-190®、SH-193®、SZ-6032®以及SF-8428®等(東麗矽氧烷株式會社(Toray Silicone Co.,Ltd.))；大日本油墨化學工業株式會社(DIC Co.,Ltd)的F-482、F-484、F-478、F-554等。 An example of a fluorosurfactant may be BM-1000®and BM-1100®(BM Chemie Inc.); MEGAFACE F 142D®, McGuires F 172®, McGulfis F 173®and the McGulfis F 183®(Dainippon Ink Kagaku Kogyo Co., Ltd.); FULORAD FC-135®, Fullerard FC-170C®, Fullerard FC-430®and Fowlerard FC-431®(Sumitomo 3M Co., Ltd.); SURFLON S-112®, Thrawn S-113®, Thrawn S-131®, Thrawn S-141®and Thrawn S-145®(ASAHI Glass Co., Ltd.); and SH-28PA®、SH-190®、SH-193®、SZ-6032®and SF-8428®etc. (Toray Silicone Co., Ltd.); F-482, F-484, F-478, F-554 of DIC Co., Ltd., etc.
另外，除氟類表面活性劑以外，根據實施例的無溶劑型可固化組合物還可包含矽氧烷類表面活性劑。矽氧烷類表面活性劑的具體實例可為東芝矽氧烷株式會社(Toshiba silicone Co.,Ltd.)的TSF400、TSF401、TSF410、TSF4440等，但不限於此。 In addition, the solventless curable composition according to the embodiment may further include a silicone-based surfactant in addition to the fluorine-based surfactant. Specific examples of silicone-based surfactants include TSF400, TSF401, TSF410, and TSF4440 from Toshiba silicone Co., Ltd., but are not limited thereto.
按100重量份無溶劑型可固化組合物計，可包含0.01重量份至5重量份(例如0.1重量份至2重量份)的量的表面活性劑。當表面活性劑包含在所述範圍內時，在所噴塗組合物中較少產生異物。 The surfactant may be included in an amount of 0.01 to 5 parts by weight (eg, 0.1 to 2 parts by weight) based on 100 parts by weight of the solventless curable composition. When the surfactant is contained within the range, foreign matter is less generated in the sprayed composition.
另外，除非性質劣化，否則根據實施例的無溶劑型可固化組合物可更包含預定量的其它添加劑，例如抗氧化劑、穩定劑等。 In addition, the solventless curable composition according to the embodiment may further include predetermined amounts of other additives, such as antioxidants, stabilizers, etc., unless properties are deteriorated.
另一實施例提供一種使用前述無溶劑型可固化組合物製造的固化膜、包含固化膜的濾色器以及包含濾色器的顯示裝置。 Another embodiment provides a cured film manufactured using the foregoing solventless curable composition, a color filter including the cured film, and a display device including the color filter.
製造固化層的方法中的一種可包含：使用噴墨噴塗方法在基板上塗佈前述無溶劑型可固化組合物以形成圖案(S1)；以及固化圖案(S2)。 One of the methods of manufacturing a cured layer may include: coating the foregoing solventless curable composition on a substrate to form a pattern using an inkjet spray coating method (S1); and curing the pattern (S2).
(S1)圖案的形成 (S1) Pattern formation
無溶劑型可固化組合物可用噴墨噴塗方法在基板上理想地塗佈為0.5微米至20微米。噴墨噴塗方法可透過根據每一噴嘴噴塗單一色彩且因此根據所需色彩數量重複噴塗多次來形成圖案，但圖案可透過經每一噴墨噴嘴同時噴塗所需色彩數量來形成，以減少製程。 The solventless curable composition can be desirably applied to a substrate from 0.5 microns to 20 microns by inkjet spraying methods. The inkjet spraying method can form a pattern by spraying a single color according to each nozzle and thus repeating the spraying multiple times according to the required number of colors, but the pattern can be formed by simultaneously spraying the required number of colors through each inkjet nozzle to reduce the process.
(S2)固化 (S2) curing
固化所獲得的圖案以獲得像素。在本文中，固化方法可為熱固化或光固化製程。熱固化製程可在大於100℃或等於100℃下，理想地在100℃至300℃的範圍內，且更理想地在160℃至250℃的範圍內進行。光固化製程可包含輻射光化射線，例如190奈米至450奈米(例如200奈米至500奈米)的紫外線。透過使用例如具有低壓、高壓或超高壓的汞燈、金屬鹵化物燈、氬氣激光器等的光源進行輻射。還可視需要使用X射線、電子束等。 The obtained pattern is cured to obtain pixels. Herein, the curing method may be thermal curing or photo-curing process. The thermal curing process may be performed at greater than or equal to 100°C, desirably in the range of 100°C to 300°C, and more desirably in the range of 160°C to 250°C. The photocuring process may include irradiating actinic rays, such as ultraviolet light at 190 nm to 450 nm (eg, 200 nm to 500 nm). Irradiation is performed by using a light source such as a mercury lamp with low, high or extra high pressure, a metal halide lamp, an argon laser, or the like. X-rays, electron beams, etc. may also be used as needed.
在下文中，參考實例更詳細地說明本發明。然而，這些實例在任何意義上都不應解釋為限製本發明的範圍。 Hereinafter, the present invention is explained in more detail with reference to examples. However, these examples should not be construed as limiting the scope of the invention in any sense.
(無溶劑型可固化組合物的製備)(Preparation of solvent-free curable composition)
實例1至實例9以及比較例1及比較例7Example 1 to Example 9 and Comparative Example 1 and Comparative Example 7
以下組分用於製備分別具有表1及表2中所示的組合物 的根據實例1至實例9以及比較例1及比較例2的無溶劑型可固化組合物。 The following components were used to prepare the compositions shown in Table 1 and Table 2 respectively The solventless curable compositions according to Examples 1 to 9 and Comparative Example 1 and Comparative Example 2.
具體來說，在燒瓶中分散於乙酸環己酯中的量子點分散液(26重量%至27重量%的固體含量)在80℃的氮氣氛圍下攪拌20小時，以獲得表面改性量子點分散液。將所得產物冷卻至室溫，且將量子點分散液添加到環己烷並接著離心。經過離心，從環己烷中分離所沉澱量子點粉末。將上部部分中的澄清溶液扔掉並丟棄，且沉澱物在真空烘箱中乾燥24小時。以預定濃度將量子點粉末(36g)取樣至HDDA(1,6-己二醇二丙烯酸酯)單體(56g)，且接著攪拌12小時以獲得量子點分散液。 Specifically, a quantum dot dispersion (26 wt% to 27 wt% solid content) dispersed in cyclohexyl acetate in a flask was stirred under a nitrogen atmosphere at 80° C. for 20 hours to obtain a surface-modified quantum dot dispersion. The resulting product was cooled to room temperature, and the quantum dot dispersion liquid was added to cyclohexane and then centrifuged. The precipitated quantum dot powder was separated from cyclohexane by centrifugation. The clear solution in the upper portion was discarded and discarded, and the precipitate was dried in a vacuum oven for 24 hours. Quantum dot powder (36 g) was sampled to HDDA (1,6-hexanediol diacrylate) monomer (56 g) at a predetermined concentration, and then stirred for 12 hours to obtain a quantum dot dispersion.
隨後，稱取量子點分散液，將HDDA單體(56g)添加至其中，且接著攪拌5小時，將聚合起始劑添加至其中，且將光漫射劑添加至其中。攪拌全部分散液1小時以製備無溶劑型可固化組合物。 Subsequently, the quantum dot dispersion liquid was weighed, HDDA monomer (56 g) was added thereto, and then stirred for 5 hours, a polymerization initiator was added thereto, and a light diffusing agent was added thereto. The entire dispersion was stirred for 1 hour to prepare a solventless curable composition.
(A)量子點 (A) quantum dots
InP/ZnSe/ZnS量子點粉末 InP/ZnSe/ZnS quantum dot powder
(B)可聚合單體 (B) Polymerizable monomer
1,6-己二醇二丙烯酸酯(HDDA，美源特殊化學有限公司(Miwon Specialty Chemical Co.,Ltd.)) 1,6-Hexanediol diacrylate (HDDA, Miwon Specialty Chemical Co., Ltd.)
(C)光漫射劑 (C) light diffuser
(C-1)金紅石型二氧化鈦分散液(HDDA中的40重量%的TiO2固體含量，初級顆粒直徑：50奈米，次級顆粒直徑：120 奈米，NJ 660，三國株式會社(Mikuni Corp.)) (C-1) Rutile-type titanium dioxide dispersion (40% by weight of TiO solid content in HDDA, primary particle diameter: 50 nm, secondary particle diameter: 120 nm, NJ 660, Mikuni Corp.)
(C-2)金紅石型二氧化鈦分散液(HDDA中的40重量%的TiO2固體含量，初級顆粒直徑：80奈米，次級顆粒直徑：140奈米，NJ 672，三國株式會社) (C-2) Rutile-type titanium dioxide dispersion (40% by weight of TiO solid content in HDDA, primary particle diameter: 80 nm, secondary particle diameter: 140 nm, NJ 672, Mikuni Co., Ltd.)
(C-3)金紅石型二氧化鈦分散液(HDDA中的40重量%的TiO2固體含量，初級顆粒直徑：100奈米，次級顆粒直徑：150奈米，NJ 661，三國株式會社) (C-3) Rutile-type titanium dioxide dispersion (40% by weight of TiO solid content in HDDA, primary particle diameter: 100 nm, secondary particle diameter: 150 nm, NJ 661, Mikuni Co., Ltd.)
(C-4)銳鈦礦型二氧化鈦分散液(HDDA中的50重量%的TiO2固體含量，初級顆粒直徑：160奈米，次級顆粒直徑：170奈米，A16，伊里多斯有限公司(Iridos Co.,Ltd.)) (C-4) Anatase-type titanium dioxide dispersion (50% by weight of TiO solid content in HDDA, primary particle diameter: 160 nm, secondary particle diameter: 170 nm, A16, Iridos Co., Ltd.)
(C-5)金紅石型二氧化鈦分散液(HDDA中的50重量%的TiO2固體含量，初級顆粒直徑：170奈米，次級顆粒直徑：185奈米，白色NS-13H，伊里多斯有限公司) (C-5) Rutile-type titanium dioxide dispersion (50% by weight of TiO solid content in HDDA, primary particle diameter: 170 nm, secondary particle diameter: 185 nm, white NS-13H, Iridos Co., Ltd.)
(C-6)金紅石型二氧化鈦分散液(HDDA中的50重量%的TiO2固體含量，初級顆粒直徑：210奈米，次級顆粒直徑：210奈米，TiO2-7，伊里多斯有限公司) (C-6) Rutile-type titanium dioxide dispersion (50% by weight of TiO2 solid content in HDDA, primary particle diameter: 210 nm, secondary particle diameter: 210 nm, TiO2-7, Iridos Co., Ltd.)
(C-7)金紅石型二氧化鈦分散液(HDDA中的50重量%的TiO2固體含量，初級顆粒直徑：250奈米，次級顆粒直徑：230奈米，TiO2-9，伊里多斯有限公司) (C-7) Rutile-type titanium dioxide dispersion (50% by weight of TiO2 solid content in HDDA, primary particle diameter: 250 nm, secondary particle diameter: 230 nm, TiO2-9, Iridos Co., Ltd.)
(C-8)金紅石型二氧化鈦分散液(HDDA中的50重量%的TiO2固體含量，初級顆粒直徑：270奈米，次級顆粒直徑：280奈米，TiO2-22，伊里多斯有限公司) (C-8) Rutile-type titanium dioxide dispersion (50% by weight of TiO2 solid content in HDDA, primary particle diameter: 270 nm, secondary particle diameter: 280 nm, TiO2-22, Iridos Co., Ltd.)
聚合起始劑 polymerization initiator
乙基(2,4,6-三甲基苯甲醯基)苯基伸膦酸酯(Ethyl(2,4,6-trimethylbenzoyl)phenylphosphinate)(IGM樹脂) Ethyl(2,4,6-trimethylbenzoyl)phenylphosphinate (IGM resin)
其它添加劑 other additives
氟類表面活性劑(F-554，大日本油墨化學工業株式會社) Fluorinated surfactant (F-554, Dainippon Ink & Chemicals Co., Ltd.)
評估1：光學特性的評估Evaluation 1: Evaluation of Optical Properties
透過使用旋轉塗佈機(由三笠株式會社(Mikasa Co.,Ltd.)制得的Opticoat MS-A150，800轉/分鐘(rpm)，5秒)將根據實例1至實例9以及比較例1及比較例2的組合物在玻璃基板上分別塗佈為15微米厚，且接著透過使用395奈米的UV曝光器在氮氣氛圍下暴露於具有5000毫焦(mJ)的光。隨後，在積分球設備(QE-2100，大塚電子株式會社(Otsuka Electronics Co.,Ltd.))上載入2公分×2公分的單層膜標本以測量藍光轉換率，且測量結果顯示於表3中。 The compositions according to Examples 1 to 9 and Comparative Examples 1 and 2 were respectively coated to a thickness of 15 microns on a glass substrate by using a spin coater (Opticoat MS-A150 manufactured by Mikasa Co., Ltd. (Mikasa Co., Ltd.), 800 revolutions per minute (rpm), 5 seconds), and then exposed to light having 5000 millijoules (mJ) under a nitrogen atmosphere by using a UV exposer of 395 nm. Subsequently, a 2 cm × 2 cm monolayer film specimen was loaded on an integrating sphere device (QE-2100, Otsuka Electronics Co., Ltd.) to measure the blue light conversion rate, and the measurement results are shown in Table 3.
評估2：沉澱的評估Assessment 2: Assessment of Precipitation
允許20毫升的根據實例1至實例9以及比較例1及比較例2的每種組合物在室溫下靜置10天。在本文中，沉澱物由於 TiO2的顆粒尺寸而自然出現，相對於參考(實例6)的組合物的沉澱程度獲得為%，且結果顯示於表3中。圖2及圖3分別是實例5及實例4中使用的光漫射劑的結晶相的X射線分析的曲線圖。 20 ml of each composition according to Examples 1 to 9 and Comparative Examples 1 and 2 were allowed to stand at room temperature for 10 days. Herein, the precipitation occurred naturally due to the particle size of the TiO 2 , the degree of precipitation was obtained in % relative to the composition of the reference (Example 6), and the results are shown in Table 3. 2 and 3 are graphs of X-ray analysis of the crystal phase of the light diffusing agent used in Example 5 and Example 4, respectively.
參考表3，當光漫射劑的初級顆粒直徑及次級顆粒直徑控制在特定範圍內時，與使用不具有所述範圍內的初級顆粒直徑及次級顆粒直徑的光漫射劑的情況相比，光學特性及沉澱特性都得以改進。另外，當包含具有在受控範圍內的顆粒直徑且因此具有金紅石類型與銳鈦礦類型的混合結晶相的光漫射劑的組合物相較金紅石類型包含更多銳鈦礦類型時，實現極好的光學特性及沉澱特性。 Referring to Table 3, when the primary particle diameter and the secondary particle diameter of the light-diffusing agent are controlled within a specific range, compared with the case of using a light-diffusing agent that does not have the primary particle diameter and the secondary particle diameter within the range, both the optical characteristics and the precipitation characteristics are improved. In addition, excellent optical and precipitation properties are achieved when the composition comprising a light diffuser having a particle diameter within a controlled range and thus a mixed crystalline phase of rutile and anatase types contains more anatase types than rutile types.
儘管本發明已結合目前視為實用實例實施例之內容來描述，但應瞭解，本發明不限於所揭露之實施例，但相反，本發明意 欲涵蓋包含在隨附申請專利範圍之精神及範疇內的各種修改及等效配置。因此，上述實施例應理解為例示性的但不以任何方式限制本發明。 While the invention has been described in conjunction with what are presently considered to be practical example embodiments, it is to be understood that the invention is not limited to the disclosed embodiments, but rather the invention is intended to Various modifications and equivalent arrangements included within the spirit and scope of the appended claims are intended to be covered. Therefore, the above-mentioned embodiments should be understood as illustrative but not restrictive of the present invention in any way.
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| TW588084B (en) * | 2000-12-27 | 2004-05-21 | Kanegafuchi Chemical Ind | Curing agents, curable compositions, compositions for optical materials, optical materials, optical materials, their production, and liquid crystal displays and LEDs made by using the materials |
| TW201925915A (en) * | 2017-12-07 | 2019-07-01 | 南韓商三星Ｓｄｉ股份有限公司 | Curable composition, photosensitive resin composition, photosensitive resin film, color filter and method of manufacturing a pixel |
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| KR102028640B1 (en) * | 2016-09-13 | 2019-11-04 | 삼성에스디아이 주식회사 | Photosensitive resin composition, photosensitive resin layer and color filter using same |
| KR102317627B1 (en) * | 2016-12-28 | 2021-10-26 | 디아이씨 가부시끼가이샤 | Ink composition, light conversion layer, and color filter |
| JP7020015B2 (en) * | 2017-09-14 | 2022-02-16 | Dic株式会社 | Ink composition, light conversion layer and color filter |
| WO2019064589A1 (en) * | 2017-09-29 | 2019-04-04 | 日立化成株式会社 | Wavelength conversion member, backlight unit, image display device, wavelength conversion resin composition, and wavelength conversion resin cured material |
| KR102237366B1 (en) * | 2017-12-07 | 2021-04-06 | 삼성에스디아이 주식회사 | Photosensitive resin composition, photosensitive resin layer using the same and color filter |
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| TW588084B (en) * | 2000-12-27 | 2004-05-21 | Kanegafuchi Chemical Ind | Curing agents, curable compositions, compositions for optical materials, optical materials, optical materials, their production, and liquid crystal displays and LEDs made by using the materials |
| TW201925915A (en) * | 2017-12-07 | 2019-07-01 | 南韓商三星Ｓｄｉ股份有限公司 | Curable composition, photosensitive resin composition, photosensitive resin film, color filter and method of manufacturing a pixel |
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| KR102449846B1 (en) | 2022-09-29 |
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