CN114729145A - Release film and preparation method thereof - Google Patents
Release film and preparation method thereof Download PDFInfo
- Publication number
- CN114729145A CN114729145A CN202180002509.8A CN202180002509A CN114729145A CN 114729145 A CN114729145 A CN 114729145A CN 202180002509 A CN202180002509 A CN 202180002509A CN 114729145 A CN114729145 A CN 114729145A
- Authority
- CN
- China
- Prior art keywords
- inorganic particles
- fluorine
- release film
- group
- organic
- 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.)
- Granted
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- 238000002360 preparation method Methods 0.000 title abstract description 32
- -1 silane compound Chemical class 0.000 claims abstract description 74
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 73
- 239000011737 fluorine Substances 0.000 claims abstract description 71
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 64
- 239000011242 organic-inorganic particle Substances 0.000 claims abstract description 62
- 229910000077 silane Inorganic materials 0.000 claims abstract description 40
- 239000000758 substrate Substances 0.000 claims abstract description 30
- 239000000126 substance Substances 0.000 claims description 54
- 239000010954 inorganic particle Substances 0.000 claims description 41
- 229920001296 polysiloxane Polymers 0.000 claims description 36
- 239000000203 mixture Substances 0.000 claims description 23
- 150000001875 compounds Chemical class 0.000 claims description 19
- 238000000576 coating method Methods 0.000 claims description 16
- 125000004429 atom Chemical group 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 15
- 125000000217 alkyl group Chemical group 0.000 claims description 14
- 229920001577 copolymer Polymers 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 12
- 125000001153 fluoro group Chemical group F* 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 125000003860 C1-C20 alkoxy group Chemical group 0.000 claims description 7
- 125000003342 alkenyl group Chemical group 0.000 claims description 7
- 125000006374 C2-C10 alkenyl group Chemical group 0.000 claims description 6
- 125000001033 ether group Chemical group 0.000 claims description 6
- 239000003377 acid catalyst Substances 0.000 claims description 5
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 5
- 229910052710 silicon Inorganic materials 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 4
- 238000002329 infrared spectrum Methods 0.000 claims description 4
- 125000003837 (C1-C20) alkyl group Chemical group 0.000 claims description 3
- 239000004215 Carbon black (E152) Substances 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 3
- 150000001242 acetic acid derivatives Chemical class 0.000 claims description 3
- 150000001642 boronic acid derivatives Chemical class 0.000 claims description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 150000004820 halides Chemical class 0.000 claims description 3
- 150000004677 hydrates Chemical class 0.000 claims description 3
- 229930195733 hydrocarbon Natural products 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 3
- 239000011707 mineral Substances 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 235000021317 phosphate Nutrition 0.000 claims description 3
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 claims description 3
- 150000003013 phosphoric acid derivatives Chemical class 0.000 claims description 3
- 150000004760 silicates Chemical class 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 150000003467 sulfuric acid derivatives Chemical class 0.000 claims description 3
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 1
- 239000010408 film Substances 0.000 description 83
- 239000010410 layer Substances 0.000 description 51
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 46
- 239000000377 silicon dioxide Substances 0.000 description 23
- 239000002245 particle Substances 0.000 description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 14
- 229920000728 polyester Polymers 0.000 description 13
- 229920005989 resin Polymers 0.000 description 12
- 239000011347 resin Substances 0.000 description 12
- 239000002904 solvent Substances 0.000 description 11
- 125000004432 carbon atom Chemical group C* 0.000 description 8
- 150000002430 hydrocarbons Chemical group 0.000 description 8
- 239000002390 adhesive tape Substances 0.000 description 7
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 6
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 5
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 5
- 229920001225 polyester resin Polymers 0.000 description 5
- 229920000139 polyethylene terephthalate Polymers 0.000 description 5
- 239000005020 polyethylene terephthalate Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 125000003545 alkoxy group Chemical group 0.000 description 4
- 125000003118 aryl group Chemical group 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- JLGNHOJUQFHYEZ-UHFFFAOYSA-N trimethoxy(3,3,3-trifluoropropyl)silane Chemical compound CO[Si](OC)(OC)CCC(F)(F)F JLGNHOJUQFHYEZ-UHFFFAOYSA-N 0.000 description 4
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 4
- 229920002554 vinyl polymer Polymers 0.000 description 4
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 3
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- NTIZESTWPVYFNL-UHFFFAOYSA-N Methyl isobutyl ketone Chemical compound CC(C)CC(C)=O NTIZESTWPVYFNL-UHFFFAOYSA-N 0.000 description 3
- UIHCLUNTQKBZGK-UHFFFAOYSA-N Methyl isobutyl ketone Natural products CCC(C)C(C)=O UIHCLUNTQKBZGK-UHFFFAOYSA-N 0.000 description 3
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000012046 mixed solvent Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229910052697 platinum Inorganic materials 0.000 description 3
- 229920006267 polyester film Polymers 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229920002050 silicone resin Polymers 0.000 description 3
- 239000007858 starting material Substances 0.000 description 3
- GETTZEONDQJALK-UHFFFAOYSA-N (trifluoromethyl)benzene Chemical compound FC(F)(F)C1=CC=CC=C1 GETTZEONDQJALK-UHFFFAOYSA-N 0.000 description 2
- OJVAMHKKJGICOG-UHFFFAOYSA-N 2,5-hexanedione Chemical compound CC(=O)CCC(C)=O OJVAMHKKJGICOG-UHFFFAOYSA-N 0.000 description 2
- QQZOPKMRPOGIEB-UHFFFAOYSA-N 2-Oxohexane Chemical compound CCCCC(C)=O QQZOPKMRPOGIEB-UHFFFAOYSA-N 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
- FJKROLUGYXJWQN-UHFFFAOYSA-N 4-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=C(O)C=C1 FJKROLUGYXJWQN-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 2
- DIOQZVSQGTUSAI-UHFFFAOYSA-N decane Chemical compound CCCCCCCCCC DIOQZVSQGTUSAI-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 125000003709 fluoroalkyl group Chemical group 0.000 description 2
- 230000005484 gravity Effects 0.000 description 2
- CATSNJVOTSVZJV-UHFFFAOYSA-N heptan-2-one Chemical compound CCCCCC(C)=O CATSNJVOTSVZJV-UHFFFAOYSA-N 0.000 description 2
- 125000004491 isohexyl group Chemical group C(CCC(C)C)* 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 2
- UAEPNZWRGJTJPN-UHFFFAOYSA-N methylcyclohexane Chemical compound CC1CCCCC1 UAEPNZWRGJTJPN-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 2
- 125000001971 neopentyl group Chemical group [H]C([*])([H])C(C([H])([H])[H])(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 2
- XNLICIUVMPYHGG-UHFFFAOYSA-N pentan-2-one Chemical compound CCCC(C)=O XNLICIUVMPYHGG-UHFFFAOYSA-N 0.000 description 2
- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 239000011112 polyethylene naphthalate Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-N sebacic acid Chemical compound OC(=O)CCCCCCCCC(O)=O CXMXRPHRNRROMY-UHFFFAOYSA-N 0.000 description 2
- 125000001424 substituent group Chemical group 0.000 description 2
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 2
- CHRJZRDFSQHIFI-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;styrene Chemical compound C=CC1=CC=CC=C1.C=CC1=CC=CC=C1C=C CHRJZRDFSQHIFI-UHFFFAOYSA-N 0.000 description 1
- XXZOEDQFGXTEAD-UHFFFAOYSA-N 1,2-bis(trifluoromethyl)benzene Chemical group FC(F)(F)C1=CC=CC=C1C(F)(F)F XXZOEDQFGXTEAD-UHFFFAOYSA-N 0.000 description 1
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 description 1
- DFUYAWQUODQGFF-UHFFFAOYSA-N 1-ethoxy-1,1,2,2,3,3,4,4,4-nonafluorobutane Chemical compound CCOC(F)(F)C(F)(F)C(F)(F)C(F)(F)F DFUYAWQUODQGFF-UHFFFAOYSA-N 0.000 description 1
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-UHFFFAOYSA-N 0.000 description 1
- UOBYKYZJUGYBDK-UHFFFAOYSA-N 2-naphthoic acid Chemical compound C1=CC=CC2=CC(C(=O)O)=CC=C21 UOBYKYZJUGYBDK-UHFFFAOYSA-N 0.000 description 1
- 125000000094 2-phenylethyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])C([H])([H])* 0.000 description 1
- FNUBKINEQIEODM-UHFFFAOYSA-N 3,3,4,4,5,5,5-heptafluoropentanal Chemical compound FC(F)(F)C(F)(F)C(F)(F)CC=O FNUBKINEQIEODM-UHFFFAOYSA-N 0.000 description 1
- 229940090248 4-hydroxybenzoic acid Drugs 0.000 description 1
- 239000005995 Aluminium silicate Substances 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- XMSXQFUHVRWGNA-UHFFFAOYSA-N Decamethylcyclopentasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 XMSXQFUHVRWGNA-UHFFFAOYSA-N 0.000 description 1
- 239000004134 Dicalcium diphosphate Substances 0.000 description 1
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- NHTMVDHEPJAVLT-UHFFFAOYSA-N Isooctane Chemical compound CC(C)CC(C)(C)C NHTMVDHEPJAVLT-UHFFFAOYSA-N 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- RGMZNZABJYWAEC-UHFFFAOYSA-N Methyltris(trimethylsiloxy)silane Chemical compound C[Si](C)(C)O[Si](C)(O[Si](C)(C)C)O[Si](C)(C)C RGMZNZABJYWAEC-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 239000004820 Pressure-sensitive adhesive Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- YIMQCDZDWXUDCA-UHFFFAOYSA-N [4-(hydroxymethyl)cyclohexyl]methanol Chemical compound OCC1CCC(CO)CC1 YIMQCDZDWXUDCA-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000001361 adipic acid Substances 0.000 description 1
- 235000011037 adipic acid Nutrition 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 125000000304 alkynyl group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 125000001797 benzyl group Chemical group [H]C1=C([H])C([H])=C(C([H])=C1[H])C([H])([H])* 0.000 description 1
- 125000004369 butenyl group Chemical group C(=CCC)* 0.000 description 1
- 229940043232 butyl acetate Drugs 0.000 description 1
- QHIWVLPBUQWDMQ-UHFFFAOYSA-N butyl prop-2-enoate;methyl 2-methylprop-2-enoate;prop-2-enoic acid Chemical compound OC(=O)C=C.COC(=O)C(C)=C.CCCCOC(=O)C=C QHIWVLPBUQWDMQ-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 235000010216 calcium carbonate Nutrition 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 235000011132 calcium sulphate Nutrition 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 229910052800 carbon group element Inorganic materials 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229920006026 co-polymeric resin Polymers 0.000 description 1
- 238000011284 combination treatment Methods 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 125000006165 cyclic alkyl group Chemical group 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 125000000392 cycloalkenyl group Chemical group 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 125000001511 cyclopentyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C1([H])[H] 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- JVSWJIKNEAIKJW-UHFFFAOYSA-N dimethyl-hexane Natural products CCCCCC(C)C JVSWJIKNEAIKJW-UHFFFAOYSA-N 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 239000003759 ester based solvent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- SVBSJWKYFYUHTF-UHFFFAOYSA-N ethyl 2-butoxyacetate Chemical compound CCCCOCC(=O)OCC SVBSJWKYFYUHTF-UHFFFAOYSA-N 0.000 description 1
- CKSRFHWWBKRUKA-UHFFFAOYSA-N ethyl 2-ethoxyacetate Chemical compound CCOCC(=O)OCC CKSRFHWWBKRUKA-UHFFFAOYSA-N 0.000 description 1
- JLEKJZUYWFJPMB-UHFFFAOYSA-N ethyl 2-methoxyacetate Chemical group CCOC(=O)COC JLEKJZUYWFJPMB-UHFFFAOYSA-N 0.000 description 1
- 229940093499 ethyl acetate Drugs 0.000 description 1
- 238000007756 gravure coating Methods 0.000 description 1
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 238000012844 infrared spectroscopy analysis Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- GJRQTCIYDGXPES-UHFFFAOYSA-N iso-butyl acetate Natural products CC(C)COC(C)=O GJRQTCIYDGXPES-UHFFFAOYSA-N 0.000 description 1
- FGKJLKRYENPLQH-UHFFFAOYSA-M isocaproate Chemical compound CC(C)CCC([O-])=O FGKJLKRYENPLQH-UHFFFAOYSA-M 0.000 description 1
- JMMWKPVZQRWMSS-UHFFFAOYSA-N isopropanol acetate Natural products CC(C)OC(C)=O JMMWKPVZQRWMSS-UHFFFAOYSA-N 0.000 description 1
- 125000000555 isopropenyl group Chemical group [H]\C([H])=C(\*)C([H])([H])[H] 0.000 description 1
- 229940011051 isopropyl acetate Drugs 0.000 description 1
- GWYFCOCPABKNJV-UHFFFAOYSA-N isovaleric acid Chemical compound CC(C)CC(O)=O GWYFCOCPABKNJV-UHFFFAOYSA-N 0.000 description 1
- OQAGVSWESNCJJT-UHFFFAOYSA-N isovaleric acid methyl ester Natural products COC(=O)CC(C)C OQAGVSWESNCJJT-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 235000014380 magnesium carbonate Nutrition 0.000 description 1
- GVALZJMUIHGIMD-UHFFFAOYSA-H magnesium phosphate Chemical compound [Mg+2].[Mg+2].[Mg+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O GVALZJMUIHGIMD-UHFFFAOYSA-H 0.000 description 1
- 239000004137 magnesium phosphate Substances 0.000 description 1
- 229910000157 magnesium phosphate Inorganic materials 0.000 description 1
- 229960002261 magnesium phosphate Drugs 0.000 description 1
- 235000010994 magnesium phosphates Nutrition 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- GYNNXHKOJHMOHS-UHFFFAOYSA-N methyl-cycloheptane Natural products CC1CCCCCC1 GYNNXHKOJHMOHS-UHFFFAOYSA-N 0.000 description 1
- YKYONYBAUNKHLG-UHFFFAOYSA-N n-Propyl acetate Natural products CCCOC(C)=O YKYONYBAUNKHLG-UHFFFAOYSA-N 0.000 description 1
- RXOHFPCZGPKIRD-UHFFFAOYSA-N naphthalene-2,6-dicarboxylic acid Chemical compound C1=C(C(O)=O)C=CC2=CC(C(=O)O)=CC=C21 RXOHFPCZGPKIRD-UHFFFAOYSA-N 0.000 description 1
- SLCVBVWXLSEKPL-UHFFFAOYSA-N neopentyl glycol Chemical compound OCC(C)(C)CO SLCVBVWXLSEKPL-UHFFFAOYSA-N 0.000 description 1
- HMMGMWAXVFQUOA-UHFFFAOYSA-N octamethylcyclotetrasiloxane Chemical compound C[Si]1(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O1 HMMGMWAXVFQUOA-UHFFFAOYSA-N 0.000 description 1
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
- 239000011146 organic particle Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N palladium Substances [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 229940090181 propyl acetate Drugs 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 239000010948 rhodium Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- VNRWTCZXQWOWIG-UHFFFAOYSA-N tetrakis(trimethylsilyl) silicate Chemical compound C[Si](C)(C)O[Si](O[Si](C)(C)C)(O[Si](C)(C)C)O[Si](C)(C)C VNRWTCZXQWOWIG-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/04—Coating
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
- C08K3/013—Fillers, pigments or reinforcing additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
-
- 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
- C08K5/54—Silicon-containing compounds
- C08K5/544—Silicon-containing compounds containing nitrogen
- C08K5/5445—Silicon-containing compounds containing nitrogen containing at least one Si-N bond
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
- C08L83/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen and oxygen
-
- 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
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
- C09D183/08—Polysiloxanes containing silicon bound to organic groups containing atoms other than carbon, hydrogen, and oxygen
-
- 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
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
-
- 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
- C09J7/40—Adhesives in the form of films or foils characterised by release liners
- C09J7/401—Adhesives in the form of films or foils characterised by release liners characterised by the release coating composition
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Chemistry (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to a release film and a preparation method thereof. In the release film, a substrate and a release layer having a surface energy of 24dyne/cm or less are sequentially positioned, the release layer includes organic-inorganic particles in which a portion (moiey) including a fluorine-containing silane compound is introduced on the surface thereof, and the organic-inorganic particles may satisfy a content ratio of F/Si element (M) shown by the following formula 1F/MSi) The range is as follows: [ formula 1 ] M is not less than 0.1F/MSiLess than or equal to 1.0 in the formula, MFIs the content of the F element (atom percent)SiIs the content (atom%) of the Si element.
Description
Technical Field
The invention relates to a release film and a preparation method thereof.
Background
In general, a silicone-based adhesive (hereinafter, this means including a pressure-sensitive adhesive) has characteristics of heat resistance, weather resistance, flexibility, chemical resistance, and the like, and recently, IT is widely used not only for general industrial tapes but also in IT fields of mobile phones, semiconductors, displays, and the like.
However, since the silicone-based release film using the silicone-based adhesive is completely laminated on the adhesive and is not peeled off, a film coated with a release agent containing a fluorine-based resin is generally used. After curing, the release agent containing a fluorine-based resin is likely to cause interlayer curing due to the residual curing agent, and the peeling force and the residual adhesion rate are likely to decrease.
In order to solve these problems, a release film excellent in light peelability, residual adhesiveness and coating appearance and a method for preparing the same are still required.
Disclosure of Invention
Technical problem
An aspect of the present invention provides a release film excellent in light peelability, residual adhesion rate, and coating appearance.
The invention also provides a preparation method of the release film.
Technical scheme
In one aspect of the present invention, there is provided a release film, wherein,
the base material and the release layer are positioned in turn,
the surface energy of the release layer is below 24dyne/cm,
the release layer includes organic-inorganic particles,
in the organic-inorganic particles, a moiety (moiety) including a fluorine-containing silane compound is introduced to a surface thereof,
the organic-inorganic particles may satisfy a content ratio (M) of F/Si element represented by the following formula 1F/MSi) The range is as follows:
[ formula 1 ]
0.1≤MF/MSi≤1.0
In the formula (I), the compound is shown in the specification,
MFmay be the content (% by atom) of the F element, MSiThe content (atomic%) of the Si element may be set.
The fluorine-containing silane compound moiety may include a fluorine-containing silane compound represented by the following chemical formula 1.
[ chemical formula 1 ]
*-OSi(Ra)(Rb)(Rc)
In the formula (I), the compound is shown in the specification,
Raand RbMay be a substituted or unsubstituted C1-C20 alkoxy group;
Rccan be represented by the following chemical formula 2,
may be binding sites to the surface of the organic-inorganic particles.
[ chemical formula 2 ]
In the formula (I), the compound has the following structure,
Rdmay be a hydrogen atom or a substituted or unsubstituted C1-C20 alkyl group;
Raand RbMay be a substituted or unsubstituted C1-C20 alkoxy group;
Rfmay be C4-C20 alkyl substituted by fluorine;
n1may be an integer from 1 to 10;
may be a binding site to a Si atom.
The weight ratio of the organic-inorganic particles to the fluorine-containing silane compound may be 1:1 to 20: 1.
in the release layer, 1064cm in infrared spectrum was compared with the organic-inorganic particles of which surface did not include a fluorine-containing silane compound moiety-1To 1066cm-1Peaks in the wavenumber range may be shifted to the right.
The organic-inorganic particles may include natural minerals; an oxide, hydroxide, sulfide, nitride or halide of an element of groups 1 to 4, 11 to 12, 14 and 16 to 18; carbonates, sulfates, acetates, phosphates, phosphites, carboxylates, silicates, titanates, borates, or hydrates thereof; and inorganic particles selected from complex compounds thereof.
The release layer may further include a polymer or copolymer containing a fluorine-containing polysiloxane.
The fluorine-containing polysiloxane may include an organopolysiloxane represented by the following chemical formula 3.
< chemical formula 3>
< chemical formula 4>
< chemical formula 5>
In the formula (I), the compound is shown in the specification,
R1may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, or a substituted or unsubstituted C2-C10 alkenyl group;
R2may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, a substituted or unsubstituted C2-C10 alkenyl group, or hydrogen;
R3may be a fluorine-containing alkyl group represented by the chemical formula 4, a fluorine-containing ether group represented by the chemical formula 5, or a combination thereof;
n may be an integer of 1 to 8, m may be an integer of 1 to 5;
p may be an integer from 1 to 5, q may be 0 or 1, r may be 0, 1 or 2, and v may be an integer from 1 to 5;
a can be an oxygen atom or a single bond;
x, y and z may each be an integer of 1 or more;
may be a binding site to an adjacent atom;
wherein R is1And R2At least one of them may be a substituted or unsubstituted alkenyl group of C2 to C10.
The release layer may further include at least one of hydrogen polysiloxane (hydrogen polysiloxane) and an acid catalyst.
The release film may have a peel force of 23gf/25mm or less.
The residual adhesion rate of the release film may be 90% or more.
In another aspect, the present invention provides a method for preparing a release film, including:
preparing a base material;
adding and stirring inorganic particles, a fluorine-containing silane compound and an aminosilane-based co-reactant, and then heating to prepare organic-inorganic particles; and
the above release film is prepared by coating a composition for forming a release layer, which includes a polymer or copolymer including a fluorine-containing polysiloxane, and organic-inorganic particles, on at least one side of the substrate and drying to form a release layer,
the weight ratio of the inorganic particles to the fluorine-containing silane compound is 4: 1 to 20: 1.
the heating may be performed at 60 ℃ or higher under an air atmosphere.
The weight ratio of the inorganic particles to the fluorine-containing silane compound may be 1:1 to 20: 1.
advantageous effects
In a release film according to an aspect, a surface energy of the release layer is 24dyne/cm or less, the release layer includes organic-inorganic particles in which a portion (moiey) including a fluorine-containing silane compound is introduced on a surface thereof, and the organic-inorganic particles may satisfy a content ratio of F/Si element (M) shown by the formula 1F/MSi) And (3) a range. The release film can provide a release film excellent in light peelability, residual adhesion and coating appearance.
Drawings
Fig. 1 is a cross-sectional view of a release film according to an embodiment of the present invention.
Fig. 2 shows the results of infrared ray spectra of three silica inorganic particles, wherein the first silica inorganic particles are starting materials of the release film prepared according to example 1, the second silica inorganic particles are intermediate reactants for introducing aminosilane on the surface, and the third silica inorganic particles are final products for introducing aminosilane and fluorine-containing silane compound on the surface.
Detailed Description
The release film and the method for manufacturing the same will be described in detail below with reference to the examples of the present invention and the accompanying drawings. It will be understood by those of ordinary skill in the art that these examples are given by way of illustration only to more specifically describe the present invention and the scope of the present invention is not limited by these examples.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, including definitions, will control.
All methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, with suitable methods and materials being described herein.
In this specification, unless stated to the contrary, the term "comprising" means that other components may be further included without excluding other components.
In the present specification, the term "combination thereof" means mixing or combination with at least one of the components.
In this specification, the term "and/or" is intended to include any and all combinations of one or more of the items described in connection with the description thereof. In this specification, the term "or" means "and/or". In this specification, the expression "at least one" or "more than one" preceding an element means that a list of all elements may be supplemented but does not mean that each element may supplement the description.
In the present specification, when it is referred to an element being "on" or "over" another element, one element may be directly on the other element or intervening elements may be present. On the other hand, when an element is referred to as being "directly on" or "directly over" another element, there may be no intervening elements present.
In the present specification, "resin system", "polymer system" or/and "copolymer system" is a broad concept and includes "resin", "polymer", "copolymer" or/and "derivative of resin, polymer or copolymer".
In the present specification, the term "polymer or copolymer crosslinked with a resin thereof" means "polymer or copolymer crosslinked with the above-mentioned resin".
In the present specification, "aminosilane-based co-reactant" is a broad concept and includes "aminosilane-based co-reactant" or "co-reactant including aminosilane".
According to the release film of an embodiment of the present invention, a substrate and a release layer are sequentially positioned, the release layer having a surface energy of 24dyne/cm or less, the release layer including organic-inorganic particles in which a portion (moiey) including a fluorine-containing silane compound is introduced on the surface thereof, the organic-inorganic particles may satisfy a content ratio of F/Si element (M) shown by the following formula 1F/MSi) The range is as follows:
[ formula 1 ]
0.1≤MF/MSi≤1.0
In the formula (I), the compound is shown in the specification,
MFis the content of the F element (atom percent)SiIs the content (atom%) of the Si element.
The release film according to an embodiment of the present invention has blocking resistance, and can provide a release film excellent in light peeling property, residual adhesion rate, and coating appearance.
The substrate constituting the release film, the release layer, the release film and the method for preparing the same will be described in detail below.
< substrate >
As the substrate used in the present invention, a known substrate film or substrate sheet can be used as the substrate of the release film. For example, a polyester resin film can be used as the substrate. As the polyester-based resin, a known substrate film commonly used in the field of release films can be used. For example, as the polyester-based resin base material film, polyester-based base material films disclosed in korean registered patent No. 10-1268584, korean registered patent No. 2012-45213, and korean registered patent No. 2012-99546, etc. can be used. However, in one embodiment of the present invention, in order to describe only the features of the present invention, the description of the polyester-based substrate film is not limited, but should be understood to include technical features related to the known polyester-based substrate film.
The polyester-based substrate film may include polyethylene terephthalate, polybutylene terephthalate, polyethylene naphthalate, or the like.
As the polyester-based resin forming the substrate film, a polyester obtained by polycondensing an aromatic dicarboxylic acid or an aliphatic dicarboxylic acid with an aliphatic diol may be used, wherein isophthalic acid, phthalic acid, terephthalic acid, 2, 6-naphthalenedicarboxylic acid, adipic acid, sebacic acid, hydroxycarboxylic acid (for example, ρ -oxybenzoic acid or 4-hydroxybenzoic acid), and the like may be used as the aromatic dicarboxylic acid or the aliphatic dicarboxylic acid, and ethylene glycol, diethylene glycol, propylene glycol, butylene glycol, 1, 4-cyclohexanedimethanol, neopentyl glycol, and the like may be used as the aliphatic diol. As such a polyester resin, two or more of a dicarboxylic acid component and a diol component may be used in combination, or a copolymer including a third component may be used.
In addition, as the polyester-based substrate film, a uniaxially or biaxially oriented film having high transparency and excellent productivity and processability can be used. As the polyester-based substrate film, polyethylene terephthalate (PET), poly (vinyl 2, 6-naphthalate) (PEN), or the like can be used.
In addition, the polyester-based substrate film may include particles to provide excellent inter-Roll (Roll) running characteristics, and may be used without limitation as long as the added particles can exhibit excellent sliding characteristics.
Examples of such particles may include particles of silica, calcium carbonate, calcium sulfate, calcium phosphate, magnesium carbonate, magnesium phosphate, barium carbonate, kaolin, alumina, titanium oxide, and the like, and the shape of the particles used is not limited, but any of, for example, spherical, block-shaped, rod-shaped, and plate-shaped particles may be used.
In addition, although there is no limitation on the hardness, specific gravity and color of the particles, two or more kinds may be used in parallel according to need, and the average particle diameter of the particles used may be 0.1 to 5 μm, for example, particles in the range of 0.1 to 2 μm may be used. At this time, when the average particle diameter of the particles is less than 0.1 μm, an aggregation phenomenon between the particles may occur, resulting in poor dispersion, and when the average particle diameter of the particles is greater than 5 μm, coating defects may occur during post-processing due to deterioration of surface roughness characteristics of the thin film.
Further, when the polyester-based substrate film includes particles, the content of the particles may be 0.01 to 5 wt%, for example, 0.01 to 3 wt%, based on the total weight of the polyester-based substrate film. When the content of the particles is less than 0.01 wt%, the slip characteristics of the polyester film may be deteriorated, resulting in deterioration of walking characteristics between rolls, and when the content of the particles is more than 5 wt%, the surface smoothness of the film may be deteriorated.
The thickness of the polyester-based substrate film is not limited, but may be 30 μm to 125 μm.
When the polyester-based substrate is too thin to 30 μm or less, deformation may be caused by heat treatment during processing, and when the polyester-based substrate is too thick to 125 μm or more, problems may occur in curing due to insufficient heat transfer.
< Release layer >
The release layer of the release film according to an embodiment of the present invention may have a surface energy of 24dyne/cm or less. Due to such low surface energy, the release film can achieve light peelability with low peel force.
The release layer includes organic-inorganic particles, a portion (moiety) including a fluorine-containing silane compound is introduced onto surfaces of the organic-inorganic particles, and the organic-inorganic particles may satisfy a content ratio (M) of F/Si element shown by the following chemical formula 1F/MSi) The range is as follows:
[ formula 1 ]
0.1≤MF/MSi≤1.0
In the formula (I), the compound is shown in the specification,
MFmay be the content (% by atom) of the F element, MSiThe content (atomic%) of the Si element may be set.
The organic-inorganic particles can prevent blocking. The organic-inorganic particles include a fluorine-containing silane compound on the surface thereof and satisfy the content ratio (M) of F/Si element represented by the formula 1F/MSi) Range, thereby notOnly the light peelability can be improved, and the residual adhesion and the coating appearance can also be improved.
The fluorine-containing silane compound moiety may include a fluorine-containing silane compound represented by the following chemical formula 1.
[ chemical formula 1 ]
*-OSi(Ra)(Rb)(Rc)
In the formula (I), the compound is shown in the specification,
Raand RbMay be a substituted or unsubstituted C1-C20 alkoxy group;
Rccan be represented by the following chemical formula 2,
may be binding sites to the surface of the organic-inorganic particles.
[ chemical formula 2 ]
In the formula (I), the compound is shown in the specification,
Rdmay be a hydrogen atom or a substituted or unsubstituted C1-C20 alkyl group;
Raand RbMay be a substituted or unsubstituted C1-C20 alkoxy group;
Rfmay be C4-C20 alkyl substituted by fluorine;
n1may be an integer from 1 to 10;
may be a binding site to a Si atom.
For example, in the chemical formula 1 and the chemical formula 2, Ra、Rb、ReAnd RgMay be, independently of one another, a substituted or unsubstituted C1-C20 alkoxy group, a substituted or unsubstituted C1-C5 alkoxy group, or an unsubstituted C1-C5 alkoxy group.
For example, in the chemical formula 2, n1May be an integer of 1 to 10, or an integer of 1 to 5.
For example, in the chemical formula 2, RfMay be a C4-C20 alkyl group substituted by fluorine, a C4-C15 alkyl group substituted by fluorine or a C4-C10 alkyl group substituted by fluorine. When R in the chemical formula 2fWhen the alkyl group has the number of carbon substituted by fluorine, the peeling force can be reduced to achieve excellent light peelability.
The weight ratio of the organic-inorganic particles to the fluorine-containing silane compound may be 1:1 to 20: 1. when the weight ratio of the organic-inorganic particles to the fluorine-containing silane compound is within the range, the peeling force may be further reduced to achieve excellent light peelability.
In the release layer, 1064cm in infrared spectrum was compared with the organic-inorganic particles of which surface did not include a fluorine-containing silane compound moiety-1To 1066cm-1Peaks in the wavenumber range may be shifted to the right.
The organic-inorganic particles may include natural minerals; an oxide, hydroxide, sulfide, nitride or halide of a group 1 to group 4, group 11 to group 12, group 14 and group 16 to group 18 element; carbonates, sulfates, acetates, phosphates, phosphites, carboxylates, silicates, titanates, borates, or hydrates thereof; and inorganic particles selected from complex compounds thereof.
The organic-inorganic particles may include organic particles selected from fluorine-based resins, melamine-based resins, styrene-based resins, acrylic-based resins, silicone-based resins, styrene-divinylbenzene-based copolymer resins, and polymers or copolymers crosslinked with the resins thereof, as required.
The shape of the organic-inorganic particles used is not particularly limited, and it may be spherical, massive, rod-like, or flat, and the like. In addition, the hardness, specific gravity, color, and the like of the organic-inorganic particles are not limited, and these organic-inorganic particles may be used alone or two or more kinds may be used if necessary.
The release layer may further include a polymer or copolymer containing a fluorine-containing polysiloxane.
The fluorine-containing polysiloxane may include an organopolysiloxane represented by the following chemical formula 3.
< chemical formula 3>
< chemical formula 4>
< chemical formula 5>
In the formula (I), the compound has the following structure,
R1may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, or a substituted or unsubstituted C2-C10 alkenyl group;
R2may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, a substituted or unsubstituted C2-C10 alkenyl group, or hydrogen;
R3may be a fluorine-containing alkyl group represented by the chemical formula 4, a fluorine-containing ether group represented by the chemical formula 5, or a combination thereof;
n may be an integer of 1 to 8, m may be an integer of 1 to 5;
p may be an integer from 1 to 5, q may be 0 or 1, r may be 0, 1 or 2, and v may be an integer from 1 to 5;
a can be an oxygen atom or a single bond;
x, y and z may each be an integer of 1 or more;
may be a binding site to an adjacent atom;
wherein R is1And R2At least one of them may be a substituted or unsubstituted alkenyl group of C2 to C10.
The fluorine-containing polysiloxane may be a blend of the organopolysiloxane represented by chemical formula 3 and the organopolysiloxane represented by chemical formula 6 below, or may be a copolymer in which the organopolysiloxane represented by chemical formula 3 and the organopolysiloxane represented by chemical formula 6 below are linked, as required:
< chemical formula 6>
< chemical formula 7>
In the formula (I), the compound is shown in the specification,
R'1may be a substituted or unsubstituted C1-C10 monovalent hydrocarbon group, or a substituted or unsubstituted C2-C10 alkenyl group;
R'2may be a fluorine-containing ether group represented by the chemical formula 7;
n 'may be an integer of 1 to 8, and m' may be an integer of 3 to 17;
may be a binding site to an adjacent atom.
For example, the weight ratio of the organopolysiloxane represented by chemical formula 3 to the organopolysiloxane represented by chemical formula 6 may be 10: 1 to 1: 10.
the release layer may further include at least one of hydrogen polysiloxane (hydrogen polysiloxane) and an acid catalyst.
The hydrogen polysiloxane may include at least one of an addition reaction type silicone resin, a condensation reaction type silicone resin, and an ultraviolet curing type silicone resin. The hydrogen polysiloxane may be linear, branched or cyclic, or may be a mixture thereof. The hydrogenpolysiloxane is not limited in viscosity and molecular weight, but must be good in compatibility with the above-mentioned organopolysiloxane, and may not include a fluorine group. However, the hydrogen polysiloxane may also include the same fluorine-containing alkyl groups and/or fluorine-containing ether groups as the above-mentioned organopolysiloxane.
The hydrogenpolysiloxane may be contained in an amount of 1.0 to 10.0 wt% based on the total weight of the composition for forming the release layer.
As the acid catalyst, at least one metal selected from group 4 to group 14 elements or an amphoteric element may be used, and for example, at least one selected from Rh, Pt, Sn, Ti, Pd, Ir, W, and Co may be used. For example, the acid catalyst may include a platinum chelate catalyst.
The release layer may further include additives for imparting various functions such as a reaction regulator, an antistatic agent, etc., if necessary.
The thickness of the release layer may be 0.03 to 3.0 μm. When the thickness of the release layer is less than 0.01um, the coverage of the release layer is not good, and when the thickness of the release layer is greater than 3um, thermal deformation of the substrate film may be caused due to a large amount of heat required in the curing process.
< Release film >
Fig. 1 is a cross-sectional view of a release film 100 according to an embodiment of the present invention.
Referring to fig. 1, a release film 120 according to an embodiment of the present invention has a structure in which a substrate 100 and a release layer 110 are sequentially positioned.
The release film 120 according to an embodiment of the present invention can provide a release film excellent in light peelability, residual adhesion, and coating appearance.
The release film may have a peel force of 23gf/25mm or less.
The residual adhesion rate of the release film may be 90% or more.
When the residual tack ratio of the release film is less than 90%, the release agent is transferred to the adhesive layer due to insufficient curing of the release layer, thereby causing a problem that the adhesiveness of the adhesive is deteriorated.
< method for producing Release film >
The preparation method of the release film according to one embodiment of the invention comprises the following steps: preparing a base material; adding and stirring inorganic particles, a fluorine-containing silane compound and an aminosilane-based co-reactant, and then heating to prepare organic-inorganic particles; and coating a composition for forming a release layer, including a polymer or copolymer including a fluorine-containing polysiloxane, and organic-inorganic particles on at least one side of the substrate and drying to form a release layer to prepare the above release film, wherein the weight ratio of the inorganic particles to the fluorine-containing silane compound may be 4: 1 to 20: 1.
the release film prepared by the method for preparing a release film according to an embodiment of the present invention can provide a release film excellent in light peelability, residual adhesion rate, and coating appearance.
In this case, the solvent used in the composition for forming a release layer may be used without limitation as long as the solid content in the composition for forming a release layer can be dispersed and coated on the substrate. When the total solid content of the composition for forming a release layer is less than 0.5 wt%, a uniform release layer cannot be formed, so that problems such as poor peeling between a silicone-based adhesive layer and a release film may occur, and when the total solid content of the composition for forming a release layer is more than 10 wt%, high viscosity of the composition for forming a release layer may cause uneven leveling, so that thickness uniformity of the release layer may be deteriorated.
As the solvent used in the composition for forming the release layer, aromatic hydrocarbon-based solvents such as toluene, xylene, and the like; aliphatic hydrocarbon solvents such as hexane, heptane, n-octane, isooctane, decane, cyclohexane, methylcyclohexane, isoparaffin, and the like; hydrocarbon solvents such as industrial gasoline (rubber gasoline, etc.), petroleum benzene, solvent oil, etc.; ketone solvents such as acetone, methyl ethyl ketone, 2-pentanone, 3-pentanone, 2-hexanone, 2-heptanone, 4-heptanone, methyl isobutyl ketone, diisobutyl ketone, acetonyl acetone, cyclohexanone, etc.; ester-based solvents such as ethyl acetate, propyl acetate, isopropyl acetate, butyl acetate, isobutyl acetate, and the like; ether solvents such as diethyl ether, dipropyl ether, diisopropyl ether, dibutyl ether, 1, 2-dimethoxyethane, 1, 4-dioxane, etc.; solvents having ester and ether moieties such as ethyl 2-methoxyacetate, ethyl 2-ethoxyacetate, propylene glycol monomethyl ether acetate, ethyl 2-butoxyacetate, and the like; siloxane-based solvents such as hexamethyldisiloxane, octamethyltrisiloxane, octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, tris (trimethylsiloxy) methylsilane, tetrakis (trimethylsiloxy) silane, and the like; fluorine-based solvents such as trifluorotoluene, hexafluoroxylene, methyl nonafluorobutyl ether, ethyl nonafluorobutyl ether and the like; or a mixed solvent thereof. For example, as the solvent used in the composition for forming a release layer, a mixed solvent of heptane and methyl isobutyl ketone may be used.
As a method of coating the composition for forming a release layer on a substrate, an off-line coating method available in the art, such as bar coating, gravure coating, die coating, etc., may be used. The energy source for curing the composition for forming the release layer is not particularly limited, but heat treatment, ultraviolet irradiation or electron beam irradiation, which may be used alone or in combination, and heat treatment may be used alone or a combination of heat treatment and ultraviolet irradiation may be used.
The heating may be performed at 60 ℃ or higher under an air atmosphere. For example, the heating may be performed at 60 ℃ or more for 24 hours under an air atmosphere. When the heating is performed at less than 60 ℃, it is difficult to introduce a portion including the fluorine-containing silane compound to the surface of the particles.
The weight ratio of the inorganic particles to the fluorine-containing silane compound may be 1:1 to 20: 1. when the weight ratio of the inorganic particles to the fluorine-containing silane compound is within the range, the peeling force can be further reduced to achieve excellent light peeling property.
In the present specification, "substitution" is induced by replacing at least one hydrogen in an unsubstituted parent group with another atom or functional group. Unless otherwise specified, when a functional group is considered to be "substituted", it means that the functional group is substituted with at least one substituent selected from an alkyl group having 1 to 40 carbon atoms, an alkenyl group having 2 to 40 carbon atoms, an alkynyl group having 2 to 40 carbon atoms, a cycloalkyl group having 3 to 40 carbon atoms, a cycloalkenyl group having 3 to 40 carbon atoms, or an aryl group having 7 to 40 carbon atoms. When a functional group is described as "optionally substituted," this means that the functional group may be substituted with the above-described substituent.
In the present specification, the monovalent hydrocarbon group of C1-C10 means, for example, a linear alkyl group such as methyl, ethyl, n-hexyl, n-octyl or n-decyl group, etc.; branched alkyl groups such as isopropyl, tert-butyl, neopentyl, isohexyl, etc.; cyclic alkyl groups such as cyclopentyl or cyclohexyl, etc.; alkenyl groups such as vinyl and allyl; aryl groups such as phenyl or tolyl; or aralkyl groups such as benzyl or phenethyl and the like. Among them, when considering the availability of raw materials, it may be an alkyl group, and when considering the usefulness of products, it may also be a methyl group or an ethyl group.
In the present specification, the alkyl group of C1 to C20 may include, for example, a linear alkyl group such as a methyl group, an ethyl group, a n-hexyl group, a n-octyl group, a n-decyl group, or the like; isopropyl, tert-butyl, neopentyl, isohexyl and the like. Among them, when considering the availability of raw materials, it may be an alkyl group, and when considering the usefulness of products, it may also be a methyl group or an ethyl group.
In the present specification, the alkenyl group having C2-C10 means a branched or unbranched hydrocarbon having at least one carbon-carbon double bond. Non-limiting examples of alkenyl groups can include vinyl, allyl, butenyl, isopropenyl, isobutenyl, or the like.
In the present specification, the alkoxy group of C1 to C20 means an alkyl group bonded to oxygen. Non-limiting examples of alkoxy groups may include methoxy, ethoxy, and the like.
The constitution of the present invention and its effect will be described in more detail by examples and comparative examples. However, it is apparent that these examples are for illustrating the present invention in more detail and the scope of the present invention is not limited to these examples.
[ examples ] A method for producing a compound
(preparation of organic-inorganic particles)
Preparation example 1: organic-inorganic particles
Silica inorganic particles (manufactured by ABC Nanotech, SILNOS 160) and Triethoxy-1H, 2H-tridecafluoro-n-octylsilane (Triethoxy-1H, 2H-tridefluoro-n-octylsilane, manufactured by TCI) as a fluorine-containing silane compound were mixed at a ratio of 4: 1 was added to 100g of ethanol and stirred for 15 minutes to obtain a mixture. While heating the mixture to 60 ℃, aminosilane (manufactured by ShinEtsu, KBP-90) as a co-reactant was slowly added in an amount of 1/4 based on the weight of the silica inorganic particles, and then reacted for 24 hours to obtain a reactant. Next, the organic-inorganic particles are prepared by removing the solvent from the reactant through a filter.
Preparation example 2: organic-inorganic particles
Organic-inorganic particles were prepared in the same manner as in preparation example 1, except that silica inorganic particles (prepared by ABC Nanotech, SILNOS 160) and Triethoxy-1H, 2H-tridecafluoro-n-octylsilane (prepared by TCI) as a fluorine-containing silane compound were mixed at a ratio of 1:1 weight ratio was added to 100g of ethanol.
Preparation example 3: organic-inorganic particles
Organic-inorganic particles were prepared in the same manner as in preparation example 1, except that silica inorganic particles (prepared by ABC Nanotech, SILNOS 160) and Triethoxy-1H, 2H-tridecafluoro-n-octylsilane (prepared by TCI) as a fluorine-containing silane compound were mixed at a ratio of 20:1 weight ratio was added to 100g of ethanol.
Preparation example 4: organic-inorganic particles
Organic-inorganic particles were prepared in the same manner as in preparation example 1, except that silica inorganic particles (prepared by ABC Nanotech, SILNOS 160) and Triethoxy-1H, 2H-nonafluorohexylsilane (prepared by TCI) as a fluorine-containing silane compound were mixed at a ratio of 4: 1 into 100g of ethanol.
Comparative preparation example 1: organic-inorganic particles
Silica inorganic particles (prepared by ABC Nanotech, E540+) were prepared.
Comparative preparation example 2: organic-inorganic particles
Organic-inorganic particles were prepared in the same manner as in preparation example 1, except that silica inorganic particles (prepared by ABC Nanotech, SILNOS 160) and Triethoxy-1H, 2H-tridecafluoro-n-octylsilane (prepared by TCI) as a fluorine-containing silane compound were mixed at a ratio of 40: 1 weight ratio was added to 100g of ethanol.
Comparative preparation example 3: organic-inorganic particles
Organic-inorganic particles were prepared in the same manner as in preparation example 1, except that silica inorganic particles (prepared by ABC Nanotech, SILNOS 160) and Trimethoxy-3,3,3-trifluoropropylsilane (Trimethoxy-3,3,3-trifluoropropylsilane, prepared by TCI) as a fluorine-containing silane compound were mixed at a ratio of 4: 1 weight ratio was added to 100g of ethanol.
Comparative preparation example 4: organic-inorganic particles
Organic-inorganic particles were prepared in the same manner as in preparation example 1, except that silica inorganic particles (prepared by ABC Nanotech, SILNOS 160) and Trimethoxy-3,3,3-trifluoropropylsilane (Trimethoxy-3,3,3-trifluoropropylsilane, prepared by TCI) as fluorine-containing silane compounds were mixed at a ratio of 1:1 weight ratio was added to 100g of ethanol.
(Release film)
Example 1: release film
A38 μm thick polyester film (Toray advanced material, XD500P) was prepared.
Separately from this, 100 parts by weight of an organopolysiloxane represented by the following Chemical formula 3 (manufactured by Dow Chemical, Q2-7785) including a fluoroalkyl group represented by the following Chemical formula 4, 3 parts by weight of a hydrogenpolysiloxane (manufactured by Dow Chemical, Q2-7560), 1 part by weight of a platinum chelate catalyst (manufactured by Dow Chemical, SYL-OFF 4000) were diluted in a mixed solvent of heptane and methyl isobutyl ketone (weight ratio; 5: 1) to prepare a composition having a total solid content of 5% by weight, and then a composition for forming a release layer was prepared by mixing the organic-inorganic particles prepared in preparation example 1 in the composition in an amount of 1% by weight based on the total solid content.
A release film was prepared by coating the composition for forming a release layer on one side of the polyester film and heat-treating in a hot air dryer at 150 ℃ for 2 minutes to form a 0.3 μm thick release layer.
< chemical formula 3>
< chemical formula 4>
In the formula (I), the compound is shown in the specification,
R1is vinyl, R2Is methyl, R3Is a fluoroalkyl group represented by the chemical formula 4;
n is 4, m is 2, and x is a binding site to an adjacent atom.
Examples 2 to 4: release film
A release film was prepared in the same manner as in example 1, except that the organic-inorganic particles prepared in preparation examples 2 to 4 were used instead of the organic-inorganic particles prepared in preparation example 1.
Comparative examples 1 to 4: release film
A release film was prepared in the same manner as in example 1, except that the (organic) inorganic particles prepared in comparative preparation example 2 to comparative preparation example 4 were used instead of the organic-inorganic particles prepared in preparation example 1.
Analytical example 1: infrared spectrum
Infrared spectroscopic analysis was performed on three kinds of silica inorganic particles, wherein the first kind of silica inorganic particles was a starting material of the release film prepared according to example 1, the second kind of silica inorganic particles was an intermediate reactant introducing aminosilane on the surface, and the third kind of silica inorganic particles was a final product introducing aminosilane and a fluorine-containing silane compound on the surface. Among them, the infrared spectral analysis was performed using Fourier transform infrared spectroscopy (FT-IR) from Perkinelmer. The results of infrared spectroscopy are shown in FIG. 2.
Referring to FIG. 2, in the silica inorganic particles as the final product, 1064cm was confirmed as compared with the silica inorganic particles as the starting material and the silica inorganic particles as the intermediate reactant-1To 1066cm-1The peak in the wavenumber range is shifted rightward, wherein the final result is silica inorganic particles having aminosilane and fluorine-containing silane compound introduced on the surface, and the intermediate reactant is silica inorganic particles having aminosilane introduced on the surface.
Evaluation example 1: evaluation of physical Properties
The physical properties of the (organic) inorganic particles prepared from preparation examples 1 to 4 and comparative preparation examples 1 to 4 and the release films prepared from example 1 to 4 and comparative example 1 to 4 were evaluated as follows, and the results thereof are shown in table 1 below.
(1) X-ray photoelectron Spectroscopy (XPS) analysis of (organic) inorganic particles
For each (organic) inorganic particle, the compositions of Si, F, C and O atoms, expressed in atomic%, were analyzed using an X-ray photoelectron spectrometer (ThermoFisher, K-ALPHA), and the content ratio (M) of F/Si element was calculatedF/MSi)。
(2) Energy dispersive spectrometer (EDAX) analysis of (organic) inorganic particles
For each of the (organic) inorganic particles, the compositions of Si, F, C and O atoms were analyzed in atomic% using an energy dispersion spectrometer (EDAX) (Hitachi, S-4800), and the content ratio of F/Si element (M) was calculatedF/MSi)。
(3) Peel force measurement from release film
Each release film was cut into a size of 500mm × 1500mm to prepare a sample. The samples shown were stored at 25 ℃ and 65% RH for 24 hours. Next, at 50 ℃, 20g/cm2Load ofA silicone-based adhesive tape (Nitto, 903UL) was pressed on the release layer of the sample for 24 hours, and then a peel force of 250mm × 1500mm size was measured at 180 ° and 0.3mpm speed using a peel force tester AR-2000 apparatus manufactured by chemistrutents. At this time, the peeling force was obtained by calculating an average value after measuring 5 times.
(4) Residual adhesion analysis of Release film
Each release film was cut into a size of 500mm × 1500mm to prepare a sample. The samples shown were stored at 25 ℃ and 65% RH for 24 hours. At room temperature and 20g/cm2After pressing an adhesive tape (Nitto, 31B) against the release layer of the sample for 24 hours under the load of (d), the adhesive tape adhered to the release layer was collected without contamination. The adhesive tape was adhered to a polyethylene terephthalate film surface having a flat and clean surface. The adhesive tape adhered to the polyethylene terephthalate film surface was pressure-bonded once with a 2kg tape roller (astm d-1000-55T) in a reciprocating manner, and a peel force of a size of 250mm × 1500mm was measured at 180 ° and a speed of 0.3mpm using a peel force tester AR-2000 apparatus manufactured by chemistruments, and then a residual tackiness rate was obtained by substituting the following formula 2.
[ formula 2 ]
Residual adhesion (%) ([ (peeling force of adhesive tape peeled off after adhering to release layer)/(peeling force of adhesive tape not adhering to release layer) × 100 ])
(5) Appearance evaluation of Release layer
Each release film was prepared as a sample of a4 size, placed on an evaluation board with a black bottom, and shrinkage cavities (crating) and appearance defects of the release layer were confirmed and recorded under a fluorescent lamp.
O: less than 2 shrinkage cavities
And (delta): 3 to 5 shrinkage cavities
X: more than 5 shrinkage cavities
[ TABLE 1 ]
Referring to table 1, it can be confirmed that the release films prepared from examples 1 to 4 have more excellent peel force (light peel property) than the release films prepared from comparative examples 1 to 4 in the range of the content ratio of F/Si element in the organic-inorganic particles prepared from preparation examples 1 to 4 included in the release films prepared from examples 1 to 4 from 0.1 to 1.0. In addition, it can be confirmed that the release films prepared from examples 1 to 4 are excellent in residual adhesion and coating appearance. In contrast, it can be confirmed that the release films prepared from comparative examples 1 and 2 have higher peel force than the release films prepared from examples 1 to 4. It can be confirmed that the organic-inorganic particles prepared from comparative preparation examples 3 to 4 included in the release films prepared from comparative preparation examples 3 to 4 have an F/Si element content ratio of less than 0.1 and a high peeling force.
Claims (13)
1. A release film, wherein a substrate and a release layer are positioned in sequence,
the surface energy of the release layer is below 24dyne/cm,
the release layer includes organic-inorganic particles,
in the organic-inorganic particles, a portion including a fluorine-containing silane compound is introduced to the surface thereof,
the organic-inorganic particles may satisfy a content ratio (M) of F/Si element represented by the following formula 1F/MSi) The range is as follows:
[ formula 1 ]
0.1≤MF/MSi≤1.0
In the formula (I), the compound is shown in the specification,
MFis the content of the F element (atom percent)SiIs the content (atom%) of the Si element.
2. The release film according to claim 1,
the fluorine-containing silane compound portion includes a fluorine-containing silane compound represented by the following chemical formula 1:
[ chemical formula 1 ]
*-OSi(Ra)(Rb)(Rc)
In the formula (I), the compound is shown in the specification,
Raand RbIs a substituted or unsubstituted C1-C20 alkoxy group;
Rcas shown in the following chemical formula 2,
is a binding site to the surface of an organic-inorganic particle,
[ chemical formula 2 ]
In the formula (I), the compound is shown in the specification,
Rdis a hydrogen atom or a substituted or unsubstituted C1-C20 alkyl group;
Reand RgIs a substituted or unsubstituted C1-C20 alkoxy group;
Rfis C4-C20 alkyl substituted by fluorine;
n1is an integer from 1 to 10;
is a binding site to a Si atom.
3. The release film according to claim 1,
the weight ratio of the organic-inorganic particles to the fluorine-containing silane compound is 1:1 to 20: 1.
4. The release film according to claim 1,
in the release layer, 1064cm in infrared spectrum was compared with the organic-inorganic particles of which surface did not include a fluorine-containing silane compound moiety-1To 1066cm-1Peaks in the wavenumber range are shifted to the right.
5. The release film according to claim 1,
the organic-inorganic particles include natural minerals; an oxide, hydroxide, sulfide, nitride or halide of a group 1 to group 4, group 11 to group 12, group 14 and group 16 to group 18 element; carbonates, sulfates, acetates, phosphates, phosphites, carboxylates, silicates, titanates, borates or hydrates thereof; and inorganic particles selected from complex compounds thereof.
6. The release film according to claim 1,
the release layer further comprises a polymer or copolymer containing a fluorine-containing polysiloxane.
7. The release film according to claim 6,
the fluorine-containing polysiloxane includes an organopolysiloxane represented by the following chemical formula 3:
< chemical formula 3>
< chemical formula 4>
< chemical formula 5>
In the formula (I), the compound is shown in the specification,
R1is a substituted or unsubstituted monovalent hydrocarbon group of C1-C10, or a substituted or unsubstituted alkenyl group of C2-C10;
R2is a substituted or unsubstituted C1-C10 monovalent hydrocarbon radical, a substituted or unsubstituted C2-C10 alkenyl radical, or hydrogen;
R3is a fluorine-containing alkyl group represented by the chemical formula 4, a fluorine-containing ether group represented by the chemical formula 5, or a combination thereof;
n is an integer of 1 to 8, m is an integer of 1 to 5;
p is an integer from 1 to 5, q is 0 or 1, r is 0, 1 or 2, v is an integer from 1 to 5;
a is oxygen atom or single bond;
x, y and z are integers of 1 or more;
is a binding site to an adjacent atom;
wherein R is1And R2At least one of which is a substituted or unsubstituted C2-C10 alkenyl group.
8. The release film according to claim 1,
the release layer further includes at least one of a hydrogen polysiloxane and an acid catalyst.
9. The release film according to claim 1,
the release film has a peel force of 23gf/25mm or less.
10. The release film according to claim 1,
the residual adhesion rate of the release film is more than 90%.
11. A method for preparing a release film, comprising: preparing a base material;
adding and stirring inorganic particles, a fluorine-containing silane compound and an aminosilane-based co-reactant, and then heating to prepare organic-inorganic particles; and
the release film according to claim 1, which is prepared by coating a composition for forming a release layer comprising a polymer or copolymer comprising a fluorine-containing polysiloxane, and organic-inorganic particles on at least one side of the substrate and drying to form a release layer,
the weight ratio of the inorganic particles to the fluorine-containing silane compound is 4: 1 to 20: 1.
12. the method for preparing a release film according to claim 11,
the heating is carried out at 60 ℃ or higher in an air atmosphere.
13. The method for preparing a release film according to claim 11,
the weight ratio of the inorganic particles to the fluorine-containing silane compound is 1:1 to 20: 1.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020200148144A KR102531723B1 (en) | 2020-11-06 | 2020-11-06 | Release film and manufacturing method thereof |
| KR10-2020-0148144 | 2020-11-06 | ||
| PCT/KR2021/008193 WO2022097872A1 (en) | 2020-11-06 | 2021-06-29 | Release film and preparation method therefor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114729145A true CN114729145A (en) | 2022-07-08 |
| CN114729145B CN114729145B (en) | 2023-12-01 |
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| CN202180002509.8A Active CN114729145B (en) | 2020-11-06 | 2021-06-29 | Release film and preparation method thereof |
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| KR (1) | KR102531723B1 (en) |
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| CN115536890B (en) * | 2022-11-04 | 2023-07-07 | 惠州市鑫亚凯立科技有限公司 | Optical fluorine release film with three-dimensional micro-nano structure and manufacturing method thereof |
| KR102601242B1 (en) | 2022-12-27 | 2023-11-14 | 이에프티솔루션주식회사 | Functional nano composite release film |
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| US20100233494A1 (en) * | 2009-03-11 | 2010-09-16 | Xerox Corporation | Self-releasing nanoparticle fillers in fusing members |
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| WO2020209450A1 (en) * | 2019-04-11 | 2020-10-15 | 도레이첨단소재 주식회사 | Fluorine group-containing release film |
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| KR102248716B1 (en) * | 2014-09-30 | 2021-05-04 | 코오롱인더스트리 주식회사 | Release film and manufacturing method thereof |
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2020
- 2020-11-06 KR KR1020200148144A patent/KR102531723B1/en active IP Right Grant
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- 2021-06-29 CN CN202180002509.8A patent/CN114729145B/en active Active
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| CN101932661A (en) * | 2007-12-05 | 2010-12-29 | 纳幕尔杜邦公司 | Inorganic particles hydrophobized with fluoroalkyl silanes |
| US20100233494A1 (en) * | 2009-03-11 | 2010-09-16 | Xerox Corporation | Self-releasing nanoparticle fillers in fusing members |
| US9777161B1 (en) * | 2010-08-16 | 2017-10-03 | The United States Of America As Represented By The Secretary Of The Air Force | Fluoroalkylsilanated mesoporous metal oxide particles and methods of preparation thereof |
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| WO2020209450A1 (en) * | 2019-04-11 | 2020-10-15 | 도레이첨단소재 주식회사 | Fluorine group-containing release film |
| CN110951288A (en) * | 2019-12-02 | 2020-04-03 | 华南协同创新研究院 | Silane low-surface-energy material capable of regulating interface wettability and preparation method and application thereof |
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| KR20220061777A (en) | 2022-05-13 |
| WO2022097872A1 (en) | 2022-05-12 |
| CN114729145B (en) | 2023-12-01 |
| KR102531723B1 (en) | 2023-05-11 |
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