CN115368832A - Mini LED packaging adhesive film and preparation method thereof - Google Patents
Mini LED packaging adhesive film and preparation method thereof Download PDFInfo
- Publication number
- CN115368832A CN115368832A CN202211118794.2A CN202211118794A CN115368832A CN 115368832 A CN115368832 A CN 115368832A CN 202211118794 A CN202211118794 A CN 202211118794A CN 115368832 A CN115368832 A CN 115368832A
- Authority
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- China
- Prior art keywords
- acrylate
- film
- mini led
- oca
- semi
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 238000004806 packaging method and process Methods 0.000 title claims abstract description 21
- 239000002313 adhesive film Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000009792 diffusion process Methods 0.000 claims abstract description 21
- 239000000178 monomer Substances 0.000 claims abstract description 20
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000003292 glue Substances 0.000 claims abstract description 12
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- 238000002834 transmittance Methods 0.000 claims abstract description 9
- 230000002745 absorbent Effects 0.000 claims abstract description 8
- 239000002250 absorbent Substances 0.000 claims abstract description 8
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 7
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 239000003999 initiator Substances 0.000 claims abstract description 5
- 230000001678 irradiating effect Effects 0.000 claims abstract description 4
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N alpha-methacrylic acid Natural products CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 13
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 claims description 8
- -1 dihexyl acrylate Chemical compound 0.000 claims description 6
- DSTUKHPLWATFCG-UHFFFAOYSA-N (2-benzoylphenyl) prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1C(=O)C1=CC=CC=C1 DSTUKHPLWATFCG-UHFFFAOYSA-N 0.000 claims description 4
- PSGCQDPCAWOCSH-UHFFFAOYSA-N (4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl) prop-2-enoate Chemical compound C1CC2(C)C(OC(=O)C=C)CC1C2(C)C PSGCQDPCAWOCSH-UHFFFAOYSA-N 0.000 claims description 4
- 239000012956 1-hydroxycyclohexylphenyl-ketone Substances 0.000 claims description 4
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims description 4
- FIHBHSQYSYVZQE-UHFFFAOYSA-N 6-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCOC(=O)C=C FIHBHSQYSYVZQE-UHFFFAOYSA-N 0.000 claims description 4
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- MQDJYUACMFCOFT-UHFFFAOYSA-N bis[2-(1-hydroxycyclohexyl)phenyl]methanone Chemical compound C=1C=CC=C(C(=O)C=2C(=CC=CC=2)C2(O)CCCCC2)C=1C1(O)CCCCC1 MQDJYUACMFCOFT-UHFFFAOYSA-N 0.000 claims description 4
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 4
- 239000006096 absorbing agent Substances 0.000 claims description 3
- KKMCJEPDHKUQRC-UHFFFAOYSA-N (2-benzoylphenyl) 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1C(=O)C1=CC=CC=C1 KKMCJEPDHKUQRC-UHFFFAOYSA-N 0.000 claims description 2
- WXPWZZHELZEVPO-UHFFFAOYSA-N (4-methylphenyl)-phenylmethanone Chemical compound C1=CC(C)=CC=C1C(=O)C1=CC=CC=C1 WXPWZZHELZEVPO-UHFFFAOYSA-N 0.000 claims description 2
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 claims description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N 1,4-butanediol Substances OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 2
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 2
- XLPJNCYCZORXHG-UHFFFAOYSA-N 1-morpholin-4-ylprop-2-en-1-one Chemical compound C=CC(=O)N1CCOCC1 XLPJNCYCZORXHG-UHFFFAOYSA-N 0.000 claims description 2
- VOBUAPTXJKMNCT-UHFFFAOYSA-N 1-prop-2-enoyloxyhexyl prop-2-enoate Chemical compound CCCCCC(OC(=O)C=C)OC(=O)C=C VOBUAPTXJKMNCT-UHFFFAOYSA-N 0.000 claims description 2
- LRZPQLZONWIQOJ-UHFFFAOYSA-N 10-(2-methylprop-2-enoyloxy)decyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCCCCCCCCOC(=O)C(C)=C LRZPQLZONWIQOJ-UHFFFAOYSA-N 0.000 claims description 2
- RHNJVKIVSXGYBD-UHFFFAOYSA-N 10-prop-2-enoyloxydecyl prop-2-enoate Chemical compound C=CC(=O)OCCCCCCCCCCOC(=O)C=C RHNJVKIVSXGYBD-UHFFFAOYSA-N 0.000 claims description 2
- YAJYJWXEWKRTPO-UHFFFAOYSA-N 2,3,3,4,4,5-hexamethylhexane-2-thiol Chemical compound CC(C)C(C)(C)C(C)(C)C(C)(C)S YAJYJWXEWKRTPO-UHFFFAOYSA-N 0.000 claims description 2
- OWDBMKZHFCSOOL-UHFFFAOYSA-N 2-[2-[2-(2-methylprop-2-enoyloxy)propoxy]propoxy]propyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)COC(C)COC(C)COC(=O)C(C)=C OWDBMKZHFCSOOL-UHFFFAOYSA-N 0.000 claims description 2
- IEVADDDOVGMCSI-UHFFFAOYSA-N 2-hydroxybutyl 2-methylprop-2-enoate Chemical compound CCC(O)COC(=O)C(C)=C IEVADDDOVGMCSI-UHFFFAOYSA-N 0.000 claims description 2
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- AKVUWTYSNLGBJY-UHFFFAOYSA-N 2-methyl-1-morpholin-4-ylprop-2-en-1-one Chemical compound CC(=C)C(=O)N1CCOCC1 AKVUWTYSNLGBJY-UHFFFAOYSA-N 0.000 claims description 2
- GNSFRPWPOGYVLO-UHFFFAOYSA-N 3-hydroxypropyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCCCO GNSFRPWPOGYVLO-UHFFFAOYSA-N 0.000 claims description 2
- QZPSOSOOLFHYRR-UHFFFAOYSA-N 3-hydroxypropyl prop-2-enoate Chemical compound OCCCOC(=O)C=C QZPSOSOOLFHYRR-UHFFFAOYSA-N 0.000 claims description 2
- NDWUBGAGUCISDV-UHFFFAOYSA-N 4-hydroxybutyl prop-2-enoate Chemical compound OCCCCOC(=O)C=C NDWUBGAGUCISDV-UHFFFAOYSA-N 0.000 claims description 2
- JHWGFJBTMHEZME-UHFFFAOYSA-N 4-prop-2-enoyloxybutyl prop-2-enoate Chemical compound C=CC(=O)OCCCCOC(=O)C=C JHWGFJBTMHEZME-UHFFFAOYSA-N 0.000 claims description 2
- NQSLZEHVGKWKAY-UHFFFAOYSA-N 6-methylheptyl 2-methylprop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C(C)=C NQSLZEHVGKWKAY-UHFFFAOYSA-N 0.000 claims description 2
- IUNVCWLKOOCPIT-UHFFFAOYSA-N 6-methylheptylsulfanyl 2-hydroxyacetate Chemical compound CC(C)CCCCCSOC(=O)CO IUNVCWLKOOCPIT-UHFFFAOYSA-N 0.000 claims description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 2
- SXNICUVVDOTUPD-UHFFFAOYSA-N CC1=CC(C)=CC(C)=C1C(=O)P(=O)C1=CC=CC=C1 Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)C1=CC=CC=C1 SXNICUVVDOTUPD-UHFFFAOYSA-N 0.000 claims description 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 claims description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 claims description 2
- 229920000604 Polyethylene Glycol 200 Polymers 0.000 claims description 2
- IAXXETNIOYFMLW-COPLHBTASA-N [(1s,3s,4s)-4,7,7-trimethyl-3-bicyclo[2.2.1]heptanyl] 2-methylprop-2-enoate Chemical compound C1C[C@]2(C)[C@@H](OC(=O)C(=C)C)C[C@H]1C2(C)C IAXXETNIOYFMLW-COPLHBTASA-N 0.000 claims description 2
- VEBCLRKUSAGCDF-UHFFFAOYSA-N ac1mi23b Chemical compound C1C2C3C(COC(=O)C=C)CCC3C1C(COC(=O)C=C)C2 VEBCLRKUSAGCDF-UHFFFAOYSA-N 0.000 claims description 2
- CSCPPACGZOOCGX-UHFFFAOYSA-N acetone Substances CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 2
- 125000005396 acrylic acid ester group Chemical group 0.000 claims description 2
- WURBFLDFSFBTLW-UHFFFAOYSA-N benzil Chemical compound C=1C=CC=CC=1C(=O)C(=O)C1=CC=CC=C1 WURBFLDFSFBTLW-UHFFFAOYSA-N 0.000 claims description 2
- RWCCWEUUXYIKHB-UHFFFAOYSA-N benzophenone Chemical compound C=1C=CC=CC=1C(=O)C1=CC=CC=C1 RWCCWEUUXYIKHB-UHFFFAOYSA-N 0.000 claims description 2
- 239000012965 benzophenone Substances 0.000 claims description 2
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 2
- 229910000420 cerium oxide Inorganic materials 0.000 claims description 2
- VFHVQBAGLAREND-UHFFFAOYSA-N diphenylphosphoryl-(2,4,6-trimethylphenyl)methanone Chemical compound CC1=CC(C)=CC(C)=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 VFHVQBAGLAREND-UHFFFAOYSA-N 0.000 claims description 2
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 2
- YMCOIFVFCYKISC-UHFFFAOYSA-N ethoxy-[2-(2,4,6-trimethylbenzoyl)phenyl]phosphinic acid Chemical compound CCOP(O)(=O)c1ccccc1C(=O)c1c(C)cc(C)cc1C YMCOIFVFCYKISC-UHFFFAOYSA-N 0.000 claims description 2
- LNCPIMCVTKXXOY-UHFFFAOYSA-N hexyl 2-methylprop-2-enoate Chemical compound CCCCCCOC(=O)C(C)=C LNCPIMCVTKXXOY-UHFFFAOYSA-N 0.000 claims description 2
- LNMQRPPRQDGUDR-UHFFFAOYSA-N hexyl prop-2-enoate Chemical compound CCCCCCOC(=O)C=C LNMQRPPRQDGUDR-UHFFFAOYSA-N 0.000 claims description 2
- 229940119545 isobornyl methacrylate Drugs 0.000 claims description 2
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 claims description 2
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- OTLDLKLSNZMTTA-UHFFFAOYSA-N octahydro-1h-4,7-methanoindene-1,5-diyldimethanol Chemical compound C1C2C3C(CO)CCC3C1C(CO)C2 OTLDLKLSNZMTTA-UHFFFAOYSA-N 0.000 claims description 2
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 claims description 2
- 229920006280 packaging film Polymers 0.000 claims description 2
- 239000012785 packaging film Substances 0.000 claims description 2
- LYXOWKPVTCPORE-UHFFFAOYSA-N phenyl-(4-phenylphenyl)methanone Chemical compound C=1C=C(C=2C=CC=CC=2)C=CC=1C(=O)C1=CC=CC=C1 LYXOWKPVTCPORE-UHFFFAOYSA-N 0.000 claims description 2
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 239000008393 encapsulating agent Substances 0.000 claims 2
- 239000000463 material Substances 0.000 claims 1
- 238000001723 curing Methods 0.000 abstract description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 4
- 239000012298 atmosphere Substances 0.000 abstract description 3
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- 239000011324 bead Substances 0.000 description 8
- 239000011521 glass Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 238000011049 filling Methods 0.000 description 5
- 238000003848 UV Light-Curing Methods 0.000 description 4
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000009472 formulation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-M Methacrylate Chemical compound CC(=C)C([O-])=O CERQOIWHTDAKMF-UHFFFAOYSA-M 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- AZIQALWHRUQPHV-UHFFFAOYSA-N prop-2-eneperoxoic acid Chemical compound OOC(=O)C=C AZIQALWHRUQPHV-UHFFFAOYSA-N 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000003851 corona treatment Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Images
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
-
- 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
-
- 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
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/221—Oxides; Hydroxides of metals of rare earth metal
- C08K2003/2213—Oxides; Hydroxides of metals of rare earth metal of cerium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/22—Compounds containing nitrogen bound to another nitrogen atom
- C08K5/23—Azo-compounds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2203/00—Applications of adhesives in processes or use of adhesives in the form of films or foils
- C09J2203/326—Applications of adhesives in processes or use of adhesives in the form of films or foils for bonding electronic components such as wafers, chips or semiconductors
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
- C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a Mini LED packaging adhesive film and a preparation method thereof, wherein the packaging adhesive film comprises a diffusion film, a semi-permeable OCA and a release film, the semi-permeable OCA is positioned between the diffusion film and the release film, the transmittance of the semi-permeable OCA at 380-500nm is 30-70%, and the preparation method comprises the following steps: adding an alkyl (meth) acrylate main monomer, a (meth) acrylate functional monomer, a first photoinitiator and a chain transfer agent into a reactor, stirring for 30min under the atmosphere of nitrogen, and performing prepolymerization reaction by using a 365nm ultraviolet lamp to obtain an acrylate prepolymer; uniformly stirring the acrylate prepolymer, the blue light absorbent, the cross-linking agent and the second initiator to obtain acrylate polymer glue; and coating the glue between the diffusion film and the release film, and irradiating and curing by using a 365nm ultraviolet lamp. The invention is beneficial to improving the whole-surface light mixing uniformity of the Mini LED structure.
Description
Technical Field
The invention belongs to the technical field of packaging films, and particularly relates to a Mini LED packaging adhesive film and a preparation method thereof.
Background
Mini LED (sub-millimeter light emitting diode) is currently a hot spot in market development, and has many advantages of being light, thin, power-saving, flexible, bendable, high in brightness, capable of manufacturing narrow-frame full-screen display devices, high-dynamic-contrast display devices, and the like, and becomes a key point of market attention.
However, the surface light source has a problem of uneven brightness over the entire surface due to the limitation of the light emitting angle of the chip and the number of chips. In addition, because the height of the Mini LED lamp bead is 50-100 mu m, the problem of insufficient filling property exists by adopting the traditional OCA optical cement.
The present invention has been made to solve the above-mentioned problems occurring in the prior art.
Disclosure of Invention
Aiming at the technical problems, the invention provides a Mini LED packaging adhesive film and a preparation method thereof, the invention weakens the brightness of the front view angle direction of the chips by adopting a semi-transparent OCA mode in the structure of the Mini LED backlight module, and increases the luminous intensity among the chips by a diffusion film in the Mini LED backlight module, thereby improving the whole surface light mixing uniformity of the Mini LED structure; in addition, the invention also ensures the filling property by controlling the curing degree of the OCA to be about 50%, and then improves the reliability by carrying out secondary UV curing.
The technical scheme of the invention is as follows:
the invention provides a Mini LED packaging adhesive film which comprises a diffusion film, a semi-permeable OCA and a release film, wherein the semi-permeable OCA is positioned between the diffusion film and the release film, and the transmissivity of the semi-permeable OCA at a 380nm-500nm position is 30-70%, so that the characteristics of allowing blue light to be semi-transmitted and red light to be fully transmitted can be realized, the luminous intensity of a chip in the normal visual angle direction can be weakened, and the phenomenon of multiple refraction, reflection and scattering of light is caused through the diffusion film, so that the light mixing uniformity of the whole surface of a Mini LED is improved.
Preferably, the semi-permeable OCA has a gel fraction of 40-60%.
Preferably, the semi-permeable OCA is made of a post-UV curable (meth) acrylate polymer.
Preferably, the post-UV curable (meth) acrylate polymer is composed of the following raw materials in parts by mass: 60-80 parts of (methyl) acrylic acid alkyl ester main monomer, 20-40 parts of (methyl) acrylic acid ester functional monomer, 0.1-1 part of first photoinitiator, 0.01-0.5 part of chain transfer agent, 1-4 parts of blue light absorbent, 0.01-0.1 part of cross-linking agent and 0.01-0.1 part of second photoinitiator.
Wherein post-UV curable (meth) acrylate polymer is used to refer to both post-UV curable acrylate polymer and post-UV curable methacrylate polymer;
the (methyl) acrylic acid alkyl ester main monomer is used for referring to acrylic acid alkyl ester main monomer and methacrylic acid alkyl ester main monomer;
the (meth) acrylate functional monomer is used to refer to both acrylate functional monomers and methacrylate functional monomers.
Preferably, the alkyl (meth) acrylate main monomer is one or more of isooctyl acrylate, isooctyl methacrylate, n-hexyl acrylate, n-hexyl methacrylate, n-butyl acrylate, n-butyl methacrylate, lauryl acrylate, lauryl methacrylate, dihexyl acrylate, and dihexyl methacrylate;
the (methyl) acrylate functional monomer is one or more of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxybutyl acrylate, hydroxybutyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, acrylamide, methacrylamide, acryloyl morpholine, methacryloyl morpholine, isobornyl acrylate and isobornyl methacrylate.
Preferably, the first photoinitiator is one or more of benzophenone, 4-methylbenzophenone, 4-phenylbenzophenone, acryloxybenzophenone and methacryloxybenzophenone;
the chain transfer agent is one or more of n-dodecyl mercaptan, tert-dodecyl mercaptan and isooctyl thioglycolate;
the blue light absorbent is one or more of azo compounds, nano cerium oxide and nano zinc oxide; the dosage of the blue light absorbent is 1-4%, so that the blue light transmittance is 30-70%, and the light emitting uniformity of the Mini LED panel is improved by combining a diffusion film; specifically, azo blue light absorbers 1229BL can be selected, such as permanent lights 1229BL in taiwan province in China;
the cross-linking agent is one or more of hexanediol diacrylate, tripropylene glycol diacrylate, 1,4-butanediol diacrylate, 1,4-butanediol methyl diacrylate, 1,6-hexanediol diacrylate, 1,6-hexanediol methyl diacrylate, tripropylene glycol dimethacrylate, tricyclodecane dimethanol diacrylate, tricyclodecane dimethanol dimethacrylate, 1,10-decanediol diacrylate, 1,10-decanediol dimethacrylate and polyethylene glycol-200 dimethacrylate;
the second photoinitiator is one or more of benzil dimethyl ether, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-one, 2-benzyl-2-dimethylamine-1- (4-morpholine benzyl phenyl) butanone, 2,4,6-trimethylbenzoylphenyl phosphine oxide, 2,4,6-trimethylbenzoyldiphenyl phosphine oxide and 2,4,6-trimethylbenzoylphenyl phosphonic acid ethyl ester.
Preferably, the total light transmittance of the diffusion film is more than 88%, and Haze is more than 60%.
Preferably, the semi-permeable OCA has a thickness of 100 to 200 μm, the diffusion film has a thickness of 75 to 200 μm, and the release film has a thickness of 50 to 100 μm.
The invention also provides a preparation method of the Mini LED packaging adhesive film, which comprises the following steps:
s1, adding a (methyl) acrylic acid alkyl ester main monomer, a (methyl) acrylic acid ester functional monomer, a first photoinitiator and a chain transfer agent into a reactor, stirring for 30min in a nitrogen atmosphere, and performing a prepolymerization reaction by using a 365nm ultraviolet lamp to obtain an acrylic acid ester prepolymer with the weight-average molecular weight of 40 ten thousand;
s2, uniformly stirring the acrylate prepolymer, the blue light absorber, the cross-linking agent and the second initiator to obtain acrylate polymer glue;
and S3, coating the glue obtained in the step S2 between the diffusion film and the release film, and irradiating and curing by using a 365nm ultraviolet lamp to obtain the Mini LED packaging glue film.
Preferably, the UV irradiation intensity of the 365nm ultraviolet lamp is 2mw/cm 2 UV irradiation energy of 1000mj/cm 2 。
The invention has the beneficial effects that:
(1) According to the invention, the light-emitting brightness in the front view angle direction of the chip is weakened by adopting a semi-transparent OCA mode in the Mini LED backlight module structure, and meanwhile, the light-emitting intensity among the chips is increased through the group diffusion film in the Mini LED backlight module, so that the whole-surface light mixing uniformity of the Mini LED structure is improved, and the light-emitting uniformity is more than 90%;
(2) The semi-permeable OCA has the gel fraction of 40-60%, can be cured for the second time, controls the curing degree of the OCA to be about 50%, and ensures the filling property and the stability of the secondary curing.
Drawings
The invention is further described with reference to the following figures and examples:
FIG. 1 is a schematic structural diagram of a Mini LED packaging adhesive film;
FIG. 2 is a schematic structural diagram of a Mini LED backlight module;
fig. 3 is a graph for testing the uniformity of light emission.
Labeled as: 1. a diffusion membrane; 2. semi-permeable OCA; 3. a release film; 4. a PCB substrate; 5. mini LED lamp pearl.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings in conjunction with the following detailed description. It should be understood that the description is intended to be exemplary only, and is not intended to limit the scope of the present invention. Moreover, in the following description, descriptions of well-known structures and techniques are omitted so as to not unnecessarily obscure the concepts of the present invention.
Example 1
S1, putting 70 parts by mass of isooctyl acrylate, 10 parts by mass of hydroxy acrylate, 20 parts by mass of isobornyl acrylate, 0.2 part by mass of acryloyloxy benzophenone and 0.05 part by mass of n-dodecyl mercaptan into a four-neck flask, stirring for 30min under the atmosphere of nitrogen, and performing prepolymerization reaction by using an ultraviolet lamp with the wavelength of 365nm to obtain an acrylate prepolymer with the weight-average molecular weight of 40 ten thousand;
s2, uniformly stirring 100 parts by mass of the obtained acrylate prepolymer, 2 parts by mass of a blue light absorbent 1229BL (national Taiwan permanent light 1229 BL), 0.02 part by mass of a cross-linking agent 1,6-hexanediol diacrylate and 0.05 part by mass of an initiator 1-hydroxycyclohexyl phenyl ketone to obtain the acrylate polymer glue.
S3, coating the obtained glue between a diffusion film and a release film, and curing by using a 365nm ultraviolet lamp, wherein the UV irradiation intensity of the 365nm ultraviolet lamp is 2mw/cm 2 UV irradiation energy of 1000mj/cm 2 To obtain semi-permeable OCA with the thickness of 150 μm.
Examples 2 to 3
The preparation method of examples 2 and 3 was the same as that of example 1, according to the formulation shown in Table 1.
Comparative examples 1 to 3
The comparative examples 1, 2 and 3 were prepared according to the formulation shown in Table 1 in the same manner as in example 1.
Comparative example 4
S1, putting 70 parts by mass of isooctyl acrylate, 10 parts by mass of hydroxy acrylate, 20 parts by mass of isobornyl acrylate, 0.2 part by mass of acryloyloxy benzophenone and 0.05 part by mass of n-dodecyl mercaptan into a four-neck flask, stirring for 30min under the atmosphere of nitrogen, and performing prepolymerization reaction by using an ultraviolet lamp with the wavelength of 365nm to obtain an acrylate prepolymer with the weight-average molecular weight of 40 ten thousand;
s2, uniformly stirring 100 parts by mass of the obtained acrylate prepolymer, 1229BL 2 parts by mass of a blue light absorbent, 1,6-hexanediol diacrylate 0.02 parts by mass of a cross-linking agent and 0.05 part by mass of 1-hydroxycyclohexyl phenyl ketone serving as an initiator to obtain the acrylate polymer glue.
S3, coating the glue between PET and a release film, and irradiating and curing by using a 365nm ultraviolet lamp; the UV irradiation intensity of the 365nm ultraviolet lamp is 2mw/cm 2 UV irradiation energy of 1000mj/cm 2 To obtain semi-permeable OCA with the thickness of 150 μm.
The products obtained in examples 1 to 3 and comparative examples 1 to 4 were subjected to the following performance tests.
And (3) testing adhesive force: a150 μm thick sample was cut into a width of 25mm, a release film was removed and attached to glass, PET having a thickness of 25 μm and a length of 300mm and subjected to corona treatment was attached to the other side, the end of each strip was clamped to a tensile jig of a tensile machine and peeled at a speed of 300mm/min, and 5 sets of data were tested to calculate an average value.
Gel fraction test: weighing a certain weight of semi-permeable OCA M1, dissolving in ethyl acetate, standing for 24h, filtering, and weighing M2, wherein the gel fraction is M2/M1 × 100%.
And (3) filling property test: tearing off a release film of a Mini LED packaging adhesive film, dispersing glass beads with different diameters of 50-150 mu m on the semi-permeable OCA, attaching the semi-permeable OCA to glass with the thickness of 1mm, vacuum attaching the semi-permeable OCA and the glass beads, placing the semi-permeable OCA and the glass beads in a high-pressure defoaming machine for high-pressure defoaming, and observing whether bubbles exist in the positions of the glass beads of the defoamed sample. If no bubble is present, the post-UV curing is carried out (1, vacuum bonding conditions: 1000pa,45 ℃,30s, 2, high-pressure defoaming barA piece: 5kg at 50 ℃; 3. UV curing conditions: 2-200mw/cm 2 ，＞3000mj/cm 2 )。
And (3) reliability testing: and (3) placing the attached sample subjected to UV curing in a double 85 high-temperature high-humidity box for 500 hours, and observing whether newly added bubbles are generated at the positions of the glass beads.
And (3) testing the blue light transmittance: the transmittance of the product was tested using a UV spectrophotometer in accordance with ASTM D1003-13.
The Mini LED packaging adhesive film can be applied to a corresponding backlight module, as shown in fig. 2, the backlight module comprises a PCB substrate, a plurality of Mini LED lamp beads are arranged on the PCB substrate, the backlight module further comprises a Mini LED packaging adhesive film, the Mini LED packaging adhesive film comprises a diffusion film and a semi-transparent OCA, and the Mini LED lamp beads are packaged in the semi-transparent OCA.
The backlight module shown in fig. 2 is used for testing the luminous uniformity, and the specific method is as follows:
1. the display screen is set to be a white field;
2. measuring points 9 in the graph 3, namely P0-P8, and recording the brightness as L0-L8 by using a color analyzer;
3. calculating the brightness uniformity P of each point i ；
i is a value at any one point of (1 to 8);
4. get P i The minimum value among them represents the brightness uniformity Lp of the Mini LED display screen.
The formulation and performance test data for examples 1-3 and comparative examples 1-4 are shown in Table 1, where E1-E3 represent examples 1-3 and D1-D4 represent comparative examples 1-4.
TABLE 1
As can be seen from the above table, the emission uniformity and reliability were poor in comparative example 1 due to high blue light transmittance and low gel fraction. It can be seen in comparative example 3 that the filling property was poor because the gel fraction was high. It can be seen in comparative example 4 that the uniformity of light emission is poor because the diffusion film is not used. In addition, in comparative example 2, the overall luminance of the MiniLED backlight unit is insufficient due to the low blue transmittance.
It is to be understood that the above-described embodiments of the present invention are merely illustrative of or explaining the principles of the invention and are not to be construed as limiting the invention. Therefore, any modification, equivalent replacement, improvement and the like made without departing from the spirit and scope of the present invention should be included in the protection scope of the present invention. Further, it is intended that the appended claims cover all such variations and modifications as fall within the scope and boundaries of the appended claims or the equivalents of such scope and boundaries.
Claims (10)
1. The Mini LED packaging adhesive film is characterized by comprising a diffusion film, a semi-permeable OCA and a release film, wherein the semi-permeable OCA is positioned between the diffusion film and the release film, and the transmittance of the semi-permeable OCA at a 380nm-500nm position is 30-70%.
2. The MiniLED encapsulant film of claim 1, wherein the semi-permeable OCA has a gel fraction of 40-60%.
3. The MiniLED encapsulant film of claim 1, wherein the semi-permeable OCA is made of a post-UV curable (meth) acrylate polymer.
4. The MiniLED packaging film of claim 3, wherein the post-UV curable (meth) acrylate polymer comprises the following materials in parts by mass: 60-80 parts of (methyl) acrylic acid alkyl ester main monomer, 20-40 parts of (methyl) acrylic acid ester functional monomer, 0.1-1 part of first photoinitiator, 0.01-0.5 part of chain transfer agent, 1-4 parts of blue light absorbent, 0.01-0.1 part of cross-linking agent and 0.01-0.1 part of second photoinitiator.
5. The Mini LED packaging adhesive film of claim 4, wherein the alkyl (meth) acrylate based main monomer is one or more of isooctyl acrylate, isooctyl methacrylate, n-hexyl acrylate, n-hexyl methacrylate, n-butyl acrylate, n-butyl methacrylate, lauryl acrylate, lauryl methacrylate, dihexyl acrylate and dihexyl methacrylate;
the (methyl) acrylate functional monomer is one or more of hydroxyethyl acrylate, hydroxyethyl methacrylate, hydroxybutyl acrylate, hydroxybutyl methacrylate, hydroxypropyl acrylate, hydroxypropyl methacrylate, acrylamide, methacrylamide, acryloyl morpholine, methacryloyl morpholine, isobornyl acrylate and isobornyl methacrylate.
6. The Mini LED package adhesive film of claim 4, wherein the first photoinitiator is one or more of benzophenone, 4-methylbenzophenone, 4-phenylbenzophenone, acryloxybenzophenone and methacryloxybenzophenone;
the chain transfer agent is one or more of n-dodecyl mercaptan, tert-dodecyl mercaptan and isooctyl thioglycolate;
the blue light absorbent is one or more of azo compounds, nano cerium oxide and nano zinc oxide;
the cross-linking agent is one or more of hexanediol diacrylate, tripropylene glycol diacrylate, 1,4-butanediol diacrylate, 1,4-butanediol methyl diacrylate, 1,6-hexanediol diacrylate, 1,6-hexanediol methyl diacrylate, tripropylene glycol dimethacrylate, tricyclodecane dimethanol diacrylate, tricyclodecane dimethanol dimethacrylate, 1,10-decanediol diacrylate, 1,10-decanediol dimethacrylate and polyethylene glycol-200 dimethacrylate;
the second photoinitiator is one or more of benzil dimethyl ether, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-methyl-1-phenyl-1-acetone, 2-methyl-1- (4-methylthiophenyl) -2-morpholine-1-one, 2-benzyl-2-dimethylamine-1- (4-morpholine benzyl phenyl) butanone, 2,4,6-trimethylbenzoylphenyl phosphine oxide, 2,4,6-trimethylbenzoyldiphenyl phosphine oxide and 2,4,6-trimethylbenzoylphenyl phosphonic acid ethyl ester.
7. The Mini LED packaging adhesive film of claim 1, wherein the total light transmittance of the diffusion film is more than 88%, and the Haze is more than 60%.
8. The Mini LED packaging adhesive film of claim 1, wherein the semi-permeable OCA has a thickness of 100-200 μm, the diffusion film has a thickness of 75-200 μm, and the release film has a thickness of 50-100 μm.
9. A preparation method of a Mini LED packaging adhesive film is characterized by comprising the following steps:
s1, adding a (methyl) acrylic acid alkyl ester main monomer, a (methyl) acrylic acid ester functional monomer, a first photoinitiator and a chain transfer agent into a reactor, stirring for 30min in a nitrogen atmosphere, and performing a prepolymerization reaction by using a 365nm ultraviolet lamp to obtain an acrylic acid ester prepolymer with the weight-average molecular weight of 40 ten thousand;
s2, uniformly stirring the acrylate prepolymer, the blue light absorber, the cross-linking agent and the second initiator to obtain acrylate polymer glue;
and S3, coating the glue obtained in the step S2 between the diffusion film and the release film, and irradiating and curing by using a 365nm ultraviolet lamp to obtain the Mini LED packaging glue film.
10. The preparation method of the Mini LED packaging adhesive film of claim 9, wherein a 365nm ultraviolet lampHas a UV irradiation intensity of 2mw/cm 2 UV irradiation energy of 1000mj/cm 2 。
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