CN107709371A - The manufacture method of Photocurable composition and electronic unit - Google Patents
The manufacture method of Photocurable composition and electronic unit Download PDFInfo
- Publication number
- CN107709371A CN107709371A CN201680038410.2A CN201680038410A CN107709371A CN 107709371 A CN107709371 A CN 107709371A CN 201680038410 A CN201680038410 A CN 201680038410A CN 107709371 A CN107709371 A CN 107709371A
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- China
- Prior art keywords
- photocurable composition
- weight
- compound
- methyl
- mentioned
- Prior art date
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- 239000000203 mixture Substances 0.000 title claims abstract description 217
- 238000000034 method Methods 0.000 title claims description 34
- 238000004519 manufacturing process Methods 0.000 title description 41
- -1 nitrogen-containing compound Chemical class 0.000 claims abstract description 141
- 239000000463 material Substances 0.000 claims abstract description 102
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 46
- 235000014692 zinc oxide Nutrition 0.000 claims abstract description 39
- 239000011787 zinc oxide Substances 0.000 claims abstract description 38
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 10
- 150000001875 compounds Chemical class 0.000 claims description 75
- 239000002904 solvent Substances 0.000 claims description 45
- 239000003795 chemical substances by application Substances 0.000 claims description 37
- 239000000178 monomer Substances 0.000 claims description 36
- 239000012948 isocyanate Substances 0.000 claims description 28
- 238000000576 coating method Methods 0.000 claims description 22
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000001029 thermal curing Methods 0.000 claims description 13
- 229920000877 Melamine resin Polymers 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 230000000694 effects Effects 0.000 claims description 10
- 238000013007 heat curing Methods 0.000 claims description 9
- 125000002757 morpholinyl group Chemical group 0.000 claims description 9
- 150000004693 imidazolium salts Chemical class 0.000 claims description 7
- 238000007711 solidification Methods 0.000 claims description 7
- 230000008023 solidification Effects 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- 150000001408 amides Chemical class 0.000 claims description 5
- IUPDXIXTYXNMFR-UHFFFAOYSA-N azane N,N-dimethylmethanamine hydrochloride Chemical compound [Cl-].[NH4+].CN(C)C IUPDXIXTYXNMFR-UHFFFAOYSA-N 0.000 claims description 5
- COYVWKMZTCAFHO-UHFFFAOYSA-N n-methyl-n-propan-2-ylprop-2-enamide Chemical compound CC(C)N(C)C(=O)C=C COYVWKMZTCAFHO-UHFFFAOYSA-N 0.000 claims description 5
- NSXOFALHYZPMNH-UHFFFAOYSA-N 1-(3-methylmorpholin-4-yl)prop-2-en-1-one Chemical compound CC1COCCN1C(=O)C=C NSXOFALHYZPMNH-UHFFFAOYSA-N 0.000 claims description 4
- QENDLNJWYIFMIM-UHFFFAOYSA-N n-[3-(dimethylamino)propyl]-n-methylprop-2-enamide Chemical compound CN(C)CCCN(C)C(=O)C=C QENDLNJWYIFMIM-UHFFFAOYSA-N 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 2
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- 150000002118 epoxides Chemical class 0.000 claims 2
- YPHQUSNPXDGUHL-UHFFFAOYSA-N n-methylprop-2-enamide Chemical compound CNC(=O)C=C YPHQUSNPXDGUHL-UHFFFAOYSA-N 0.000 claims 1
- 238000002310 reflectometry Methods 0.000 abstract description 11
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- 229910052717 sulfur Inorganic materials 0.000 description 18
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 17
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 12
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 9
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- 229910001928 zirconium oxide Inorganic materials 0.000 description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 8
- 125000003118 aryl group Chemical group 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 8
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- 150000004767 nitrides Chemical class 0.000 description 8
- 239000000047 product Substances 0.000 description 8
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- KCTAWXVAICEBSD-UHFFFAOYSA-N prop-2-enoyloxy prop-2-eneperoxoate Chemical compound C=CC(=O)OOOC(=O)C=C KCTAWXVAICEBSD-UHFFFAOYSA-N 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 5
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical class OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 5
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical class SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 5
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 5
- 239000001273 butane Substances 0.000 description 5
- 239000013530 defoamer Substances 0.000 description 5
- 238000011161 development Methods 0.000 description 5
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 5
- 238000005227 gel permeation chromatography Methods 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 5
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- 229910052698 phosphorus Inorganic materials 0.000 description 5
- 239000011574 phosphorus Substances 0.000 description 5
- 229920000647 polyepoxide Polymers 0.000 description 5
- 229910000679 solder Inorganic materials 0.000 description 5
- 238000004381 surface treatment Methods 0.000 description 5
- 238000003786 synthesis reaction Methods 0.000 description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea group Chemical group NC(=O)N XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 5
- 229920002554 vinyl polymer Polymers 0.000 description 5
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- 229910000831 Steel Inorganic materials 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
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- 238000001579 optical reflectometry Methods 0.000 description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
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- WBHQBSYUUJJSRZ-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [H+].[H+].[Na+].[O-]S([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-N 0.000 description 4
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- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
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- 150000002989 phenols Chemical class 0.000 description 1
- 125000000843 phenylene group Chemical group C1(=C(C=CC=C1)*)* 0.000 description 1
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 125000004437 phosphorous atom Chemical group 0.000 description 1
- 238000001259 photo etching Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001223 polyethylene glycol Polymers 0.000 description 1
- 239000003505 polymerization initiator Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- ZJLMKPKYJBQJNH-UHFFFAOYSA-N propane-1,3-dithiol Chemical class SCCCS ZJLMKPKYJBQJNH-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- RVEZZJVBDQCTEF-UHFFFAOYSA-N sulfenic acid Chemical class SO RVEZZJVBDQCTEF-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- WMXCDAVJEZZYLT-UHFFFAOYSA-N tert-butylthiol Chemical compound CC(C)(C)S WMXCDAVJEZZYLT-UHFFFAOYSA-N 0.000 description 1
- UWHCKJMYHZGTIT-UHFFFAOYSA-N tetraethylene glycol Chemical compound OCCOCCOCCOCCO UWHCKJMYHZGTIT-UHFFFAOYSA-N 0.000 description 1
- 125000003831 tetrazolyl group Chemical group 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- BWPNIANVWARHPR-UHFFFAOYSA-N tridecyl dihydrogen phosphite Chemical class CCCCCCCCCCCCCOP(O)O BWPNIANVWARHPR-UHFFFAOYSA-N 0.000 description 1
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 description 1
- ODHXBMXNKOYIBV-UHFFFAOYSA-N triphenylamine Chemical compound C1=CC=CC=C1N(C=1C=CC=CC=1)C1=CC=CC=C1 ODHXBMXNKOYIBV-UHFFFAOYSA-N 0.000 description 1
- QQBLOZGVRHAYGT-UHFFFAOYSA-N tris-decyl phosphite Chemical compound CCCCCCCCCCOP(OCCCCCCCCCC)OCCCCCCCCCC QQBLOZGVRHAYGT-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- PAPBSGBWRJIAAV-UHFFFAOYSA-N ε-Caprolactone Chemical compound O=C1CCCCCO1 PAPBSGBWRJIAAV-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
- C08F2/50—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light with sensitising agents
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/44—Polymerisation in the presence of compounding ingredients, e.g. plasticisers, dyestuffs, fillers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
- C08F220/56—Acrylamide; Methacrylamide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
- C08F290/02—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups on to polymers modified by introduction of unsaturated end groups
- C08F290/06—Polymers provided for in subclass C08G
-
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/22—Secondary treatment of printed circuits
- H05K3/28—Applying non-metallic protective coatings
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Macromonomer-Based Addition Polymer (AREA)
- Non-Metallic Protective Coatings For Printed Circuits (AREA)
- Materials For Photolithography (AREA)
- Polymerisation Methods In General (AREA)
- Paints Or Removers (AREA)
- Graft Or Block Polymers (AREA)
- Epoxy Resins (AREA)
Abstract
The present invention provide it is a kind of can obtain the high solidfied material film of pencil hardness, and the Photocurable composition of the high solidfied material film of the reflectivity that light can be obtained by using Chinese white.Photocurable composition of the present invention contains：Oligomer, nitrogen-containing compound, Chinese white and Photoepolymerizationinitiater initiater, the oligomer is with the ethylenic unsaturated bond of more than 2 but does not have carboxyl, and under 25 DEG C and 10rpm, the viscosity of Photocurable composition is more than 1Pas and below 30Pas.
Description
Technical field
The present invention relates to a kind of Photocurable composition solidified by light irradiation to use.In addition, the present invention relates to
A kind of and manufacture method of electronic unit using above-mentioned Photocurable composition.
Background technology
As the diaphragm for being protected under high-temperature soldering to printed wiring board, soldering-resistance layer is widely used.
In addition, in various electronic units, light emitting diode (following, letter is equipped with the upper surface of printed wiring board
Referred to as LED) chip.In the light sent by LED, in order to be utilized to the light for reaching above-mentioned printed substrate upper surface side,
Sometimes formed with white solder masks on the upper surface of printed substrate.White solder masks include Chinese white.As formation
During white solder masks, it can not only utilize from the surface of LED chip and shine directly into light with printed substrate opposite side, also
It can use the upper surface side up to printed substrate and the reflected light reflected by white solder masks.Therefore, it is possible to carry
The high utilization ratio from light caused by LED.
In addition, in addition to soldering-resistance layer purposes, reflected in various light in purposes, use the solidfied material comprising Chinese white
Film.
As an example of the material for forming above-mentioned white solder masks, the following Patent Document 1 discloses
A kind of Photocurable composition, it is included：Molecular weight is 500~5000 compound (A), and the compound (A) has more than 2
Unsaturated group but do not have carboxyl；Photoepolymerizationinitiater initiater (B)；Reactivity dilution with the unsaturated groups of more than 2
Agent (C)；And the compound (D) with least one amino or imino group.
The following Patent Document 2 discloses a kind of Photocurable composition, and it is included：There is at least two in 1 molecule
The active energy ray-curable resin (A) of ethylenic unsaturated bond, Photoepolymerizationinitiater initiater (B), diluent (C), titanium oxide (D),
And epoxies Thermocurable compound (E).Above-mentioned Photocurable composition includes epoxy (methyl) acrylate of two functions
(A1) it is used as above-mentioned (A) composition.
Prior art literature
Patent document
Patent document 1：WO2011/065228A1
Patent document 2：Japanese Unexamined Patent Publication 2011-158628 publications
The content of the invention
The technical problems to be solved by the invention
For current Photocurable composition, the pencil hardness step-down of solidfied material film sometimes.At present, it is difficult to simultaneously full
The high light reflectivity of foot and high pencil hardness.
The high solidfied material film of pencil hardness can be obtained it is an object of the invention to provide a kind of, and by using white face
Material can obtain the Photocurable composition of the high solidfied material film of light reflectivity.In addition, the present invention also aims to provide one
Kind uses the manufacture method of the electronic unit of above-mentioned Photocurable composition.
For solving the technical scheme of technical problem
According to an aspect of the present invention, there is provided a kind of Photocurable composition, it contains：Oligomer, nitrogen-containing compound,
Chinese white and Photoepolymerizationinitiater initiater, the oligomer is with the ethylenic unsaturated bond of more than 2 but does not have carboxyl,
Under 25 DEG C and 10rpm, the viscosity of Photocurable composition is more than 1Pas and below 30Pas.
In a particular aspects of Photocurable composition of the present invention, Photocurable composition contains epoxidation
During compound, in the weight % of composition 100 in Photocurable composition in addition to solvent, the content of epoxide is 5 weight %
Below.
In a particular aspects of Photocurable composition of the present invention, Photocurable composition includes heat cure
When agent and the Thermocurable compound solidified by the effects of the thermal curing agents, solvent is removed in Photocurable composition
In the weight % of composition 100 in addition, the content of the Thermocurable compound is below 5 weight %.
In the specific aspect of one of Photocurable composition of the present invention, the nitrogen-containing compound is with 1
The amide-containing monomer of ethylenic unsaturated bond above or the monomer containing morpholinyl with the ethylenic unsaturated bond of more than 1.
In a particular aspects of Photocurable composition of the present invention, the nitrogen-containing compound is dimethyl
(methyl) acrylamide, (methyl) acryloyl morpholine, isopropyl (methyl) acrylamide, diethyl (methyl) acrylamide, two
Dimethylaminopropyl (methyl) acrylamide, (3- acrylamide propyls) trimethyl ammonia chloride ammonium salt or ethoxy (methyl) propylene
Acid amides.
In a particular aspects of Photocurable composition of the present invention, in Photocurable composition except solvent with
In the outer weight % of composition 100, the content of the nitrogen-containing compound is more than 1 weight % and below 40 weight %.
In a particular aspects of Photocurable composition of the present invention, the nitrogen-containing compound is tetrazolium chemical combination
Thing, imidazolium compounds, triazole compounds, isocyanate compound or melamine compound.
In a particular aspects of Photocurable composition of the present invention, in Photocurable composition except solvent with
In the outer weight % of composition 100, the content of the nitrogen-containing compound is more than 0.1 weight % and is below 5 weight %.
In a particular aspects of Photocurable composition of the present invention, the nitrogen-containing compound is containing morpholinyl
Compound or isocyanate compound.
In a particular aspects of Photocurable composition of the present invention, Photocurable composition passes through light irradiation
And used after being solidified, and for not carrying out forming solidfied material film with developing to it.
Photocurable composition of the present invention, it is preferred for partly being coated on coating object Part surface, and
It is coated on multiple positions.
Photocurable composition of the present invention, it is preferably not used for carrying out heat cure by the effect of thermal curing agents.
According to an aspect of the present invention, there is provided a kind of manufacture method of electronic unit, it includes：In electronic component body
Surface on be coated with above-mentioned Photocurable composition, so as to form the process of composition layer；And the composition layer is shone
Light is penetrated, so as to form the process of solidfied material film, without showing to form the solidfied material film to the composition layer
The operation of shadow.
In a specific aspect of the manufacture method of electronic unit of the present invention, make the photocurable compositions
Thing is partly coated on the electronic component body surface, and is coated on multiple positions.
In a specific aspect of the manufacture method of electronic unit of the present invention, without described in order to be formed
Solidfied material film and make the composition layer pass through thermal curing agents effect carry out heat cure operation.
Because Photocurable composition of the present invention contains：Oligomer, nitrogen-containing compound, Chinese white, Yi Jiguang
Polymerization initiator, the oligomer is with the ethylenic unsaturated bond of more than 2 but does not have carboxyl, under 25 DEG C and 10rpm,
The viscosity of Photocurable composition is more than 1Pas and below 30Pas, accordingly, it is capable to access the high solidfied material of pencil hardness
Film, and by using Chinese white, the high solidfied material film of the reflectivity of light can be obtained.
Brief description of the drawings
Fig. 1 (a)~(c) is to make for illustrating the Photocurable composition that is related to using one embodiment of the present invention
Make the profile of an example of the method for electronic unit.
Fig. 2 (a)~(e) is for illustrating to manufacture the method for electronic unit using current developable anti-corrosion agent composition
An example profile.
Description of reference numerals
1 ... electronic unit
2 ... resist films (solidfied material film)
11 ... coating object Parts (electronic component body)
11A ... substrates
11B ... electrodes
12 ... resist layers (composition layer)
Embodiment
Illustrate the details of the present invention below.
[Photocurable composition]
Photocurable composition of the present invention, used after preferably being solidified by light irradiation, and for not
It is carried out to form solidfied material film with developing.Photocurable composition of the present invention is preferably that non-developable resist light is consolidated
The property changed composition.Without being developed using Photocurable composition of the present invention to form resist film
In the case of, Photocurable composition is different from the developable anti-corrosion agent composition to be developed to form resist film.Just
For Photocurable composition of the present invention, using the group that good resist film can be also obtained even if without development
Into.
Photocurable composition of the present invention contains：(A) there is the ethylenic unsaturated bond of more than 2 but do not have carboxylic
The oligomer of base, (C) nitrogen-containing compound, (D) Chinese white and (E) Photoepolymerizationinitiater initiater.
In the present invention, due to using above-mentioned technical proposal, therefore it is (against corrosion to form the high solidfied material film of pencil hardness
Agent film etc.).Further, Photocurable composition of the present invention, due to containing (D) Chinese white, and white can be formed
Solidfied material film (resist film etc.), the high solidfied material film of light reflectivity can be obtained.By making solidfied material film for white, Neng Gouti
The light reflectivity of high solidification thing film.Further, in the present invention, due to using above-mentioned technical proposal, and solidfied material film phase is caused
Also uprised for the adaptation for being coated with object Part.
Further, in the present invention, even if without multiple processes such as the exposure process in photoetching process and developing procedure,
Also good solidfied material film (resist film etc.) can be formed.In the case of without exposure process and developing procedure, energy
Quantity of refuse is enough reduced, carrying capacity of environment can be mitigated.Further, additionally it is possible to reduce the manufacturing cost of electronic unit etc..
Above-mentioned Photocurable composition, due to being solidified by light irradiation, (F) Thermocurable compound can be free of,
Thermal curing agents can also be free of.Above-mentioned Photocurable composition, it is preferably not used for carrying out heat cure by the effect of thermal curing agents.
, can not be to configuring the composition layer on the surface of coating object Part in order to form above-mentioned solidfied material film (resist film etc.)
(resist layer etc.) carries out heat cure., can not be to configuring on the surface of coating object Part in order to form above-mentioned solidfied material film
On composition layer heated.But in combinations thereof nitride layer, the heating under low temperature can be carried out.It is above-mentioned in order to be formed
Solidfied material film, is not preferably heated to more than 280 DEG C by combinations thereof nitride layer, is more preferably not heated to more than 180 DEG C, further excellent
Choosing is not heated to more than 60 DEG C.It is lower to heat the temperature of combinations thereof nitride layer, can more suppress the coating pair such as electronic component body
As the heat deterioration of part.
In order to improve the pencil hardness of solidfied material film, the viscosity of Photocurable composition is under 25 DEG C and 10rpm
More than 1Pas and below 30Pas.By combining (A), (C)~(F) compositions, and make the viscosity of Photocurable composition upper
In the range of stating, the pencil hardness of solidfied material can be effectively improved.Above-mentioned viscosity be less than above-mentioned lower limit when, sometimes print after and
The thickness of solidfied material film after solidification is thinning, and pencil hardness declines.When above-mentioned viscosity exceedes the above-mentioned upper limit, the group after printing sometimes
The thickness of compound layer is thickening, and illumination declines less than inside, internal curability step-down, pencil hardness.
From the viewpoint of the pencil hardness for further effectively improving solidfied material film, photocuring under 25 DEG C and 10rpm
Property composition viscosity be preferably more than 5Pas, more preferably above 5Pas, more preferably more than 7Pas, be preferably
Below 25Pas.
Above-mentioned viscosity, using E type viscosimeters, determined under conditions of 25 DEG C and 10rpm.As above-mentioned E types viscosimeter,
" VISCOMETER TV-22 " etc. of Toki Sangyo Co., Ltd.'s manufacture can be included.
Hereinafter, each composition contained in above-mentioned Photocurable composition is illustrated.
(oligomer of (A) with the ethylenic unsaturated bond of more than 2 but without carboxyl)
Contained (A) oligomer in above-mentioned Photocurable composition, with the ethylenic unsaturated bond of more than 2 but does not have
Carboxyl.By using (A) oligomer, solidfied material film effectively uprises relative to the adaptation of coating object Part.Particularly exist
(D) in the case that the content of Chinese white is more, when (A) oligomer is not used, solidfied material film be present relative to coating object Part
The easy step-down of adaptation trend.By using (A) oligomer, even if the content of (D) Chinese white is more, it is possible to increase solidification
Thing film is relative to the adaptation for being coated with object Part.In addition, by making (A) oligomer not have carboxyl, can prevent by solidifying
The harmful effect that carboxyl in thing film is brought, such as the discoloration of solidfied material film can be suppressed.(A) oligomer can be used alone one
Kind, can also be simultaneously using two or more.
(A) oligomer is preferably photocurable compound.
(A) as the group containing ethylenic unsaturated bond in oligomer, vinyl, pi-allyl, (methyl) can be included
Acryloyl group etc..From effectively reacted, further suppress to peel off and discoloration from the viewpoint of, preferred (methyl) acryloyl
Base.(A) oligomer preferably has (methyl) acryloyl group.
From the viewpoint of adaptation of the solidfied material film relative to coating object Part is improved, preferably (A) oligomer is
(A1) epoxy (methyl) acrylate.From the viewpoint of the pencil hardness for improving solidfied material film, preferred (A1) epoxy (methyl)
Acrylate contains epoxy (methyl) acrylate more than epoxy (methyl) acrylate and trifunctional of two functions.Two
Epoxy (methyl) acrylate of function preferably has 2 (methyl) acryloyl groups.Epoxy (methyl) propylene more than trifunctional
Acid esters preferably has more than 3 (methyl) acryloyl group.
(A1) epoxy (methyl) acrylate is by making (methyl) acrylic acid be reacted with epoxide to obtain.(A1) ring
Oxygen (methyl) acrylate is obtained by the way that epoxy radicals to be transformed to (methyl) acryloyl group.Above-mentioned Photocurable composition, by
Solidified in by light irradiation, therefore, (A1) epoxy (methyl) acrylate does not preferably have epoxy radicals.
As (A1) epoxy (methyl) acrylate, can include biphenol type epoxy (methyl) acrylate (such as, bis-phenol
A type rings oxygen (methyl) acrylate, bisphenol F type epoxy (methyl) acrylate, bisphenol S type epoxy (methyl) acrylate), first
Biphenol type epoxy (methyl) propylene that phenol phenol aldehyde type (Cresol novolak type) epoxy (methyl) acrylate, amine are modified
Acid esters, biphenol type epoxy (methyl) acrylate of caprolactone modification, carboxylic acid anhydride modified epoxy (methyl) acrylate and
Phenol novolak type (Phenol novolak type) epoxy (methyl) acrylate etc..
As the commercially available product of epoxy (methyl) acrylate of two functions, KAYARAD R-381 (Nippon can be included
Kayaku Co., Ltd. prepare, bisphenol-a epoxy acrylate), EBECRYL3700, EBECRYL3701 and
EBECRYL3708 (prepared by DAICEL-ALLNEX Co., Ltd., modified bisphenol A type epoxy acrylate) etc..In addition, as three
The commercially available product of epoxy (methyl) acrylate more than function, EBECRYL3603 (DAICEL-ALLNEX strain formula meetings can be included
Prepared by society, Epoxy Phenolic Acrylates) etc..Furthermore it is possible to by changing the hydroxyl of the epoxy of two functions (methyl) acrylate
Property and import (methyl) acryloyl group, so as to obtain epoxy (methyl) acrylate more than trifunctional.
" (methyl) acryloyl group " represents acryloyl group and methylacryloyl." (methyl) acrylic acid " represent acrylic acid and
Methacrylic acid." (methyl) acrylate " represents acrylate and methacrylate.
Oligomer is different from monomer, is the polymer that more than 2 monomers are formed by connecting.(A) weight average molecular weight of oligomer
Preferably greater than 500, more preferably above 600, further preferably more than 800, particularly preferably more than 1000, most preferably 2000 with
On.(A) weight average molecular weight of oligomer is preferably less than 10000.(A) weight average molecular weight of oligomer is more than above-mentioned lower limit
When, the adaptation of solidfied material film becomes higher, the discoloration being less also easy to produce after backflow.
(A) weight average molecular weight of oligomer is the weight with polystyrene basis determined using gel permeation chromatography (GPC)
Average molecular weight, it can be measured using following measure device and condition determination.When being determined under the condition determination, rear
The EBECRYL3700 used in the embodiment stated weight average molecular weight is 1300.
Determine device：" the Waters GPC System (Waters2690+ of Nihon Waters Co., Ltd. manufacture
Waters 2414(RI))”
Condition determination
Post：Shodex GPC LF-G × 1, Shodex GPC LF-804 × 2
Mobile phase：THF 1.0mL/ minutes
Sample concentration：5mg/mL
Detector：Differential refraction rate detector (RID)
Standard substance：Polystyrene (manufacture of TOSOH companies, molecular weight：620~590000)
From the viewpoint of effective suppression is peeled off and changed colour, (A) oligomer is preferably not with alicyclic skeleton
Compound, it is epoxy (methyl) acrylate with alicyclic skeleton not preferably to be.Suppress stripping and change from further
From the viewpoint of color, (A) oligomer preferably comprises the compound with aromatic backbone, preferably comprises with aromatic backbone
Epoxy (methyl) acrylate.
From it is effective suppress to peel off and discoloration from the viewpoint of, (A) oligomer be preferably polyurethane (methyl) acrylate,
Polyester (methyl) acrylate or epoxy (methyl) acrylate with aromatic backbone, more preferably polyurethane (methyl) third
Olefin(e) acid ester or epoxy (methyl) acrylate with aromatic backbone.
(A1) there is no particular limitation for epoxy (methyl) acrylate, can be by making bisphenol A type epoxy compound, Bisphenol F
Type ring oxygen compound, bisphenol S type epoxy compound, phenol novolak type epoxide, cresol novolak type epoxy compound or fat
The epoxides such as fat race epoxide obtain with (methyl) propylene acid reaction.
(A1) epoxy (methyl) acrylate can be the hydroxyl modification of epoxy (methyl) acrylate for making to have hydroxyl
Epoxy (methyl) acrylate formed.In this case, it is possible to increase the degree of cross linking, pencil hardness can be effectively improved.As energy
For modified compound, silane coupler and the monomer with NCO etc. can be included.It is even as above-mentioned silane
Join agent, can include with vinyl, (methyl) acryloyl group, styryl, sulfydryl, epoxy radicals, amino, thioether group, urea groups,
And the compound of the functional group such as NCO.Due to photoreactivity, therefore preferably there is vinyl, (methyl) propylene
The compound of acyl group, styryl or sulfydryl.As the monomer with NCO, vinyl, (methyl) third can be included
Enoyl-, styryl or compound with sulfydryl etc..
(A) acid number of oligomer is preferably below 20mgKOH/g.If acid number is below the above-mentioned upper limit, the shadow of acidic-group
Sound is suppressed, it is possible to increase the heat resistance of solidfied material film.In addition, above-mentioned Photocurable composition contains a variety of (A) with 2
During the oligomer of above ethylenic unsaturated bond, above-mentioned acid number refers to, (A) has the oligomer of more than 2 ethylenic unsaturated bonds
The acid number of mixture.
(A) acid number of oligomer proceeds as described below measure.
(A) 30g acetone is added in 1g oligomer, by (A) oligomer uniform dissolution, obtains solution.It is in addition, low at (A)
When in polymers added with volatile ingredients such as synthetic, retarder thinners, before above-mentioned solution is obtained, in advance than volatile ingredient
Heated 1~4 hour at a temperature of high 10 DEG C or so of boiling point, remove volatile ingredient.Then, add as the phenolphthalein of indicator in right amount
It is added in resulting solution, is titrated using 0.1N potassium hydroxide (KOH) aqueous solution.It is used as measure by calculating to neutralize
The mg numbers of KOH required for the above-mentioned solution (acetone soln of (A) oligomer) of object, obtain acid number.
In the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, (A) oligomer and (A1) epoxy
The content of (methyl) acrylate is preferably more than 5 weight %, more preferably more than 10 weight %, preferably 40 weight % with
Under, more preferably below 30 weight %.The content of (if A) oligomer and (A1) epoxy (methyl) acrylate is above-mentioned lower limit
More than, then the adaptation of solidfied material film effectively uprises.In addition, from the viewpoint of the adaptation for effectively improving solidfied material film, on
State in the weight % of composition 100 in Photocurable composition in addition to solvent, the epoxy (methyl) as two functions of oligomer
Acrylate and the total content as epoxy (methyl) acrylate more than trifunctional of oligomer be preferably 5 weight % with
On, more preferably more than 10 weight %, preferably below 40 weight %, more preferably below 30 weight %.
The weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent refers to that Photocurable composition contains
During solvent, the weight % of composition 100 in Photocurable composition in addition to solvent；When Photocurable composition is free of solvent, light
The weight % of solidification compound 100.
(monomer (reactive diluent) of (B) with the ethylenic unsaturated bond of more than 1)
From the adaptation for effectively improving solidfied material film, and easily the viscosity of Photocurable composition is controlled in optimal model
From the viewpoint of enclosing, above-mentioned Photocurable composition preferably comprises the monomer of (B) with the ethylenic unsaturated bond of more than 1.(B)
Monomer is, for example, reactive diluent.By being used together (B) monomer with (A) oligomer, even if the content of (D) Chinese white
It is more, the adaptation of solidfied material film can be also effectively improved, easily further controls the viscosity of Photocurable composition optimal
Scope.(B) molecular weight of monomer is preferably less than 2000, more preferably less than 800, more preferably less than 600, especially excellent
Elect less than 500 as.(B) monomer can be used alone, can also be simultaneously using two or more.(B) molecular weight of monomer can
To be calculated by structural formula.
As the group containing ethylenic unsaturated bond in (B) monomer, vinyl, pi-allyl, (methyl) third can be included
Enoyl- etc..From effectively reacted, further suppress to peel off and discoloration from the viewpoint of, preferred (methyl) acryloyl
Base.(B) monomer preferably has (methyl) acryloyl group.
As (B) monomer, there is no particular limitation, can include (methyl) acrylic acid adduct, the Yi Jiduo of polyalcohol
(methyl) acrylic acid adduct of the epoxide modification thing of first alcohol etc..As above-mentioned polyalcohol, diethylene glycol, three can be included
Ethylene glycol, polyvinyl alcohol, DPG, tripropylene glycol, polypropylene glycol, trimethylolpropane, cyclohexanedimethanol, tristane
Dimethanol, the epoxides addition product of bisphenol-A and pentaerythrite etc..
(B) monomer can be the compound that (B1) has 1 ethylenic unsaturated bond.From further raising solidfied material film
From the viewpoint of adaptation, (B) monomer preferably comprises the compound of (B1) with 1 ethylenic unsaturated bond, preferably comprises with 1
The compound of individual (methyl) acryloyl group.
(B) monomer can contain the compound with 2 ethylenic unsaturated bonds, and can also contain (B2) has more than 2
The compound of ethylenic unsaturated bond.From the viewpoint of the further adaptation for improving solidfied material film, (B) monomer preferably comprises
(B2) there is the compound of more than 2 ethylenic unsaturated bonds, preferably comprise the chemical combination with more than 2 (methyl) acryloyl groups
Thing.
From the viewpoint of the further adaptation for improving solidfied material film, preferably (B) monomer contain ester ring type compound,
Or contain aromatic rings or hydroxyl.Although it is preferred that the composition of simple function group, it is polyfunctional can to contain two functions or trifunctional etc.
Multiple compositions.
In the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, (B) monomer and (B2) have 2
The content of the compound of individual above ethylenic unsaturated bond is preferably more than 5 weight %, more preferably more than 10 weight %, is preferably
Below 50 weight %, more preferably below 40 weight %.(if B) monomer and (B2) have more than 2 ethylenic unsaturated bonds
The content of compound is that then the adaptation of solidfied material film effectively uprises more than above-mentioned lower limit and below the above-mentioned upper limit.
((C) nitrogen-containing compound)
By using (C) nitrogen-containing compound, the high solidfied material film of pencil hardness can be obtained, solidfied material film can be suppressed
Scar.(C) nitrogen-containing compound is not (E) Photoepolymerizationinitiater initiater.(C) nitrogen-containing compound can be used alone, can also two
Used simultaneously more than kind.
As (C) nitrogen-containing compound, can include dimethyl (methyl) acrylamide, isopropyl (methyl) acrylamide,
Diethyl (methyl) acrylamide, dimethylaminopropyl (methyl) acrylamide, (3- acrylamide propyls) trimethyl ammonia chloride
Ammonium salt etc. has the amide-containing monomer of more than 1 ethylenic unsaturated bond；(methyl) acryloyl morpholine etc. has more than 1 alkene
Belong to the monomer containing morpholinyl of unsaturated bond；Ethoxy (methyl) acrylamide, tetrazole compound, imidazolium compounds, triazole chemical combination
Thing, isocyanate compound and melamine compound etc..
From the viewpoint of the further pencil hardness for improving solidfied material film, (C) nitrogen-containing compound is preferably dimethyl
(methyl) acrylamide, (methyl) acryloyl morpholine, isopropyl (methyl) acrylamide, diethyl (methyl) acrylamide, two
Dimethylaminopropyl (methyl) acrylamide, (3- acrylamide propyls) trimethyl ammonia chloride ammonium salt, ethoxy (methyl) acryloyl
Amine, tetrazole compound, imidazolium compounds, triazole compounds, isocyanate compound or melamine compound.
From the viewpoint of the further pencil hardness for improving solidfied material film, (C) nitrogen-containing compound is preferably methyl (first
Base) acrylic acid amides, (methyl) acryloyl morpholine, isopropyl (methyl) acrylamide, diethyl (methyl) acrylamide, diformazan
Base aminopropyl (methyl) acrylamide, (3- acrylamide propyls) trimethyl ammonia chloride ammonium salt or ethoxy (methyl) acryloyl
They (are also referred to as (C1) composition) by amine.From the viewpoint of the further pencil hardness for improving solidfied material film, (C) nitrogen
Compound is preferably also tetrazole compound, imidazolium compounds, triazole compounds, isocyanate compound or melamine compound
(they are also referred to as (C2) composition).(C2) composition does not preferably have olefinic double bond.
As above-mentioned tetrazole compound, 1H-TETRAZOLE, 5- amino -1H-TETRAZOLE, 5- methyl isophthalic acid H- tetrazoliums, 5- benzene can be included
Base -1H-TETRAZOLE, 1- methyl -5- ethyls -1H-TETRAZOLE, 1- methyl -5- sulfydryls -1H-TETRAZOLE, 1- phenyl -5- sulfydryls -1H-TETRAZOLE,
1- (2- dimethyl aminoethyls) -5- sulfydryls -1H-TETRAZOLE, 2- methoxyl groups -5- (5- Trifluoromethyl-1 H- tetrazolium -1- bases)-benzene first
Aldehyde, 5,5 '-bis- -1H-TETRAZOLE di-ammonium salts, 4,5- bis- (5- tetrazoliums)-[1,2,3] triazole, 5,5 '-azo, two -1H-TETRAZOLE, 1- first
Base -5- benzoyls -1H-TETRAZOLE, 1- methyl isophthalic acid H- tetrazolium -5- bases and phenyl ketone oxime (E+Z) (are TOYOBO strain formulas
Commercial firm manufactures) etc..Above-mentioned tetrazole compound can be used alone, can also be simultaneously using two or more.
As above-mentioned imidazolium compounds, can include imidazoles -4- carbonyls aldehyde, 2- phenylimidazole -4- carbonyls aldehyde, imidazoles -2- carbonyls aldehyde,
Imidazoles -4- formonitrile HCNs, 2- phenylimidazole -4- formonitrile HCNs, 4- hydroxy methylimidazoles hydrochloride, 2- hydroxy methylimidazoles hydrochloride, 4- imidazoles carboxylics
Acid, 4- imidazoles carbodithioic acid, 4- imidazoles thiocarboxyl groups acid amides, 2- limidazoliums and 2- mercaptoimidazoles (are four countries' chemical conversion
Industrial Co., Ltd manufactures) etc..Above-mentioned imidazolium compounds can be used alone, can also be simultaneously using two or more.
As above-mentioned triazole compounds, 1,2,3- BTAs, 1- [double (2- ethylhexyls) amino first of N, N- can be included
Base] BTA, carboxyl benzotriazole, 1- [N, N- double (2- ethylhexyls) amino methyls] methylbenzotrazole, 2,2 '-
[[(methyl isophthalic acid H- BTA -1- bases) methyl] imino group] diethanol and l, 2,3 triazole sodium salt solution (are city
Northern chemical industry Co., Ltd. manufacture) etc..Above-mentioned triazole compounds can be used alone, can also be applied in combination two kinds with
On.
As above-mentioned isocyanate compound, for example, can include toluene di-isocyanate(TDI), xylylene diisocyanate,
The aromatic isocyanates such as methylenediphenyl diisocyanates, phenylene vulcabond, naphthalene diisocyanate；α,α,α’,
α '-tetramethyl xylylene diisocyanate etc. has the aliphatic isocyanates of aromatic rings；Methylene diisocyanate, Asia third
The fat such as group diisocyanate, lysine diisocyanate, trimethyl hexamethylene diisocyanate, hexamethylene diisocyanate
Fat race isocyanates；Cyclohexane diisocyanate, methylcyclohexane diisocyanate, IPDI, methylene
Alicyclic isocyanates such as two (4- cyclohexyl isocyanates), isopropylidene dicyclohexyl diisocyanate etc..In addition, these are different
Biuret compound, isocyanuric acid carboxylate, urea diketonate and the Carbodiimide-Modified body of cyanate esters etc. gather
Compound or derivative, it can also be included as above-mentioned isocyanate compound.Above-mentioned isocyanate compound can be independent
Using one kind, can also be applied in combination two or more.From the viewpoint of the xanthochromia by UV-induced solidfied material film is avoided,
Compared with aromatic isocyanate compound, more preferably aliphatic isocyanates compound or alicyclic isocyanate compound.
Above-mentioned isocyanate compound is using the state of blocked isocyanate in use, as end-capping reagent, such as can include
Bisulfites；The oxybenzene compounds such as phenol, cresols, ethyl -phenol；Propylene glycol monomethyl ether, ethylene glycol, phenmethylol, methanol,
The alcoholic compounds such as ethanol；Dimethyl malenate, diethyl malonate, methyl acetoacetate, ethyl acetoacetate, acetylacetone,2,4-pentanedione etc.
Activity methene compound；The mercaptan compounds such as butyl mercaptan, lauryl mercaptan；Acyl in epsilon-caprolactams, δ-valerolactam etc.
Amines；The amines such as diphenyl aniline, aniline, aziridine；The amide compound of antifebrin, amide；First
Oxime compounds such as aldehyde, acetyl oxime, acetoxime, methyl ethyl ketone oxime, cyclohexanone oxime etc..Above-mentioned end-capping reagent can be used alone one
Kind, it can also be applied in combination two or more.
As the commercially available product of above-mentioned isocyanate compound, the 2- acryloyls that Showa Denko K. K manufactures can be included
Epoxide ethyl isocyanate (Karenz AOI), 2- methacryloxyethyls isocyanates (Karenz MOI), methyl-prop
Isocyanate-terminated body (the Karenz of alkene oyloxyethoxy ethyl isocyanate (Karenz MOI-EG), Karenz MOI
MOI-BM), Karenz MOI isocyanate-terminated body (Karenz MOI-BP) and 1,1- (two acryloyloxymethyls)
Ethyl isocyanate) (Karenz BEI) etc..
As above-mentioned melamine compound, alcohol of sening as an envoy to can be enumerated and refined with alkyl alcoholization melamine derivative, alkyl
The partial ethers compound that melamine derivative reaction forms；And alcohol and alkyl is refined melamine derivative reaction and
Into complete Esterifying compounds etc..Above-mentioned melamine compound can be used alone, can also be applied in combination two kinds with
On.As the alcohol used in above-mentioned etherificate, methanol, ethanol, isopropanol, n-butanol and isobutanol etc. can be included.In addition,
Melamine compound can be monomer, can be polymer more than dimer, or the mixing of monomer and polymer
Thing.Melamine compound can be a part for urea etc. and melamine is carried out the compound that cocondensation forms.In order to
The reactivity of melamine compound is improved, catalyst can also be used.
From the further scar for suppressing solidfied material film, the viewpoint for further improving the pencil hardness of solidfied material film is examined
Consider, (C) nitrogen-containing compound is preferably contain morpholinyl compounds or isocyanate compound, can for containing morpholinyl compounds,
It can be isocyanate compound.In this case, from the further scar for suppressing solidfied material film, further improve solidfied material
From the viewpoint of the pencil hardness of film, with regard to it is above-mentioned contain morpholinyl compounds for, preferably monomer containing morpholinyl, preferably with 1
Individual above ethylenic unsaturated bond, isocyanate compound are preferably aliphatic isocyanates compound or alicyclic isocyanate
Compound.
In the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, the content of (C) nitrogen-containing compound is excellent
Elect as more than 0.1 weight %, more preferably more than 0.5 weight %, preferably below 45 weight %, more preferably 33 weight % with
Under.If the content of (C) nitrogen-containing compound is more than above-mentioned lower limit and below the above-mentioned upper limit, the pencil hardness of solidfied material film enters
One step uprises.
When above-mentioned Photocurable composition contains (C1) composition, the composition in above-mentioned Photocurable composition in addition to solvent
In 100 weight %, the content of (C1) composition is preferably more than 1 weight %, more preferably more than 5 weight %, preferably 40 weights
Below % is measured, more preferably below 33 weight %, more preferably below 30 weight %.The content of (if C1) composition is above-mentioned
More than lower limit and below the above-mentioned upper limit, then the pencil hardness of solidfied material film further uprises.
When above-mentioned Photocurable composition contains (C2) composition, the composition in above-mentioned Photocurable composition in addition to solvent
In 100 weight %, the content of (C2) composition is preferably more than 0.1 weight %, more preferably more than 0.5 weight %, preferably 5 weights
Below % is measured, more preferably below 3 weight %.If the content of (C2) composition is more than above-mentioned lower limit and below the above-mentioned upper limit,
Then the pencil hardness of solidfied material film further uprises.
(C) nitrogen-containing compound is when containing morpholinyl compounds, from the sight of the further pencil hardness for improving solidfied material film
Point considers that in the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, the content containing morpholinyl compounds is excellent
Elect as more than 1 weight %, more preferably more than 5 weight %, preferably below 40 weight %, more preferably below 33 weight %,
More preferably below 30 weight %.(C) when nitrogen-containing compound is isocyanate compound, solidfied material is improved from further
From the viewpoint of the pencil hardness of film, in the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, isocyanic acid
The content of ester compounds is preferably more than 0.1 weight %, more preferably more than 0.5 weight %, preferably below 5 weight %, more
Preferably below 3 weight %.
((D) Chinese white)
By making above-mentioned Photocurable composition contain (D) Chinese white, the high solidfied material of the reflectivity of light can be formed
Film.By using (D) Chinese white, when using only packing material in addition to (D) Chinese white compared with, light can be obtained
The high solidfied material film of reflectivity.(D) Chinese white can be used alone, and can also be applied in combination two or more.
As (D) Chinese white, aluminum oxide, titanium oxide, zinc oxide, zirconium oxide, antimony oxide and magnesia can be included
Deng.
From the viewpoint of the further reflectivity for improving solidfied material film to light, (D) Chinese white be preferably titanium oxide,
Zinc oxide or zirconium oxide.During using the preferable Chinese white, in titanium oxide, zinc oxide and zirconium oxide, one can be used
Kind or two or more Chinese whites.(D) Chinese white is preferably titanium oxide or zinc oxide, preferably titanium oxide, preferably oxygen
Change zinc.(D) Chinese white is preferably zirconium oxide.
Above-mentioned titanium oxide is preferably Titanium Dioxide Rutile Top grade.By using Titanium Dioxide Rutile Top grade, solidfied material film it is heat-resisting
Property further uprises, and the further discoloration to solidfied material film suppresses.
Above-mentioned titanium oxide is preferably that the Titanium Dioxide Rutile Top grade being surface-treated using aluminum oxide (is aoxidized as utilizing
The Titanium Dioxide Rutile Top grade for the surface treatment that aluminium is surface-treated).Table has been carried out by using using above-mentioned aluminum oxide
The Titanium Dioxide Rutile Top grade of face processing, the heat resistance of solidfied material film further uprise.
As the Titanium Dioxide Rutile Top grade being surface-treated using above-mentioned aluminum oxide, such as can include：As gold
" CR-90-2 ", the stone as rutile chloridising titanium oxide of Ishihara Sangyo Kaisha, Ltd.'s manufacture of red stone chloridising titanium oxide
" the R- that " CR-58 " of original industry Co., Ltd. manufacture, Du Pont Co., Ltd. as rutile chloridising titanium oxide manufacture
900 " and " R-630 " of Ishihara Sangyo Kaisha, Ltd.'s manufacture as rutile sulfuric acid process titanium oxide etc..
Above-mentioned zinc oxide is preferably the zinc oxide being surface-treated.From the further processability for improving solidfied material film
And from the viewpoint of the reflectivity of the light of solidfied material film, above-mentioned zinc oxide is preferably by the material containing silicon, aluminium or zirconium oxide
It is surface-treated, is more preferably surface-treated using the material containing silicon.Above-mentioned zinc oxide is preferably to utilize above-mentioned material
Expect the surface treatment being surface-treated.Material containing above-mentioned silicon is preferably organo-silicon compound.
The zirconium oxide that above-mentioned zirconium oxide has preferably been surface treated.From the reflection of the further light for improving solidfied material film
From the viewpoint of rate, above-mentioned zirconium oxide is surface-treated preferably by the material containing silicon, aluminium or zirconium oxide, is more preferably utilized
Material containing silicon is surface-treated.The above-mentioned material containing silicon is preferably organo-silicon compound.
There is no particular limitation for the method for above-mentioned surface treatment.As the method for surface treatment, dry process, wet can be used
Formula method, overall mixing method (integral blending) and other known usual surface treatment methods.
(D) average grain diameter of Chinese white is preferably more than 1nm, preferably less than 40 μm.If above-mentioned average grain diameter is upper
State more than lower limit and below the above-mentioned upper limit, then can further improve the reflectivity of the light of solidfied material film.
In the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, the content of (D) Chinese white is preferred
For more than 30 weight %, more preferably more than 40 weight %, preferably below 70 weight %, more preferably below 60 weight %.
If the content of (D) Chinese white is more than above-mentioned lower limit and below the above-mentioned upper limit, the reflectivity of the light of solidfied material film more enters
One step uprises, and the adaptation of above-mentioned solidfied material film further uprises.In above-mentioned Photocurable composition in addition to solvent into
Divide in 100 weight %, the content of (D) Chinese white can be more than 50 weight %.
In the present invention, due to using specific composition, therefore, even if the content of (D) Chinese white is more, can also improve solid
The adaptation of compound film.For example, in the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, even if (D) is white
The content of color pigment is more than 50 weight %, and the adaptation of solidfied material film also fully uprises.
((E) Photoepolymerizationinitiater initiater)
Because above-mentioned Photocurable composition contains (E) Photoepolymerizationinitiater initiater, therefore, it can consolidate light by the irradiation of light
The property changed composition solidification.(E) Photoepolymerizationinitiater initiater can be used alone, and can also be applied in combination two or more.
As (E) Photoepolymerizationinitiater initiater, acylphosphine oxide, halogenated methylation triazine, halogenated methyl Evil can be included
Diazole, imidazoles, benzoin, benzoin alkyl ether, anthraquinone, benzanthrone, benzophenone, acetophenone, thioxanthones, benzoic ether,
Acridine, azophenlyene, luxuriant titanium, alpha-aminoalkyl benzophenone, oxime and their derivative.
As benzophenone Photoepolymerizationinitiater initiater, o-benzoyl yl benzoic acid methyl esters and michler's ketone can be included
Deng.As the commercially available product of benzophenone series Photoepolymerizationinitiater initiater, EAB (manufacture of hodogaya chemical company) etc. can be included.
As the commercially available product of acylphosphine oxide class Photoepolymerizationinitiater initiater, Lucirin TPO (manufacture of BASF Co., Ltd.),
And Irgacure 819 (manufacture of Chiba SPECIALTYCHEMICALS Co., Ltd.) etc..
As the commercially available product of thioxanthene ketone class Photoepolymerizationinitiater initiater, isopropyl thioxanthone and diethyl thioxanthene can be included
Ketone etc..
As the commercially available product of alkyl phenyl ketones Photoepolymerizationinitiater initiater, Darocur 1173, Darocur can be included
2959th, Irgacure 184, Irgacure 907, Irgacure 369, Irgacure 379, Irgacure651 (BASF strain formulas
Commercial firm manufactures) and ESACURE1001M (manufacture of Lamberti companies) etc..
Suppress from further from the viewpoint of foaming, peel off and changing colour, (E) Photoepolymerizationinitiater initiater preferably comprises acyl group
Phosphine oxide class Photoepolymerizationinitiater initiater, further preferably acetophenones Photoepolymerizationinitiater initiater draw with acylphosphine oxide class photopolymerization
Both agent are sent out, also further preferably acylphosphine oxide class Photoepolymerizationinitiater initiater and the photopolymerization of bisacylphosphine oxides class trigger
Both agent.
Relative to the parts by weight of total 100 of (A) oligomer He (B) monomer, the content of (E) Photoepolymerizationinitiater initiater is preferably 1
More than parts by weight, more preferably more than 3 parts by weight, preferably below 20 parts by weight, more preferably below 15 parts by weight.(if E)
The content of Photoepolymerizationinitiater initiater is more than above-mentioned lower limit and below the above-mentioned upper limit, then can make Photocurable composition well
Carry out photocuring.
(A) parts by weight of total 100 of oligomer and (B) monomer, when Photocurable composition is free of (B) monomer, refer to (A)
The parts by weight of oligomer 100；When Photocurable composition contains (B) monomer, refer to 100 weights that (A) oligomer amounts to (B) monomer
Measure part.
((F) Thermocurable compound)
Above-mentioned Photocurable composition is preferably free of (F) Thermocurable compound, or, removed in Photocurable composition
In the weight % of composition 100 beyond solvent, contain (F) Thermocurable compound with below 5 weight %.That is, above-mentioned photo-curable
When compound contains thermal curing agents and (F) the Thermocurable compound solidified by the effects of the thermal curing agents, light is solid
In the weight % of composition 100 in the property changed composition in addition to solvent, the content of (F) Thermocurable compound is preferably 5 weight %
Below.In the present invention, when using (F) Thermocurable compound, preferably make the usage amount of (F) Thermocurable compound few.Light
The content of (F) Thermocurable compound is below 5 weight % in the weight % of composition 100 in solidification compound in addition to solvent
Composition and the weight % of composition 100 in Photocurable composition in addition to solvent in (F) Thermocurable compound
Content is, for example, that the basic physical properties of solidfied material are typically different in compositions more than 10 weight %.(F) Thermocurable compound can
So that one kind is used alone, can also be applied in combination two or more.
As (F) Thermocurable compound, (F1) epoxide etc. can be included.
Above-mentioned Photocurable composition is preferably free of (F1) epoxide, or, except molten in Photocurable composition
In the weight % of composition 100 beyond agent, contain (F1) epoxide with below 5 weight %.That is, above-mentioned photocurable compound
During containing (F1) epoxide, in the weight % of composition 100 in Photocurable composition in addition to solvent, (F1) epoxy compound
The content of thing is preferably below 5 weight %.(F1) epoxide can be solidified in the presence of thermal curing agents.In this hair
In bright, when using (F1) epoxide, the usage amount of (F1) epoxide is preferably reduced.Except molten in Photocurable composition
The content of (F1) epoxide is below 5 weight % composition and photo-curable in the weight % of composition 100 beyond agent
The content of (F1) epoxide is, for example, group more than 10 weight % in the weight % of composition 100 in composition in addition to solvent
In compound, the basic physical properties of solidfied material are typically different.(F1) epoxide can be used alone, and can also be applied in combination
It is two or more.
From the viewpoint of further suppression is peeled off and changed colour, the composition in Photocurable composition in addition to solvent
In 100 weight %, the content of (F) Thermocurable compound is more few better.Composition in Photocurable composition in addition to solvent
In 100 weight %, the content of (F) Thermocurable compound is preferably below 3 weight %, more preferably below 1 weight %, enters one
Step is preferably below 0.5 weight %, particularly preferably 0 weight % (unused).
From the viewpoint of further suppression is peeled off and changed colour, the composition in Photocurable composition in addition to solvent
In 100 weight %, the content of (F1) epoxide is more few better.Composition 100 in Photocurable composition in addition to solvent
In weight %, the content of (F1) epoxide is preferably below 3 weight %, more preferably below 1 weight %, further preferably
For below 0.5 weight %, particularly preferably 0 weight % (unused).
((G) has the sulfur-bearing alcohol-based compounds of more than 1 mercapto)
(G) by using the sulfur-bearing alcohol-based compounds with more than 1 mercapto, even if being exposed under high temperature, also can
The solidfied material film for being not likely to produce foaming and peeling off is accessed, and the high solidfied material film of heat resistance can be obtained.(G) mercapto is contained
Compound does not preferably have nitrogen-atoms.(G) sulfur-bearing alcohol-based compounds can be used alone, can also be applied in combination two kinds with
On.
As (G) sulfur-bearing alcohol-based compounds, methyl thioglycolate, 3- mercapto-propionates, 3- mercaptopropionic acids can be included
Double (the 3- of 4- methoxybutyls, 3- mercaptopropionic acid 2- ethylhexyls, 3- mercaptopropionic acids n-octyl, 3- mercaptopropionic acids stearyl ester, 1,4-
Mercaptopropionyl epoxide) butane, 1,4- double (3- sulfydryls butyryl acyloxy) butane, trimethylolethane trimethacrylate (3-thiopropionate), three
Hydroxymethyl ethane three (3- mercaptobutylates), trimethylolpropane tris (3-thiopropionate), trimethylolpropane tris (3- sulfydryls
Butyrate), pentaerythrite four (3-thiopropionate), pentaerythrite four (3- mercaptobutylates), (the 3- sulfydryls of dipentaerythritol six
Propionic ester), mercaptan carboxylic acid's ester compounds such as dipentaerythritol six (3- mercaptobutylates)；Ethanethio, 1,2- dimercaptoethanes,
The mercapto alkane compound of 1,3- dimercaptopropanes, tert-butyl mercaptan, n-dodecane mercaptan, tertiary dodecyl mercaptans etc.；2- sulfydryl second
The mercaptoalcohol compounds of alcohol, 4- sulfydryls-n-butyl alcohol etc.；Benzenethiol, benzyl mercaptan, a toluenethiol, to toluenethiol, 2- naphthalene sulphur
The mercaptan compound containing aromatic rings of alcohol etc.；(γ-mercaptopropyi) trimethoxy silane and (γ-mercaptopropyi) triethoxysilicane
Siliceous alkylthiol compounds of alkane etc. etc..
(G) sulfur-bearing alcohol-based compounds are preferably mercaptan carboxylic acid's ester compounds, more preferably secondary mercaptan compound.If use mercapto
Base carboxyl esterification compound, then because mercapto carboxy ester compounds add cross-linked structure in photocuring, therefore, it is possible to suppress solid
Volatile ingredient after change, it can further suppress to foam.If using secondary mercaptan compound, sulfur-bearing alcohol-based compounds can be suppressed
Unique smell.
(G) concrete example as sulfur-bearing alcohol-based compounds, three hydroxyl first of SC organic chemistry Co., Ltd. manufacture can be included
Double (the 3- sulfydryls of base propane three (3-thiopropionate) (TMMP), pentaerythrite four (3-thiopropionate) (PEMP), tetraethylene glycol
Propionic ester) (EGMP-4), the multifunctional primary mercaptan of dipentaerythritol six (3-thiopropionate) (DPMP) etc.；Showa electrician's strain formula
Double (3- sulfydryls butyryl acyloxy) butane of pentaerythrite four (3- mercaptobutylates) (Karenz MT PE1), 1,4- of commercial firm's manufacture
The multifunctional secondary mercaptan of (Karenz MT BD1) etc.；The β-mercaptopropionic acid (BMPA) of SC organic chemistry Co., Ltd. manufacture, first
Base -3-thiopropionate (MPM), 2- ethylhexyls -3-thiopropionate (EHMP), n-octyl -3-thiopropionate (NOMP),
Simple function mercaptan such as methoxybutyl -3-thiopropionate (MBMP), stearyl -3-thiopropionate (STMP) etc..
In the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, (G) sulfur-bearing alcohol-based compounds contain
Amount is preferably more than 0.1 weight %, more preferably more than 0.5 weight %, preferably below 10 weight %, and more preferably 5 weights
Measure below %.The content of (if G) sulfur-bearing alcohol-based compounds is more than above-mentioned lower limit and below the above-mentioned upper limit, in solidfied material film
Foaming, stripping and discoloration be further suppressed.In addition, the content of (if G) sulfur-bearing alcohol-based compounds is the above-mentioned upper limit
Hereinafter, then the gelation of Photocurable composition is not easy to carry out in preserving.Under the content of (if G) sulfur-bearing alcohol-based compounds is above-mentioned
More than limit, then curability further uprises.
Relative to the parts by weight of total 100 of (A) oligomer and (B) monomer, the content of (G) sulfur-bearing alcohol-based compounds is preferably
More than 0.2 parts by weight, more preferably more than 1 parts by weight, preferably below 20 parts by weight, more preferably below 10 parts by weight, enter
One step is preferably below 6 parts by weight.The content of (if G) sulfur-bearing alcohol-based compounds be above-mentioned lower limit more than and the above-mentioned upper limit with
Under, then the foaming in solidfied material film, stripping and discoloration is further suppressed.In addition, (if G) sulfur-bearing alcohol-based compounds
Content is below the above-mentioned upper limit, then the gelation of Photocurable composition is not easy to carry out in preservation.(if G) sulfur-bearing alcohol-based compounds
Content for more than above-mentioned lower limit, then curability further uprises.
(other compositions)
From the viewpoint of high pencil hardness and high-fire resistance is had concurrently, above-mentioned Photocurable composition preferably comprises antioxygen
Agent.
As above-mentioned antioxidant, phenol kind antioxidant, sulfur type antioxidant and Phosphorus antioxidant etc. can be included.Above-mentioned benzene
Phenolic antioxidant is the antioxidant with phenol backbone.Above-mentioned sulfur type antioxidant is the antioxidant containing sulphur atom.It is above-mentioned Phosphorus
Antioxidant is the antioxidant containing phosphorus atoms.
From the viewpoint of further raising antioxygenic property, high pencil hardness and high-fire resistance effectively improve,
Above-mentioned antioxidant is preferably phenol kind antioxidant or Phosphorus antioxidant.
As above-mentioned phenol kind antioxidant, 2,6- di-t-butyl -s paracresol (BHT), Butylated hydroxy benzene first can be included
Ether (BHA), 2,6- di-t-butyl -4- ethyl -phenols, stearyl-β-(3,5- di-tert-butyl-hydroxy phenyls) propionic ester,
2,2 '-di-2-ethylhexylphosphine oxide-(4- methyl -6- butylphenols), 2,2 '-di-2-ethylhexylphosphine oxide-(4- ethyl -6- tert-butyl phenols), 4,4 '-fourth
Pitch base-bis- (3 methy 6 tert butyl phenols), 1,1,3- tri--(2- methyl-hydroxyl -5- tert-butyl-phenyls) butane, four [methylenes
Base -3- (3 ', 5 '-butyl -4- hydroxy phenyls) propionic ester] methane, 1,3,3- tri--(2- methyl -4- hydroxyl -5- tert-butyl phenols)
Butane, 1,3,5- trimethyls -2,4,6- three (3,5- di-tert-butyl-4-hydroxyl benzyls) benzene, double (3,3 '-tert-butyl phenol) butyric acid
Glycol ester and double (3- tertiary butyl-4-hydroxy -5- methyl benzenpropanoic acid) ethylenebis (ethylene oxide) etc..It is preferred that use these
It is more than one or both of antioxidant.
As above-mentioned Phosphorus antioxidant, tridecyl phosphite, three (tridecyl) phosphite esters, triphen can be included
Base phosphite ester, trisnonylphenyl phosphite, double (tridecyl) pentaerythritol diphosphites, double (decyl) pentaerythrites
Diphosphites, three (2,4- di-tert-butyl-phenyls) phosphite esters, double (2,4- di-t-butyl -6- aminomethyl phenyls) ethyl ester phosphorous
Acid, three (2,4- di-tert-butyl-phenyls) phosphite esters and 2,2 '-di-2-ethylhexylphosphine oxide (4,6- di-t-butyl -1- phenoxy groups) (2- second
Base hexyloxy) phosphorus etc..It is preferred that more than using one or both of these antioxidant.
From the viewpoint of high pencil hardness and high-fire resistance is had concurrently, above-mentioned antioxidant is preferably phenol kind antioxidant, more
Preferably Hinered phenols antioxidant, particularly preferably pentaerythrite four [3- (3,5- di-tert-butyl-hydroxy phenyl) propionic ester].
Relative to the parts by weight of (D) Chinese white 100, the content of above-mentioned antioxidant is preferably more than 0.1 parts by weight, more preferably
More than 1 parts by weight, preferably below 10 parts by weight, more preferably below 6 parts by weight.If the content of above-mentioned antioxidant is above-mentioned
More than lower limit and below the above-mentioned upper limit, then high pencil hardness and high heat resistance can be had concurrently.
From the viewpoint of further raising pencil hardness, above-mentioned Photocurable composition preferably comprises defoamer.
As above-mentioned defoamer, KS-66 and KS-69 (Shin-Etsu Chemial Co., Ltd's manufacture) etc. can be included.
In the weight % of composition 100 in above-mentioned Photocurable composition in addition to solvent, the content of above-mentioned defoamer is preferred
For more than 0.1 weight %, more preferably more than 0.5 weight %, preferably below 5 weight %, more preferably below 3 weight %.
If the content of above-mentioned defoamer is more than above-mentioned lower limit, the uniformity of solidfied material film uprises, and the pencil hardness of solidfied material film is more
Further uprise.If the content of above-mentioned defoamer is below the above-mentioned upper limit, curability further uprises.
Above-mentioned Photocurable composition preferably comprises stabilizer.By making above-mentioned Photocurable composition contain stabilizer,
Even if using (G) sulfur-bearing alcohol-based compounds, the gelation of Photocurable composition and viscosity B coefficent also more progressive one in keeping
Step is suppressed.Specifically, as stabilizer, such as Unexamined Patent 5-155987 publications, JP 2012-17448 can be used
Compound described in number publication etc..
Above-mentioned Photocurable composition, can also be inorganic containing solvent, in addition to Chinese white in addition to mentioned component
Filler, organic filler, colouring agent, polymerization inhibitor, chain-transferring agent, ultra-violet absorber, levelling agent, surfactant, increasing are slided
Agent, anticaking agent, wax, screening agent, deodorant, aromatic, preservative, antiseptic, antistatic additive and adaptation imparting agent etc..
As above-mentioned adaptation imparting agent, silane coupler etc. can be included.
Above-mentioned Photocurable composition can contain solvent.Above-mentioned solvent can be used alone, and can also combine makes
With two or more.
In general, above-mentioned solvent is organic solvent.As above-mentioned organic solvent, methyl ethyl ketone, hexamethylene can be included
The assimilation compound such as ketone；The molten fibre of the aromatic hydrocarbon compounds such as toluene, dimethylbenzene, durol, cellosolve, methyl cellosolve, butyl
Agent, carbitol, methyl carbitol, butyl carbitol, propylene glycol monomethyl ether, DPGME, DPG diethyl
The glycol ether compounds such as base ether, tripropylene glycol monomethyl ether, ethyl acetate, butyl acetate, butyl lactate, cellosolve acetate,
Butylacetic acid cellosolve, carbitol acetate, acetate of butyl carbitol, propylene glycol monomethyl ether, diethylene glycol list
The ester compounds such as monoethyl ether acetate, DPGME acetic acid esters, propylene carbonate；The aliphatic hydrocarbons such as octane, decane
Compound；The petroleum solvents such as petroleum ether, naphtha and dibasic acid ester etc..Above-mentioned dibasic acid ester is the solvent for being referred to as DBE.
Above-mentioned Photocurable composition is preferably free of solvent, or the solvent containing below 50 weight %.The content of solvent is got over
It is few better.In the above-mentioned weight % of Photocurable composition 100, the content of above-mentioned solvent is preferably below 5 weight %.
[manufacture method of electronic unit and electronic unit]
The manufacture method of electronic unit of the present invention, it includes：It is coated with the surface of electronic component body above-mentioned
Photocurable composition, so as to form the process of composition layer；And to combinations thereof nitride layer irradiation light, so as to form solidfied material
The process of film.In the manufacture method of electronic unit of the present invention, preferably without in order to form above-mentioned solidfied material film and
The operation developed to combinations thereof nitride layer.Combinations thereof nitride layer is preferably resist layer, and above-mentioned solidfied material film is preferably anti-
Lose agent film, more preferably soldering-resistance layer.Above-mentioned Photocurable composition is suitable for forming resist film, is particularly suited for forming resistance
Weld film.
Because above-mentioned Photocurable composition is suitable for forming solidfied material film without development, it is therefore preferable that making
State Photocurable composition to be partly coated on the surface of electronic component body, and be coated on multiple positions.
From the viewpoint of the heat deterioration for preventing electronic component body, preferably without in order to form above-mentioned solidfied material film and
Combinations thereof nitride layer is set to carry out the operation of heat cure by the effect of thermal curing agents.
Hereinafter, referring to the drawings, the manufacture method of the specific electronic unit of the present invention is illustrated.Described below
In embodiment, combinations thereof nitride layer is resist layer, and above-mentioned solidfied material film is resist film.Make to form resist film
With non-developable resist Photocurable composition.
First, as shown in Fig. 1 (a), coating object Part 11 is prepared.Coating object Part 11 is electronic component body.Make
To be coated with object Part 11, using substrate 11A, multiple electrodes 11B is set on substrate 11A surface.
Then, as shown in Fig. 1 (b), on the surface of coating object Part 11, it is coated with non-developable resist photo-curable
Composition, form resist layer 12 (composition layer).In Fig. 1 (b), by above-mentioned non-developable resist Photocurable composition
Partly it is coated on the surface of coating object Part 11, and is coated on multiple positions, forms multiple resist layers 12.Specifically
Ground, between the multiple electrodes 11B on substrate 11A surface, form multiple resist layers 12.Resist layer 12 is for example, against corrosion
Pattern.For example, for resist layer 12, it is assumed that using conventional developable anti-corrosion agent composition when, only with it is residual after development
Position corresponding to the resist layer part stayed and formed is formed.For resist layer 12, conventional developable resist is used
Composition, it will not be formed with by development and the corresponding position in the resist layer part that is removed.
The coating method of Photocurable composition, such as the coating method carried out using distributor can be included, utilize net
The coating method that version printing is carried out and the coating method using ink discharge device progress etc..From manufacture efficiency it is excellent in terms of examine
Consider, preferably screen painting.The non-developable resist Photocurable composition of preferred pair carries out pattern printing.
Then, to the irradiation light of resist layer 12.For example, one opposite with coating object Part 11 side from resist layer 12
Side, to the irradiation light of resist layer 12.The result, as shown in Fig. 1 (c), resist layer 12 carries out photocuring, forms resist film 2
(solidfied material film).As a result, obtained on the surface of coating object Part 11 (electronic component body) formed with resist film 2
Electronic unit 1.
An in addition, example of the manufacture method of the electronic unit with the resist film illustrated using Fig. 1 (a)~Fig. 1 (c)
Son, the manufacture method of electronic unit can suitably change.When manufacturing electronic unit, preferably without in order to form resist film
The operation developed.
It is in addition, more using the situation of developable anti-corrosion agent composition at present.Combined using the developable resist of negativity
During thing, as shown in Fig. 2 (a), for example, preparing with the substrate 111A and electrode 111B set on substrate 111A surface
Coating object Part 111.Then, as shown in Fig. 2 (b), resist layer is integrally formed on the surface of coating object Part 111
112.Then, as shown in Fig. 2 (c), via blindage 113, only to the irradiation light of resist layer 112 on electrode 111B.Afterwards, as schemed
Shown in 2 (d), developed, part removes on electrode 111B and the resist layer 112 of non-irradiation light.Part removes against corrosion
After oxidant layer 112, make the heat cure of resist layer 112 of residual.As a result, as shown in Fig. 2 (e), in the coating (electricity of object Part 111
Subassembly main body) surface on obtain the electronic unit 101 formed with resist film 102.
When so, using developable anti-corrosion agent composition, the formation efficiency of resist film and the manufacture effect of electronic unit
Rate is poor.Further, it is necessary to be developed.
In contrast, by using Photocurable composition of the present invention, it is possible to increase solidfied material film (resist film
Deng) formation efficiency and electronic unit manufacture efficiency.In addition, it is not necessary that developed.
In addition, in the present invention, as electronic unit, it can prepare with above-mentioned solidfied material film as the anti-of reflection layer
Penetrate plate.
Hereinafter, embodiment and comparative example are enumerated, illustrates the present invention.The present invention is not limited to following implementation
Example.
(synthesis example)
The synthesis example 1 of epoxy (methyl) acrylate：
By bisphenol A type epoxy resin (" YD-127 " of Nippon Steel ＆ Sumitomo Metal Corporation's manufacture) 100g and acrylic acid
28g is put into reaction vessel, adds hydroquinone monomethyl ether 0.06g and TBAB 0.64g, reaction 4 is carried out at 90 DEG C
Hour.Then, toluene 300ml and water 200ml and sodium carbonate 1g is added, is stirred 1 hour at normal temperatures.Then, aqueous phase will be entered
Row split-phase simultaneously removes.Thenardite 10g is added in toluene phase, is stirred 1 hour at normal temperatures.Then, awns is removed by filtration
Nitre, toluene is removed under reduced pressure, obtains 120g object epoxy acrylate 1.
The weight average molecular weight of resulting condensation product is 900, acid number 10mgKOH/g.
The synthesis example 2 of epoxy (methyl) acrylate：
By bisphenol A type epoxy resin (" YD-134 " of Nippon Steel ＆ Sumitomo Metal Corporation's manufacture) 100g and acrylic acid
22g is put into reaction vessel, adds hydroquinone monomethyl ether 0.06g and TBAB 0.64g, reaction 4 is carried out at 90 DEG C
Hour.Then, toluene 300ml and water 200ml and sodium carbonate 2g is added, is stirred 1 hour at normal temperatures.Then, aqueous phase is carried out
Split-phase simultaneously removes.Thenardite 10g is added in toluene phase, is stirred 1 hour at normal temperatures.Afterwards, saltcake is removed by filtration,
Toluene is removed under reduced pressure, obtains 120g object epoxy acrylate 2.
The weight average molecular weight of obtained condensation product is 1700, acid number 1mgKOH/g.
The synthesis example 3 of epoxy (methyl) acrylate：
By bisphenol A type epoxy resin (" YD-011 " of Nippon Steel ＆ Sumitomo Metal Corporation's manufacture) 100g and acrylic acid
18g is put into reaction vessel, adds hydroquinone monomethyl ether 0.06g and TBAB 0.64g, reaction 4 is carried out at 90 DEG C
Hour.Then, toluene 300ml and water 200ml and sodium carbonate 2g is added, is stirred 1 hour at normal temperatures.Then, aqueous phase is carried out
Split-phase simultaneously removes.Thenardite 10g is added in toluene phase, is stirred 1 hour at normal temperatures.Then, saltcake is removed by filtration,
Toluene is removed under reduced pressure, obtains 100g object epoxy acrylate 3.
The weight average molecular weight of resulting condensation product is 3000, acid number 1mgKOH/g.
The synthesis example 4 of epoxy (methyl) acrylate：
By phenol aldehyde type epoxy resin (" YDCN-704 " of Nippon Steel ＆ Sumitomo Metal Corporation's manufacture) 100g and acrylic acid
22g is put into reaction vessel, adds hydroquinone monomethyl ether 0.06g and TBAB 0.64g, reaction 4 is carried out at 90 DEG C
Hour.Then, toluene 300ml and water 200ml and sodium carbonate 2g is added, is stirred 1 hour at normal temperatures.Then, aqueous phase is carried out
Split-phase simultaneously removes.Thenardite 10g is added in toluene phase, is stirred 1 hour at normal temperatures.Then, saltcake is removed by filtration,
Toluene is removed under reduced pressure, obtains 110g object epoxy acrylate 4.
The weight average molecular weight of obtained condensation product is 1900, acid number 1mgKOH/g.
(embodiment 1~14 and comparative example 1~3)
(1) preparation of non-developable resist Photocurable composition
According to the gradation composition shown in the use level cooperation table 1 below shown in following table 1,2,2, non-development is prepared
Type resist Photocurable composition.
(2) preparation of electronic unit
Preparation is laminated with the substrate of copper foil on 100mm × 100mm × thickness 0.8mm FR-4.Utilize on the substrate
MD-4S-UFF (manufacture of 3M companies, numbering：1000) after being processed by shot blasting, by screen painting method, 255 meshes are used
The plate of Polyester bias manufactures, is printed, shape using blindage pattern to non-developable resist Photocurable composition
Into resist layer.After printing, using ultraviolet lamp, with 500mJ/cm2Ultraviolet illumination using passing through belt-conveying
Machine formula exposer make it that irradiation energy is 1500mJ/cm to the ultraviolet that resist layer illumination wavelength is 365nm2, made
For the resist film of determination sample.The thickness of obtained resist film is 20 μm.
(evaluation)
(1) viscosity
To obtained Photocurable composition, E type viscosimeters are used：Toki Sangyo Co., Ltd.'s manufacture
" VISCOMETER TV-22 ", viscosity is determined under conditions of 25 DEG C and 10rpm.
[criterion of viscosity]
A：More than 1Pas and below 30Pas
B：Less than 1Pas or more than 30Pas
(2) hardness (pencil hardness)
To the resist film of resulting electronic unit, on the basis of JIS K5600-5-4, pencil hardness is obtained.
(3) size of the scar in hardness (pencil hardness) experiment
To the resist film of the electronic unit of embodiment, in the experiment of above-mentioned (2) hardness (pencil hardness), evaluation uses
The size of scar during 4H pencils.Using embodiment 1 as STD, the size of the scar of other embodiment is evaluated.
[criterion of the size of scar]
A：Scar is very small compared with embodiment 1 (STD)
B：Scar is slightly smaller compared with embodiment 1 (STD)
C：Embodiment 1 (STD) is same degree with embodiment 1 (STD)
D：Scar is larger compared with embodiment 1 (STD)
-：Do not evaluate
(4) reflectivity
To the resist film of obtained electronic unit, using color colorimeter, (KONICA MINOLTA Co., Ltd. manufactures
" CR-400 ") measure reflectivity Y, judged with following benchmark.
[criterion of reflectivity]
○：More than 80%
×：Less than 80%
(5) adaptation (checkerboard test)
To resulting electronic unit, confirmed with lattice tape test (JIS 5600) is drawn, confirm adaptation.Use icking tool
The gridiron pattern that 20 lattice are made in solidfied material is included in 1mm intervals, glassine paper is fully then pasted to the solidfied material with cut out portion
Adhesive tape (JIS Z1522), with one end of 60 degree of angle strength stripping tape, confirm exfoliated state.According to JIS to exfoliated state
Classified.In the case of being categorized as 0,1,2, the grid number of stripping is 0.
Composition and result are represented in following tables 1,2.
Claims (15)
1. a kind of Photocurable composition, it contains：Oligomer, nitrogen-containing compound, Chinese white and Photoepolymerizationinitiater initiater,
The oligomer is with the ethylenic unsaturated bond of more than 2 but does not have carboxyl,
Under 25 DEG C and 10rpm, the viscosity of Photocurable composition is more than 1Pas and below 30Pas.
2. Photocurable composition according to claim 1, wherein, when Photocurable composition contains epoxide,
In the weight % of composition 100 in Photocurable composition in addition to solvent, the content of epoxide is below 5 weight %.
3. Photocurable composition according to claim 1, wherein, Photocurable composition includes thermal curing agents and led to
When crossing the Thermocurable compound that the effects of the thermal curing agents solidifies, in Photocurable composition in addition to solvent into
Divide in 100 weight %, the content of the Thermocurable compound is below 5 weight %.
4. according to Photocurable composition according to any one of claims 1 to 3, wherein, the nitrogen-containing compound is with 1
The amide-containing monomer of ethylenic unsaturated bond more than individual or the monomer containing morpholinyl with the ethylenic unsaturated bond of more than 1.
5. according to Photocurable composition according to any one of claims 1 to 4, wherein, the nitrogen-containing compound is diformazan
Base (methyl) acrylamide, (methyl) acryloyl morpholine, isopropyl (methyl) acrylamide, diethyl (methyl) acrylamide,
Dimethylaminopropyl (methyl) acrylamide, (3- acrylamide propyls) trimethyl ammonia chloride ammonium salt or ethoxy (methyl) third
Acrylamide.
6. the Photocurable composition according to claim 4 or 5, wherein, in Photocurable composition in addition to solvent
In the weight % of composition 100, the content of the nitrogen-containing compound is more than 1 weight % and below 40 weight %.
7. according to Photocurable composition according to any one of claims 1 to 3, wherein, the nitrogen-containing compound is tetrazolium
Compound, imidazolium compounds, triazole compounds, isocyanate compound or melamine compound.
8. Photocurable composition according to claim 7, wherein, the composition in Photocurable composition in addition to solvent
In 100 weight %, the content of the nitrogen-containing compound is more than 0.1 weight % and is below 5 weight %.
9. according to Photocurable composition according to any one of claims 1 to 8, wherein, the nitrogen-containing compound be containing
Quinoline based compound or isocyanate compound.
10. according to Photocurable composition according to any one of claims 1 to 9, after it is solidified by light irradiation
Use, and for not carrying out forming solidfied material film with developing to it.
11. according to Photocurable composition according to any one of claims 1 to 10, it is used to partly be coated on coating pair
As on parts surface, and it is coated on multiple positions.
12. the Photocurable composition according to any one of claim 1~11, it is not used in the work by thermal curing agents
With carrying out heat cure.
13. a kind of preparation method of electronic unit, it includes：
The Photocurable composition any one of claim 1~12 is coated with the surface of electronic component body, so as to
The process for forming composition layer；And
To the composition layer irradiation light, so as to form the process of solidfied material film,
Without the operation developed to form the solidfied material film to the composition layer.
14. the preparation method of electronic unit according to claim 13, wherein, make the Photocurable composition partly
It is coated on the electronic component body surface, and is coated on multiple positions.
15. the preparation method of the electronic unit according to claim 13 or 14, wherein, without in order to form the solidification
Thing film and make the composition layer pass through thermal curing agents effect carry out heat cure operation.
Applications Claiming Priority (3)
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|---|---|---|---|
| JP2015256978 | 2015-12-28 | ||
| JP2015-256978 | 2015-12-28 | ||
| PCT/JP2016/088746 WO2017115755A1 (en) | 2015-12-28 | 2016-12-26 | Photocurable composition and method for producing electronic component |
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| Publication Number | Publication Date |
|---|---|
| CN107709371A true CN107709371A (en) | 2018-02-16 |
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ID=59225088
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| CN201680038410.2A Pending CN107709371A (en) | 2015-12-28 | 2016-12-26 | The manufacture method of Photocurable composition and electronic unit |
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|---|---|
| JP (2) | JP6221010B1 (en) |
| KR (1) | KR20180099456A (en) |
| CN (1) | CN107709371A (en) |
| TW (1) | TW201736421A (en) |
| WO (1) | WO2017115755A1 (en) |
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| TWI808187B (en) * | 2018-06-08 | 2023-07-11 | 日商東伸工業股份有限公司 | Screen printing device and screen printing method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010144090A (en) * | 2008-12-19 | 2010-07-01 | Idemitsu Technofine Co Ltd | Ultraviolet-curing type coating agent and molded product |
| CN103901725A (en) * | 2014-04-19 | 2014-07-02 | 长兴电子（苏州）有限公司 | Light-cured resin composition |
| CN104017403A (en) * | 2014-05-28 | 2014-09-03 | 江苏巨珩新材料科技有限公司 | Solvent-free UV paint applied to aluminium plate surfaces and preparation method thereof |
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| IT1309578B1 (en) * | 1998-02-27 | 2002-01-24 | Ciba Sc Holding Ag | PIGMENTED PHOTOINDURABLE COMPOSITION. |
| JP5667080B2 (en) | 2009-11-30 | 2015-02-12 | 株式会社タムラ製作所 | Curable composition, cured product thereof and use thereof |
| JP5325805B2 (en) | 2010-01-29 | 2013-10-23 | 株式会社タムラ製作所 | Photosensitive resin composition and printed wiring board using cured film thereof |
| JP5302935B2 (en) * | 2010-06-28 | 2013-10-02 | 十条ケミカル株式会社 | UV curable ink for light guide plate and light guide plate |
| JP6299159B2 (en) * | 2013-11-06 | 2018-03-28 | セイコーエプソン株式会社 | Ultraviolet curable composition and recorded matter |
| WO2016002923A1 (en) * | 2014-07-04 | 2016-01-07 | 積水化学工業株式会社 | Photocurable composition and method for manufacturing electronic component |
| JP6286395B2 (en) * | 2015-08-05 | 2018-02-28 | 太陽インキ製造株式会社 | Curable resin composition, dry film, cured product and printed wiring board |
| JP2016160372A (en) * | 2015-03-03 | 2016-09-05 | 東洋インキＳｃホールディングス株式会社 | Active energy ray-polymerizable resin composition for optical three-dimensional molding, and three-dimensional molded object |
| JP2016199671A (en) * | 2015-04-09 | 2016-12-01 | 積水化学工業株式会社 | Photo/moisture curable resin composition |
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2016
- 2016-12-26 CN CN201680038410.2A patent/CN107709371A/en active Pending
- 2016-12-26 KR KR1020177035722A patent/KR20180099456A/en unknown
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- 2016-12-26 WO PCT/JP2016/088746 patent/WO2017115755A1/en active Application Filing
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010144090A (en) * | 2008-12-19 | 2010-07-01 | Idemitsu Technofine Co Ltd | Ultraviolet-curing type coating agent and molded product |
| CN103901725A (en) * | 2014-04-19 | 2014-07-02 | 长兴电子（苏州）有限公司 | Light-cured resin composition |
| CN104017403A (en) * | 2014-05-28 | 2014-09-03 | 江苏巨珩新材料科技有限公司 | Solvent-free UV paint applied to aluminium plate surfaces and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI808187B (en) * | 2018-06-08 | 2023-07-11 | 日商東伸工業股份有限公司 | Screen printing device and screen printing method |
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| JPWO2017115755A1 (en) | 2017-12-28 |
| JP2018024884A (en) | 2018-02-15 |
| WO2017115755A1 (en) | 2017-07-06 |
| TW201736421A (en) | 2017-10-16 |
| JP6221010B1 (en) | 2017-10-25 |
| KR20180099456A (en) | 2018-09-05 |
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Application publication date: 20180216 |