JP2011021156A - Mold detergent composition and mold detergent, and method for cleaning mold using the same - Google Patents
Mold detergent composition and mold detergent, and method for cleaning mold using the same Download PDFInfo
- Publication number
- JP2011021156A JP2011021156A JP2009169330A JP2009169330A JP2011021156A JP 2011021156 A JP2011021156 A JP 2011021156A JP 2009169330 A JP2009169330 A JP 2009169330A JP 2009169330 A JP2009169330 A JP 2009169330A JP 2011021156 A JP2011021156 A JP 2011021156A
- Authority
- JP
- Japan
- Prior art keywords
- mold
- cleaning
- molding
- resin
- alkali metal
- 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
Links
- 239000000203 mixture Substances 0.000 title claims abstract description 70
- 238000004140 cleaning Methods 0.000 title claims description 92
- 238000000034 method Methods 0.000 title claims description 15
- 239000003599 detergent Substances 0.000 title abstract description 7
- 229920003051 synthetic elastomer Polymers 0.000 claims abstract description 35
- 239000005061 synthetic rubber Substances 0.000 claims abstract description 35
- -1 alkali metal salt Chemical class 0.000 claims abstract description 34
- 239000000463 material Substances 0.000 claims abstract description 26
- 239000002585 base Substances 0.000 claims abstract description 24
- 229920003002 synthetic resin Polymers 0.000 claims abstract description 24
- 239000000057 synthetic resin Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 21
- 150000008044 alkali metal hydroxides Chemical class 0.000 claims abstract description 15
- 239000012778 molding material Substances 0.000 claims abstract description 15
- 239000011538 cleaning material Substances 0.000 claims description 39
- 239000000356 contaminant Substances 0.000 claims description 28
- 239000003795 chemical substances by application Substances 0.000 claims description 21
- 229910052751 metal Inorganic materials 0.000 claims description 18
- 239000002184 metal Substances 0.000 claims description 18
- 229920002857 polybutadiene Polymers 0.000 claims description 14
- 239000005062 Polybutadiene Substances 0.000 claims description 13
- 229920000181 Ethylene propylene rubber Polymers 0.000 claims description 11
- 238000003856 thermoforming Methods 0.000 claims description 2
- 150000001340 alkali metals Chemical class 0.000 claims 1
- 238000000465 moulding Methods 0.000 abstract description 44
- 230000003252 repetitive effect Effects 0.000 abstract 1
- 229920005989 resin Polymers 0.000 description 31
- 239000011347 resin Substances 0.000 description 31
- 229920001971 elastomer Polymers 0.000 description 19
- 239000005060 rubber Substances 0.000 description 19
- 229920001187 thermosetting polymer Polymers 0.000 description 16
- 238000001723 curing Methods 0.000 description 14
- 239000003822 epoxy resin Substances 0.000 description 13
- 229920000647 polyepoxide Polymers 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 238000011156 evaluation Methods 0.000 description 11
- 238000002156 mixing Methods 0.000 description 9
- 239000004065 semiconductor Substances 0.000 description 9
- 229920000877 Melamine resin Polymers 0.000 description 8
- 239000004640 Melamine resin Substances 0.000 description 8
- UTOPWMOLSKOLTQ-UHFFFAOYSA-N octacosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCCCCCC(O)=O UTOPWMOLSKOLTQ-UHFFFAOYSA-N 0.000 description 8
- 239000011342 resin composition Substances 0.000 description 8
- 150000003839 salts Chemical class 0.000 description 8
- 230000000694 effects Effects 0.000 description 7
- 239000006082 mold release agent Substances 0.000 description 7
- 229920002943 EPDM rubber Polymers 0.000 description 6
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 5
- 229910052736 halogen Inorganic materials 0.000 description 5
- 150000002367 halogens Chemical class 0.000 description 5
- 229920013716 polyethylene resin Polymers 0.000 description 5
- 239000003566 sealing material Substances 0.000 description 5
- 238000001721 transfer moulding Methods 0.000 description 5
- 239000001993 wax Substances 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 239000005977 Ethylene Substances 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 239000004203 carnauba wax Substances 0.000 description 4
- 235000013869 carnauba wax Nutrition 0.000 description 4
- 238000011109 contamination Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000001746 injection moulding Methods 0.000 description 4
- 239000000178 monomer Substances 0.000 description 4
- 150000001451 organic peroxides Chemical class 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 150000002989 phenols Chemical class 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000012744 reinforcing agent Substances 0.000 description 4
- 238000007789 sealing Methods 0.000 description 4
- 239000004711 α-olefin Substances 0.000 description 4
- 229920000459 Nitrile rubber Polymers 0.000 description 3
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 3
- 229910019142 PO4 Inorganic materials 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- RWRDLPDLKQPQOW-UHFFFAOYSA-N Pyrrolidine Chemical compound C1CCNC1 RWRDLPDLKQPQOW-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000008065 acid anhydrides Chemical class 0.000 description 3
- 230000002411 adverse Effects 0.000 description 3
- 239000012670 alkaline solution Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 150000004668 long chain fatty acids Chemical class 0.000 description 3
- 239000010452 phosphate Substances 0.000 description 3
- 150000004291 polyenes Chemical class 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- 239000004636 vulcanized rubber Substances 0.000 description 3
- RXYPXQSKLGGKOL-UHFFFAOYSA-N 1,4-dimethylpiperazine Chemical compound CN1CCN(C)CC1 RXYPXQSKLGGKOL-UHFFFAOYSA-N 0.000 description 2
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- LLPKQRMDOFYSGZ-UHFFFAOYSA-N 2,5-dimethyl-1h-imidazole Chemical compound CC1=CN=C(C)N1 LLPKQRMDOFYSGZ-UHFFFAOYSA-N 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-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
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 2
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 description 2
- 239000004593 Epoxy Substances 0.000 description 2
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 2
- 244000043261 Hevea brasiliensis Species 0.000 description 2
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 2
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 2
- AFBPFSWMIHJQDM-UHFFFAOYSA-N N-methylaniline Chemical compound CNC1=CC=CC=C1 AFBPFSWMIHJQDM-UHFFFAOYSA-N 0.000 description 2
- PVNIIMVLHYAWGP-UHFFFAOYSA-N Niacin Chemical compound OC(=O)C1=CC=CN=C1 PVNIIMVLHYAWGP-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- NQRYJNQNLNOLGT-UHFFFAOYSA-N Piperidine Chemical compound C1CCNCC1 NQRYJNQNLNOLGT-UHFFFAOYSA-N 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 2
- 235000011054 acetic acid Nutrition 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 2
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 description 2
- 230000001588 bifunctional effect Effects 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 229920005549 butyl rubber Polymers 0.000 description 2
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical compound CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 2
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 2
- UKMSUNONTOPOIO-UHFFFAOYSA-N docosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCC(O)=O UKMSUNONTOPOIO-UHFFFAOYSA-N 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 229910052731 fluorine Inorganic materials 0.000 description 2
- 239000011737 fluorine Substances 0.000 description 2
- 159000000011 group IA salts Chemical class 0.000 description 2
- 150000004820 halides Chemical group 0.000 description 2
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 2
- 239000000383 hazardous chemical Substances 0.000 description 2
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 description 2
- 150000002460 imidazoles Chemical class 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 238000004898 kneading Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 229920003052 natural elastomer Polymers 0.000 description 2
- 229920001194 natural rubber Polymers 0.000 description 2
- 230000007935 neutral effect Effects 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical class OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 230000003578 releasing effect Effects 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- YGSDEFSMJLZEOE-UHFFFAOYSA-N salicylic acid Chemical compound OC(=O)C1=CC=CC=C1O YGSDEFSMJLZEOE-UHFFFAOYSA-N 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
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- 229920001897 terpolymer Polymers 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 description 2
- RIOQSEWOXXDEQQ-UHFFFAOYSA-N triphenylphosphine Chemical compound C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 RIOQSEWOXXDEQQ-UHFFFAOYSA-N 0.000 description 2
- QEQBMZQFDDDTPN-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy benzenecarboperoxoate Chemical compound CC(C)(C)OOOC(=O)C1=CC=CC=C1 QEQBMZQFDDDTPN-UHFFFAOYSA-N 0.000 description 1
- MYOQALXKVOJACM-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy pentaneperoxoate Chemical compound CCCCC(=O)OOOC(C)(C)C MYOQALXKVOJACM-UHFFFAOYSA-N 0.000 description 1
- KDGNCLDCOVTOCS-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy propan-2-yl carbonate Chemical compound CC(C)OC(=O)OOC(C)(C)C KDGNCLDCOVTOCS-UHFFFAOYSA-N 0.000 description 1
- MUTGBJKUEZFXGO-OLQVQODUSA-N (3as,7ar)-3a,4,5,6,7,7a-hexahydro-2-benzofuran-1,3-dione Chemical compound C1CCC[C@@H]2C(=O)OC(=O)[C@@H]21 MUTGBJKUEZFXGO-OLQVQODUSA-N 0.000 description 1
- PRBHEGAFLDMLAL-GQCTYLIASA-N (4e)-hexa-1,4-diene Chemical compound C\C=C\CC=C PRBHEGAFLDMLAL-GQCTYLIASA-N 0.000 description 1
- RIPYNJLMMFGZSX-UHFFFAOYSA-N (5-benzoylperoxy-2,5-dimethylhexan-2-yl) benzenecarboperoxoate Chemical compound C=1C=CC=CC=1C(=O)OOC(C)(C)CCC(C)(C)OOC(=O)C1=CC=CC=C1 RIPYNJLMMFGZSX-UHFFFAOYSA-N 0.000 description 1
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- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 description 1
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- KYVBNYUBXIEUFW-UHFFFAOYSA-N 1,1,3,3-tetramethylguanidine Chemical compound CN(C)C(=N)N(C)C KYVBNYUBXIEUFW-UHFFFAOYSA-N 0.000 description 1
- NALFRYPTRXKZPN-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane Chemical compound CC1CC(C)(C)CC(OOC(C)(C)C)(OOC(C)(C)C)C1 NALFRYPTRXKZPN-UHFFFAOYSA-N 0.000 description 1
- HSLFISVKRDQEBY-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)cyclohexane Chemical compound CC(C)(C)OOC1(OOC(C)(C)C)CCCCC1 HSLFISVKRDQEBY-UHFFFAOYSA-N 0.000 description 1
- VZXTWGWHSMCWGA-UHFFFAOYSA-N 1,3,5-triazine-2,4-diamine Chemical compound NC1=NC=NC(N)=N1 VZXTWGWHSMCWGA-UHFFFAOYSA-N 0.000 description 1
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- 239000004912 1,5-cyclooctadiene Substances 0.000 description 1
- UICXTANXZJJIBC-UHFFFAOYSA-N 1-(1-hydroperoxycyclohexyl)peroxycyclohexan-1-ol Chemical compound C1CCCCC1(O)OOC1(OO)CCCCC1 UICXTANXZJJIBC-UHFFFAOYSA-N 0.000 description 1
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- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 1
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- LBLYYCQCTBFVLH-UHFFFAOYSA-N 2-Methylbenzenesulfonic acid Chemical compound CC1=CC=CC=C1S(O)(=O)=O LBLYYCQCTBFVLH-UHFFFAOYSA-N 0.000 description 1
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Landscapes
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Abstract
Description
本発明は、射出成形またはトランスファー成形等の成形作業の繰り返しにより汚染された金型、例えば、熱硬化性樹脂組成物の成形作業に用いた半導体装置成形用金型等の洗浄再生等に用いられる金型洗浄剤組成物および金型洗浄材、ならびにそれを用いた金型のクリーニング方法に関するものである。 INDUSTRIAL APPLICABILITY The present invention is used for cleaning and regeneration of a mold contaminated by repeated molding operations such as injection molding or transfer molding, for example, a mold for molding a semiconductor device used for molding a thermosetting resin composition. The present invention relates to a mold cleaning composition, a mold cleaning material, and a mold cleaning method using the same.
一般に、射出成形またはトランスファー成形等の成形作業の繰り返しにより金型は、成形材料を加熱した際に発生する揮発成分、成形品表面への滲出物、成形時に使用される離型剤等がその金型表面に付着し、さらにこれら付着物が酸化により変質することによって汚染される。このように金型が汚染すると、成形品の仕上がり寸法、外観、離型性等に悪影響を及ぼすこととなり好ましいことではない。 In general, a mold is made up of a volatile component generated when a molding material is heated, exudates on the surface of the molded product, a mold release agent used during molding, etc. by repeating molding operations such as injection molding or transfer molding. It adheres to the mold surface, and further, these deposits are contaminated by alteration due to oxidation. If the mold is contaminated in this manner, it is not preferable because it adversely affects the finished size, appearance, releasability, and the like of the molded product.
したがって、このような汚染された金型による悪影響を防止するため、射出成形またはトランスファー成形等に用いる金型は、定期的に洗浄作業が行なわれ、上記汚染物を金型表面から除去する必要がある。従来の金型の洗浄方法としては、例えば、成形装置から金型を外して強アルカリ溶液や溶剤を用いて洗浄する方法等が知られている。 Therefore, in order to prevent such an adverse effect due to the contaminated mold, the mold used for injection molding or transfer molding or the like needs to be periodically cleaned to remove the contaminants from the mold surface. is there. As a conventional mold cleaning method, for example, a method of removing a mold from a molding apparatus and cleaning it using a strong alkaline solution or a solvent is known.
しかしながら、成形装置から金型を外して強アルカリ溶液や溶剤を用いて洗浄する方法は、金型の冷却・昇温、脱着、洗浄等の工程が必要であり、洗浄に長時間を要するという問題があり労力も大きく、さらに、強アルカリ溶液や溶剤の使用による作業者への悪影響、洗浄後の廃液処理等、人や環境に与える負荷が大きいという問題があった。 However, the method of removing the mold from the molding apparatus and cleaning it with a strong alkaline solution or solvent requires steps such as cooling / heating of the mold, desorption, and cleaning, and requires a long time for cleaning. In addition, there is a problem in that the labor is large and the load on humans and the environment is large, such as adverse effects on workers due to the use of strong alkaline solutions and solvents, and waste liquid treatment after washing.
このようなことから、熱硬化性メラミン樹脂成形材料、未加硫ゴム系コンパウンド等を使用し、これらを用いて金型内で成形することにより金型表面に生成した汚染物を成形物と一体化させ、この成形物を金型から取り出すことにより金型表面を洗浄するという方法が提案され一部で実施されている（例えば、特許文献１参照）。 For this reason, thermosetting melamine resin molding materials, unvulcanized rubber compounds, etc. are used, and the contaminants generated on the mold surface by molding in these molds are integrated with the molding. A method of cleaning the surface of the mold by removing the molded product from the mold has been proposed and implemented in part (see, for example, Patent Document 1).
例えば、熱硬化性樹脂組成物の成形作業に用いた半導体装置成形用金型は、上記方法により洗浄が行なわれているが、上記熱硬化性樹脂組成物は、その要求特性によって構成する成分組成が異なり多種類であって、成形作業の繰り返しにより発生する金型汚染の状態および汚染物の成分そのものも多種多様である。なかでも、鉛やハロゲンに代表される環境負荷物質を排除した、ノンハロゲンの環境対応樹脂成形材料を用いて成形を繰り返した際の金型に形成された汚染物質は、金型表面に対する焼き付けが特にひどく、前述の熱硬化性メラミン樹脂成形材料や未加硫ゴム系コンパウンドを用いた従来の洗浄方法では汚染物質を完全に除去することが不可能であり、このような汚染物質に対しても洗浄可能となるような洗浄材料が望まれている。 For example, a mold for molding a semiconductor device used for a molding operation of a thermosetting resin composition is cleaned by the above method, but the thermosetting resin composition has a component composition constituted by its required characteristics. However, there are many types, and the state of mold contamination generated by repeated molding operations and the components of the contaminants are also various. In particular, contaminants formed on molds when molding with non-halogen environmentally friendly resin molding materials that exclude environmentally hazardous substances such as lead and halogen are particularly baked on the mold surface. Severely, the conventional cleaning method using the thermosetting melamine resin molding material and the unvulcanized rubber compound described above cannot completely remove the contaminants. There is a desire for a cleaning material that would enable it.
本発明は、このような事情に鑑みなされたもので、成形作業の繰り返しにより汚染された金型に対して優れた洗浄効果を発揮する金型洗浄剤組成物および金型洗浄材、ならびにそれを用いた金型のクリーニング方法の提供をその目的とする。 The present invention has been made in view of such circumstances, a mold cleaning composition and a mold cleaning material that exhibit an excellent cleaning effect on a mold contaminated by repeated molding operations, and the same. The object is to provide a cleaning method for the mold used.
上記の目的を達成するため、本発明は、成形材料を用い繰り返し成形を行う加熱成形用金型の洗浄剤組成物であって、上記洗浄剤組成物が、母材となる合成ゴムおよび合成樹脂の少なくとも一方と、アルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方と、水を含有してなる金型洗浄剤組成物を第１の要旨とする。 In order to achieve the above object, the present invention provides a cleaning composition for a thermoforming mold in which molding is repeatedly performed using a molding material, and the cleaning composition is a synthetic rubber and a synthetic resin that serve as a base material. A first aspect of the present invention is a mold cleaning composition containing at least one of the above, at least one of an alkali metal salt and an alkali metal hydroxide, and water.
また、本発明は、金型洗浄剤組成物を用いてシート状に形成されてなる金型洗浄材を第２の要旨とする。 Moreover, this invention makes the 2nd summary the metal mold | die cleaning material formed in a sheet form using a metal mold | die cleaning composition.
そして、本発明は、上記金型洗浄剤組成物からなる金型洗浄材を、開いた金型の型面に載置する工程と、上記金型を締めて上記金型洗浄材を挟み加熱加圧することにより、金型の表面に形成された汚染物を上記金型洗浄材に一体化させる工程と、汚染物が一体化した金型洗浄材を金型から剥離することにより、金型表面をクリーニングする工程とを備えた金型のクリーニング方法を第３の要旨とする。 Then, the present invention includes a step of placing a mold cleaning material comprising the above-described mold cleaning composition on the mold surface of the opened mold, and clamping the mold and sandwiching the mold cleaning material to heat the mold cleaning material. The process of integrating the contaminants formed on the mold surface into the mold cleaning material by pressing, and the mold cleaning material integrated with the contaminants is peeled from the mold to remove the mold surface. A third gist is a mold cleaning method including a cleaning step.
すなわち、本発明者らは、先に述べたように、ノンハロゲンの環境対応樹脂成形材料を用いて成形を繰り返した際の金型に形成される汚染物質でさえも効果的に洗浄除去することのできる洗浄剤組成物を得るべく鋭意検討を重ねた。その結果、母材となる合成ゴムおよび合成樹脂の少なくとも一方と、アルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方と、水を含有すると、水の作用によって汚れの溶解や分解作用を生じるとともに、上記アルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方を併存させることによって、汚れの溶解や分解作用を促進するという作用を奏することから、これらの相乗作用により、従来に比べてより一層優れた洗浄効果を発揮することを見出し本発明に到達した。 That is, as described above, the present inventors can effectively clean and remove even the contaminants formed on the mold when the molding is repeated using a non-halogen environmentally-friendly resin molding material. The earnest examination was repeated in order to obtain the cleaning composition which can be performed. As a result, when containing at least one of a synthetic rubber and a synthetic resin as a base material, at least one of an alkali metal salt and an alkali metal hydroxide, and water, it causes dissolution and decomposition of dirt by the action of water, By coexisting at least one of the alkali metal salt and the alkali metal hydroxide, the effect of accelerating the dissolution and decomposition of dirt is achieved. The inventors have found that the present invention is effective and have reached the present invention.
このように、本発明の金型洗浄剤組成物は、母材となる合成ゴムおよび合成樹脂の少なくとも一方と、アルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方と、水を必須成分として含有するものである。このため、成形作業の繰り返しにより形成された汚染物、特に従来の洗浄用組成物では充分な洗浄が困難であった、熱硬化性樹脂成形材料の鉛やハロゲン、アンチモンに代表される環境負荷物質を排除した、ノンハロゲンの環境対応樹脂成形材料を用いて成形作業を繰り返した際の金型表面に形成される汚染物質に対しても、水の作用によって汚れの溶解や分解作用を生じるとともに、上記アルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方を併存させることによって、汚れの溶解や分解作用を促進するという効果の相乗作用から、優れた洗浄除去作用を発揮する。したがって、本発明の金型洗浄剤組成物を用いて金型表面の洗浄を行うことにより、金型表面に形成された汚染物がこの金型洗浄剤組成物に付着して一体化し金型から汚染物が効果的に除去されることとなり、例えば、エポキシ樹脂組成物を用いて繰り返し成形した半導体素子封止用の金型表面の汚染物がこの金型洗浄剤組成物からなる成形品と一体化し、金型から汚染物が効果的に除去されて金型の洗浄が効果的になされる。その結果、本発明の金型洗浄剤組成物により洗浄された金型を用いて形成される半導体装置は、外観的にも問題のない優れた製品が得られる。そして、本発明の金型洗浄剤組成物からなる金型洗浄材を、開いた金型の型面に載置した後、上記金型を締めて上記金型洗浄材を挟み加熱加圧することにより、金型の表面に形成された汚染物を上記金型洗浄材に一体化させ、汚染物が一体化した金型洗浄材を金型から剥離することにより、金型表面をクリーニングすることが可能となる。 Thus, the mold cleaning composition of the present invention contains at least one of a synthetic rubber and a synthetic resin as a base material, at least one of an alkali metal salt and an alkali metal hydroxide, and water as essential components. Is. For this reason, environmentally hazardous substances typified by lead, halogen, and antimony of thermosetting resin molding materials that are difficult to clean sufficiently with contaminants formed by repeated molding operations, particularly conventional cleaning compositions. Contaminants are dissolved and decomposed by the action of water, even on contaminants formed on the mold surface when molding operations are repeated using non-halogen environmentally friendly resin molding materials The coexistence of at least one of an alkali metal salt and an alkali metal hydroxide exhibits an excellent cleaning and removing action from the synergistic effect of promoting the dissolution and decomposition action of dirt. Therefore, by cleaning the mold surface using the mold cleaning composition of the present invention, contaminants formed on the mold surface adhere to the mold cleaning composition and are integrated into the mold. Contaminants are effectively removed. For example, contaminants on the surface of a mold for sealing a semiconductor element, which are repeatedly molded using an epoxy resin composition, are integrated with a molded product made of this mold cleaning composition. Thus, contaminants are effectively removed from the mold, and the mold is effectively cleaned. As a result, a semiconductor device formed using a mold cleaned with the mold cleaning composition of the present invention can provide an excellent product having no problem in appearance. Then, after placing the mold cleaning material comprising the mold cleaning composition of the present invention on the mold surface of the opened mold, the mold cleaning material is tightened and the mold cleaning material is sandwiched and heated and pressed. It is possible to clean the mold surface by integrating the contaminants formed on the mold surface into the mold cleaning material and peeling the mold cleaning material with the contaminants integrated from the mold. It becomes.
そして、上記合成ゴムが、エチレン−プロピレン系ゴムおよび／またはブタジエンゴムであると、金型洗浄の際の取り扱いが容易となり洗浄作業性の向上が実現する。 If the synthetic rubber is ethylene-propylene rubber and / or butadiene rubber, handling during mold cleaning is facilitated, and cleaning workability is improved.
また、上記アルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方の含有量を、母材となる合成ゴムおよび合成樹脂の少なくとも一方１００重量部に対して特定の割合に設定すると、より一層優れた洗浄作用が得られるようになる。 Further, when the content of at least one of the alkali metal salt and the alkali metal hydroxide is set to a specific ratio with respect to 100 parts by weight of at least one of the synthetic rubber and the synthetic resin as a base material, further excellent cleaning is performed. The effect comes to be obtained.
さらに、上記水の含有量を、母材となる合成ゴムおよび合成樹脂の少なくとも一方１００重量部に対して特定の割合に設定すると、より一層優れた洗浄作用が得られるようになる。 Furthermore, when the water content is set to a specific ratio with respect to 100 parts by weight of at least one of the synthetic rubber and the synthetic resin as a base material, a further excellent cleaning action can be obtained.
つぎに、本発明の実施の形態を詳しく説明する。 Next, embodiments of the present invention will be described in detail.
本発明の金型洗浄剤組成物は、母材となる合成ゴムおよび合成樹脂の少なくとも一方と、アルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方と、水を必須成分として用いて得られるものである。 The mold cleaning composition of the present invention is obtained using at least one of a synthetic rubber and a synthetic resin as a base material, at least one of an alkali metal salt and an alkali metal hydroxide, and water as essential components. is there.
上記合成ゴムは、いわゆる未加硫ゴムであり、例えば、天然ゴム（ＮＲ）、ブタジエンゴム（ＢＲ）、ニトリルゴム（ＮＢＲ）、エチレン−プロピレンゴム（ＥＰＲ）等のエチレン−α−オレフィンゴム、スチレン−ブタジエンゴム（ＳＢＲ）、ポリイソプレンゴム（ＩＲ）、ブチルゴム（ＩＩＲ）、シリコーンゴム（Ｑ）、フッ素ゴム（ＦＫＭ）等があげられる。これらは単独でもしくは２種以上併せて用いられる。なお、本発明においては、上記エチレン−α−オレフィンゴムには、エチレン−プロピレン−ポリエンゴム（ＥＰＤＭ）等のエチレン−α−オレフィン−ポリエンゴムをも含む。そして、これら未加硫ゴムは、金型内において加硫され加硫ゴムとなる。 The synthetic rubber is a so-called unvulcanized rubber, such as ethylene-α-olefin rubber such as natural rubber (NR), butadiene rubber (BR), nitrile rubber (NBR), ethylene-propylene rubber (EPR), styrene, etc. -Butadiene rubber (SBR), polyisoprene rubber (IR), butyl rubber (IIR), silicone rubber (Q), fluorine rubber (FKM) and the like. These may be used alone or in combination of two or more. In the present invention, the ethylene-α-olefin rubber includes ethylene-α-olefin-polyene rubber such as ethylene-propylene-polyene rubber (EPDM). These unvulcanized rubbers are vulcanized in the mold to become vulcanized rubbers.
上記合成ゴムのなかでも、金型を用いた成形に際して、汚染性が少ない、また加硫時の臭気が少ないという点から、ＥＰＲ（ＥＰＤＭを含む）、ＢＲを単独でもしくはこれらの混合物が好ましく用いられる。 Among the above synthetic rubbers, EPR (including EPDM), BR alone or a mixture thereof is preferably used from the viewpoint of low contamination during molding using a mold and low odor during vulcanization. It is done.
上記ＥＰＤＭについて詳述すると、ＥＰＤＭはエチレン，α−オレフィン（特にプロピレン）および以下に列挙するポリエンモノマーからなるターポリマーであり、上記ポリエンモノマーとしては、ジシクロペンタジエン、１，５−シクロオクタジエン、１，１−シクロオクタジエン、１，６−シクロドデカジエン、１，７−シクロドデカジエン、１，５，９−シクロドデカトリエン、１，４−シクロヘプタジエン、１，４−シクロヘキサジエン、ノルボルナジエン、メチレンノルボルネン、２−メチル−１，４−ペンタジエン、１，５−ヘキサジエン、１，６−ヘプタジエン、メチル−テトラヒドロインデン、１，４−ヘキサジエン等があげられる。 The EPDM will be described in detail. The EPDM is a terpolymer composed of ethylene, α-olefin (particularly propylene) and the polyene monomer listed below. Examples of the polyene monomer include dicyclopentadiene, 1,5-cyclooctadiene, 1,1-cyclooctadiene, 1,6-cyclododecadiene, 1,7-cyclododecadiene, 1,5,9-cyclododecatriene, 1,4-cycloheptadiene, 1,4-cyclohexadiene, norbornadiene Methylene norbornene, 2-methyl-1,4-pentadiene, 1,5-hexadiene, 1,6-heptadiene, methyl-tetrahydroindene, 1,4-hexadiene and the like.
上記ＥＰＤＭにおける各モノマーの共重合割合は、好ましくはエチレンが３０〜８０モル％、ポリエンモノマーが０．１〜２０モル％で、残りがα−オレフィンとなるようなターポリマーである。より好ましいのはエチレンが３０〜６０モル％である。 The copolymerization ratio of each monomer in the EPDM is preferably a terpolymer in which ethylene is 30 to 80 mol%, polyene monomer is 0.1 to 20 mol%, and the remainder is an α-olefin. More preferably, ethylene is 30 to 60 mol%.
また、上記ＢＲとしては、１，２−ポリブタジエン、１，４−ポリブタジエンをそれぞれ単独でもしくは併用してなる混合物として使用される。 Moreover, as said BR, 1, 2- polybutadiene and 1, 4- polybutadiene are used individually or in mixture as a combination, respectively.
上記合成樹脂としては、例えば、ナイロン６やナイロン６６等のポリアミド樹脂、ポリエチレンテレフタレートやポリブチレンテレフタレート等のポリエステル樹脂、ポリカーボネート樹脂、ポリアリレート樹脂、塩化ビニル樹脂、塩素化塩化ビニル樹脂、ポリエチレン樹脂、塩素化ポリエチレン樹脂、塩素化ポリプロピレン樹脂、ポリプロピレン樹脂、ポリスチレン樹脂、アクリルニトリル・スチレン系樹脂、塩化ビニリデン樹脂、酢酸ビニル樹脂、ポリアクリレート樹脂、ポリイミド樹脂、ブタジエン樹脂、ポリアセタール樹脂、アイオノマー樹脂、エチレン−塩化ビニル共重合樹脂、エチレン−酢酸ビニルコポリマー樹脂、エチレン−酢酸ビニル−塩化ビニルグラフト重合樹脂、ポリフェニレン樹脂、ポリサルフォン樹脂、メタクリル樹脂、アクリル−フッ素樹脂、アクリル−シリコーンオリゴマー、シリコーン樹脂、エポキシ含有シリコーン・アクリル樹脂、ビニルエステル樹脂、フラン樹脂、フェノール樹脂、メラミン樹脂、グアナミン樹脂、ユリア樹脂、ポリウレタン樹脂、ジアクリルフタレート樹脂、ケトン樹脂、エポキシ樹脂、キシレン樹脂、マレイン樹脂、フェノキシ樹脂、クマロン樹脂、ポリビニルホルマール樹脂、ポリビニルブチラール樹脂等があげられる。これらは単独でもしくは２種以上併せて用いることができる。これら合成樹脂のなかでも、金型を用いた成形に際して汚染が少ないという点から、ポリエチレン樹脂、エポキシ樹脂、メラミン樹脂が好適に用いられる。 Examples of the synthetic resin include polyamide resins such as nylon 6 and nylon 66, polyester resins such as polyethylene terephthalate and polybutylene terephthalate, polycarbonate resins, polyarylate resins, vinyl chloride resins, chlorinated vinyl chloride resins, polyethylene resins, chlorine Polyethylene resin, chlorinated polypropylene resin, polypropylene resin, polystyrene resin, acrylonitrile / styrene resin, vinylidene chloride resin, vinyl acetate resin, polyacrylate resin, polyimide resin, butadiene resin, polyacetal resin, ionomer resin, ethylene-vinyl chloride Copolymer resin, ethylene-vinyl acetate copolymer resin, ethylene-vinyl acetate-vinyl chloride graft polymer resin, polyphenylene resin, polysulfone resin, methacryl Fat, acrylic-fluorine resin, acrylic-silicone oligomer, silicone resin, epoxy-containing silicone / acrylic resin, vinyl ester resin, furan resin, phenol resin, melamine resin, guanamine resin, urea resin, polyurethane resin, diacryl phthalate resin, ketone Resins, epoxy resins, xylene resins, maleic resins, phenoxy resins, coumarone resins, polyvinyl formal resins, polyvinyl butyral resins, and the like. These may be used alone or in combination of two or more. Among these synthetic resins, polyethylene resin, epoxy resin, and melamine resin are preferably used because they are less contaminated during molding using a mold.
そして、これら合成ゴムおよび合成樹脂の少なくとも一方からなる母材において、合成ゴムまたは合成樹脂を各々単独で用いてもよいし、合成ゴムおよび合成樹脂を組み合わせて用いても、さらには各々複数種類を組み合わせて用いてもよい。なかでも、金型洗浄を行なう際の取り扱いが容易であるという点から、合成ゴム、ポリエチレン樹脂、エポキシ樹脂、メラミン樹脂が好適に用いられる。特に、上記合成ゴムを用いることが好ましく、その合成ゴムの中でも、先に述べたように、ＥＰＲを単独で用いる、もしくはこのＥＰＲとＢＲを混合した混合物が好ましく用いられる。 In the base material composed of at least one of these synthetic rubber and synthetic resin, each of synthetic rubber and synthetic resin may be used alone, or a combination of synthetic rubber and synthetic resin may be used. You may use it in combination. Of these, synthetic rubber, polyethylene resin, epoxy resin, and melamine resin are preferably used because they are easy to handle when performing mold cleaning. In particular, the synthetic rubber is preferably used, and among the synthetic rubbers, as described above, EPR is used alone or a mixture of EPR and BR is preferably used.
母材として、上記ＥＰＲとＢＲの混合物を用いる場合におけるＥＰＲ（ｘ）とＢＲ（ｙ）の混合割合（ｘ／ｙ）は、重量比で、ｘ／ｙ＝１００／０〜２０／８０の範囲に設定することが好ましい。特に好ましくはｘ／ｙ＝７０／３０〜３０／７０の範囲である。すなわち、両者の混合割合において、ＥＰＲが２０未満（ＥＲが８０以上）では、成形作業時に行なうゴム成形品の除去に際し、成形品の強度が低下するため、破れ等の不都合が生じ易く、金型からの除去作業が困難となる傾向がみられるからである。 When the mixture of EPR and BR is used as a base material, the mixing ratio (x / y) of EPR (x) and BR (y) is in the range of x / y = 100/0 to 20/80 by weight ratio. It is preferable to set to. Particularly preferably, x / y = 70/30 to 30/70. That is, when the EPR is less than 20 (ER is 80 or more) in the mixing ratio of the two, since the strength of the molded product is reduced when the rubber molded product is removed during the molding operation, inconvenience such as tearing is likely to occur. This is because there is a tendency that the removal work from the water becomes difficult.
これら合成ゴムおよび合成樹脂の少なくとも一方からなる母材は、汚れの除去時に金型より取り外す際に硬化状態であることが好ましい。上記硬化状態とするための硬化方法としては、加熱による硬化、熱可塑性樹脂等のような冷却による硬化等があげられ、例えば、加熱により硬化させる場合には、硬化剤が用いられる。 It is preferable that the base material made of at least one of these synthetic rubber and synthetic resin is in a cured state when being removed from the mold when removing the dirt. Examples of the curing method for obtaining the cured state include curing by heating, curing by cooling such as a thermoplastic resin, and the like. For example, when curing by heating, a curing agent is used.
上記硬化剤は、母材を硬化させることが可能であるものであればよく、例えば、合成ゴムやポリエチレン樹脂には有機過酸化物等があげられ、エポキシ樹脂の場合には、フェノール化合物、アミン系化合物、イミダゾール類、酸無水物系硬化剤、有機リン酸化合物等があげられる。 The curing agent only needs to be capable of curing the base material. For example, synthetic rubbers and polyethylene resins include organic peroxides. In the case of epoxy resins, phenolic compounds, amines, etc. Compounds, imidazoles, acid anhydride curing agents, and organic phosphoric acid compounds.
上記有機過酸化物としては、例えば、１，１−ビス（ｔ−ブチルパーオキシ）−３，３，５−トリメチルシクロヘキサン、１，１−ビス（ｔ−ブチルパーオキシ）シクロヘキサン、ｔ−ブチルパーオキシマレイン酸、ｔ−ブチルパーオキシオレート、ｔ−ブチルパーオキシ−３，３，５−トリメチルヘキサノエート、シクロヘキサノンパーオキサイド、ｔ−ブチルパーオキシアリールカーボネート、ｔ−ブチルパーオキシイソプロピルカーボネート、２，５−ジメチル−２，５−ジ（ベンゾイルパーオキシ）ヘキサン、２，２−ビス（ｔ−ブチルパーオキシ）オクタン、ｔ−ブチルパーオキシアセテート、２，２−ビス（ｔ−ブチルパーオキシ）ブタン、ｔ−ブチルパーオキシベンゾエート、ｎ−ブチル−４，４−ビス（ｔ−ブチルパーオキシ）バレレート、ジ−ｔ−ブチルパーオキシイソフタレート、メチルエチルケトンパーオキサイド、ジクミルパーオキサイド、２，５−ジメチル−２，５−ジ（ｔ−ブチルパーオキシ）ヘキサン、α，α′−ビス（ｔ−ブチルパーオキシ−ｍ−イソプロピル）ベンゼン、ｔ−ブチルクミルパーオキサイド、ジイソプロピルベンゼンハイドロパーオキサイド、ジ−ｔ−ブチルパーオキサイド、２，５−ジメチル−２，５−ジ（ｔ−ブチルパーオキシ）ヘキサン−３等の有機過酸化物等があげられる。 Examples of the organic peroxide include 1,1-bis (t-butylperoxy) -3,3,5-trimethylcyclohexane, 1,1-bis (t-butylperoxy) cyclohexane, and t-butylperoxide. Oxymaleic acid, t-butyl peroxyolate, t-butyl peroxy-3,3,5-trimethylhexanoate, cyclohexanone peroxide, t-butyl peroxyaryl carbonate, t-butyl peroxyisopropyl carbonate, 2, 5-dimethyl-2,5-di (benzoylperoxy) hexane, 2,2-bis (t-butylperoxy) octane, t-butylperoxyacetate, 2,2-bis (t-butylperoxy) butane , T-butylperoxybenzoate, n-butyl-4,4-bis (t-butylperoxy ) Valerate, di-t-butylperoxyisophthalate, methyl ethyl ketone peroxide, dicumyl peroxide, 2,5-dimethyl-2,5-di (t-butylperoxy) hexane, α, α'-bis (t -Butylperoxy-m-isopropyl) benzene, t-butylcumyl peroxide, diisopropylbenzene hydroperoxide, di-t-butyl peroxide, 2,5-dimethyl-2,5-di (t-butylperoxy) And organic peroxides such as hexane-3.
上記フェノール化合物としては、例えば、単環二官能フェノールであるヒドロキノン、レゾルシノール、カテコール；多環二官能フェノールであるビスフェノールＡ、ビスフェノールＦ、ナフタレンジオール類、ビフェノール類；およびこれらのハロゲン化物、アルキル基置換体等の多官能フェノール類があげられる。 Examples of the phenol compound include hydroquinone, resorcinol and catechol which are monocyclic bifunctional phenols; bisphenol A, bisphenol F, naphthalenediols and biphenols which are polycyclic bifunctional phenols; and halides and alkyl group substitution thereof. And polyfunctional phenols such as the body.
上記アミン系化合物としては、例えば、Ｎ，Ｎ−ベンジルジメチルアミン、２−（ジメチルアミノメチル）フェノール、２，４，６−トリス（ジメチルアミノメチル）フェノール、テトラメチルグアニジン、トリエタノールアミン、Ｎ，Ｎ′−ジメチルピペラジン、１，４−ジアザビシクロ［２．２．２］オクタン、１，８−ジアザビシクロ［５．４．０］−７−ウンデセン、１，５−ジアザビシクロ［４．４．０］−５−ノネン、ヘキサメチレンテトラミン、ピリジン、ピコリン、ピペリジン、ピロリジン、ジメチルシクロヘキシルアミン、ジメチルヘキシルアミン、シクロヘキシルアミン、ジイソブチルアミン、ジ−ｎ−ブチルアミン、ジフェニルアミン、Ｎ−メチルアニリン、トリ−ｎ−プロピルアミン、トリ−ｎ−オクチルアミン、トリ−ｎ−ブチルアミン、トリフェニルアミン、テトラメチルアンモニウムクロライド、テトラメチルアンモニウムブロマイド、テトラメチルアンモニウムアイオダイド、トリエチレンテトラミン、ジアミノジフェニルメタン、ジアミノジフェニルエーテル、ジシアミンジアミド、トリルビグアニド、グアニル尿素、ジメチル尿素等があげられる。 Examples of the amine compound include N, N-benzyldimethylamine, 2- (dimethylaminomethyl) phenol, 2,4,6-tris (dimethylaminomethyl) phenol, tetramethylguanidine, triethanolamine, N, N'-dimethylpiperazine, 1,4-diazabicyclo [2.2.2] octane, 1,8-diazabicyclo [5.4.0] -7-undecene, 1,5-diazabicyclo [4.4.0]- 5-nonene, hexamethylenetetramine, pyridine, picoline, piperidine, pyrrolidine, dimethylcyclohexylamine, dimethylhexylamine, cyclohexylamine, diisobutylamine, di-n-butylamine, diphenylamine, N-methylaniline, tri-n-propylamine, Tri-n-octylamine, Ri-n-butylamine, triphenylamine, tetramethylammonium chloride, tetramethylammonium bromide, tetramethylammonium iodide, triethylenetetramine, diaminodiphenylmethane, diaminodiphenyl ether, diciaminediamide, tolylbiguanide, guanylurea, dimethylurea, etc. can give.
上記イミダゾール類としては、例えば、イミダゾール、２−エチルイミダゾール、２−エチル−４−メチルイミダゾール、２−メチルイミダゾール、２−フェニルイミダゾール、２−ウンデシルイミダゾール、１−ベンジル−２−メチルイミダゾール、２−ヘプタデシルイミダゾール、４，５−ジフェニルイミダゾール、２−メチルイミダゾリン、２−フェニルイミダゾリン、２−ウンデシルイミダゾリン、２−ヘプタデシルイミダゾリン、２−イソプロピルイミダゾール、２，４−ジメチルイミダゾール、２−フェニル−４−メチルイミダゾール、２−エチルイミダゾリン、２−フェニル−４−メチルイミダゾリン、ベンズイミダゾール、１−シアノエチルイミダゾール、２，４−ジアミノ−６−［２′−メチルイミダゾリル−（１′）］エチル−ｓ−トリアジン等があげられる。 Examples of the imidazoles include imidazole, 2-ethylimidazole, 2-ethyl-4-methylimidazole, 2-methylimidazole, 2-phenylimidazole, 2-undecylimidazole, 1-benzyl-2-methylimidazole, 2 -Heptadecylimidazole, 4,5-diphenylimidazole, 2-methylimidazoline, 2-phenylimidazoline, 2-undecylimidazoline, 2-heptadecylimidazoline, 2-isopropylimidazole, 2,4-dimethylimidazole, 2-phenyl- 4-methylimidazole, 2-ethylimidazoline, 2-phenyl-4-methylimidazoline, benzimidazole, 1-cyanoethylimidazole, 2,4-diamino-6- [2'-methylimidazolyl- (1 ')] Chill -s- triazine, and the like.
上記酸無水物系硬化剤としては、例えば、無水フタル酸、ヘキサヒドロ無水フタル酸、ピロメリット酸二無水物、ベンゾフェノンテトラカルボン酸二無水物等の酸無水物があげられる。 Examples of the acid anhydride curing agent include acid anhydrides such as phthalic anhydride, hexahydrophthalic anhydride, pyromellitic dianhydride, and benzophenone tetracarboxylic dianhydride.
上記有機リン酸化合物としては、例えば、ヘキサメチルリン酸トリアミド、リン酸トリ（ジクロロプロピル）、リン酸トリ（クロロプロピル）、亜リン酸トリフェニル、リン酸トリメチル、フェニルホスホン酸、トリフェニルホスフィン、トリ−ｎ−ブチルホスフィン、ジフェニルホスフィン有機リン化合物およびこれらのハロゲン化物等があげられる。 Examples of the organic phosphate compound include hexamethyl phosphate triamide, tri (dichloropropyl) phosphate, tri (chloropropyl) phosphate, triphenyl phosphite, trimethyl phosphate, phenylphosphonic acid, triphenylphosphine, Examples thereof include tri-n-butylphosphine, diphenylphosphine organophosphorus compounds and halides thereof.
これら硬化剤は単独で使用してもよいし、２種以上任意の組み合わせで用いてもよい。 These curing agents may be used alone or in any combination of two or more.
これら硬化剤の配合量は、適宜に設定されるが、例えば、合成ゴムであれば、合成ゴム１００重量部（以下「部」と略す）に対して１〜３部の範囲に設定することが好ましい。 The blending amount of these curing agents is appropriately set. For example, in the case of synthetic rubber, it may be set within a range of 1 to 3 parts with respect to 100 parts by weight of synthetic rubber (hereinafter abbreviated as “part”). preferable.
さらに、これら硬化剤は、合成ゴムや合成樹脂の熱硬化だけではなく、金型の洗浄剤としての機能を有しており、必要に応じて、硬化剤としての目的以外に本発明の金型洗浄剤組成物に配合することができる。このような場合における硬化剤の配合量は、合成ゴムや合成樹脂の少なくとも一方１００部に対して、５〜６０部に設定することが好ましく、特に好ましくは５〜２５部である。 Furthermore, these curing agents have a function not only as a thermosetting of synthetic rubber and synthetic resin but also as a mold cleaning agent. It can mix | blend with a cleaning composition. In such a case, the compounding amount of the curing agent is preferably set to 5 to 60 parts, particularly preferably 5 to 25 parts with respect to at least one part of synthetic rubber or synthetic resin.
上記母材に配合されるアルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方のうち、上記アルカリ金属塩としては、リチウム、ナトリウム、カリウム、ルビジウム、セシウム等の金属塩があげられる。 Among at least one of the alkali metal salt and alkali metal hydroxide blended in the base material, examples of the alkali metal salt include metal salts such as lithium, sodium, potassium, rubidium, and cesium.
そして、このようなアルカリ金属塩として、例えば、ホウ酸塩、リン酸、メタリン酸、次リン酸、亜リン酸（ホスホン酸）、次亜リン酸（ホスフィン酸）、ピロリン酸、トリメタリン酸、テトラメタリン酸、ピロ亜リン酸等のリン酸塩、炭酸塩、硫酸塩、硝酸塩、塩酸塩、アクリル酸、アジピン酸、アスコルビン酸、アスパラギン酸、アミノ安息香酸、アルギン酸、安息香酸、オレイン酸、ギ酸、クエン酸、グリコール酸、グルコン酸、グルタミン酸、ケイ皮酸、コハク酸、酢酸、サリチル酸、シュウ酸、酒石酸、トルエンスルホン酸、ニコチン酸、乳酸、尿酸、ハロゲン置換酢酸、フタル酸、ベンゼンスルホン酸、マロン酸、酪酸、リンゴ酸等の有機酸塩等があげられる。 Examples of such alkali metal salts include borate, phosphoric acid, metaphosphoric acid, hypophosphoric acid, phosphorous acid (phosphonic acid), hypophosphorous acid (phosphinic acid), pyrophosphoric acid, trimetaphosphoric acid, tetra Phosphate such as metaphosphoric acid, pyrophosphorous acid, carbonate, sulfate, nitrate, hydrochloride, acrylic acid, adipic acid, ascorbic acid, aspartic acid, aminobenzoic acid, alginic acid, benzoic acid, oleic acid, formic acid, Citric acid, glycolic acid, gluconic acid, glutamic acid, cinnamic acid, succinic acid, acetic acid, salicylic acid, oxalic acid, tartaric acid, toluenesulfonic acid, nicotinic acid, lactic acid, uric acid, halogen-substituted acetic acid, phthalic acid, benzenesulfonic acid, malon Examples thereof include organic acid salts such as acid, butyric acid, and malic acid.
これらのアルカリ金属塩は、多価酸の塩の場合、部分的にアルカリ金属の塩となったものも利用可能であり、例えば、三価のリン酸塩の場合、１個の金属と２個の水素を有する第一塩、２個の金属と１個の水素を有する第二塩、３個の金属を有する第三塩のいずれであってもよい。また、酸性塩、アルカリ性塩、中性塩のいずれであってもよい。なかでも、金型の腐食性の観点から、アルカリ性塩、中性塩が好ましい。さらに、これらアルカリ金属塩は、水への溶解性の観点から、水和物を用いることが好ましい。 In the case of a salt of a polyvalent acid, these alkali metal salts can be used in the form of a partial alkali metal salt. For example, in the case of a trivalent phosphate, one metal and two The first salt having two hydrogens, the second salt having two metals and one hydrogen, and the third salt having three metals may be used. Moreover, any of acidic salt, alkaline salt, and neutral salt may be sufficient. Of these, alkaline salts and neutral salts are preferable from the viewpoint of the corrosiveness of the mold. Furthermore, these alkali metal salts are preferably hydrates from the viewpoint of solubility in water.
上記アルカリ金属水酸化物としては、例えば、水酸化ナトリウム、水酸化カリウム等があげられる。 Examples of the alkali metal hydroxide include sodium hydroxide and potassium hydroxide.
これらアルカリ金属塩、アルカリ金属水酸化物は、単独で用いてもよいし、２種以上併せて用いてもよい。 These alkali metal salts and alkali metal hydroxides may be used alone or in combination of two or more.
そして、上記アルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方は、母材となる合成ゴムおよび合成樹脂の少なくとも一方１００部に対して０．１〜１０部の範囲に設定することが好ましく、特に好ましくは０．１〜５部である。すなわち、配合量が少な過ぎると、金型表面に形成された汚染物質の除去性が著しく低下し、金型汚れを完全に除去することが困難となる傾向がみられ、逆に多過ぎると、アルカリ金属塩、アルカリ金属水酸化物が金型表面に析出し易く、逆に金型を汚染してしまう傾向がみられるからである。 And at least one of the alkali metal salt and the alkali metal hydroxide is preferably set in a range of 0.1 to 10 parts with respect to 100 parts of at least one of the synthetic rubber and the synthetic resin as a base material, Preferably it is 0.1-5 parts. That is, when the blending amount is too small, the removability of the contaminants formed on the mold surface is remarkably lowered, and there is a tendency that it is difficult to completely remove the mold dirt. This is because alkali metal salts and alkali metal hydroxides are likely to precipitate on the mold surface, and conversely tend to contaminate the mold.
つぎに、本発明において配合される水としては、水道水、不純物を除去したＲＯ水（逆浸透膜による処理をした水）、イオン交換水等を好適に用いることができる。 Next, tap water, RO water from which impurities have been removed (water treated with a reverse osmosis membrane), ion-exchanged water, or the like can be suitably used as the water blended in the present invention.
上記水の配合量は、母材となる合成ゴムおよび合成樹脂の少なくとも一方１００部に対して３〜３０部の範囲に設定することが好ましく、特に好ましくは５〜２０部である。すなわち、配合量が少な過ぎると、金型表面に形成された汚染物質の除去性が著しく低下し、金型汚れを完全に除去することが困難となる傾向がみられ、逆に多過ぎると、洗浄効果は向上せず、配合する手間も増え無駄となる傾向がみられるからである。 The blending amount of the water is preferably set in the range of 3 to 30 parts, particularly preferably 5 to 20 parts with respect to 100 parts of at least one of the synthetic rubber and the synthetic resin as the base material. That is, when the blending amount is too small, the removability of the contaminants formed on the mold surface is remarkably lowered, and there is a tendency that it is difficult to completely remove the mold dirt. This is because the cleaning effect does not improve, and there is a tendency to increase the amount of time and effort for blending.
本発明の金型洗浄剤組成物には、必須成分である上記各配合成分以外に、必要に応じて、離型剤、補強剤等を適宜に配合することができる。 In the mold cleaning composition of the present invention, a mold release agent, a reinforcing agent, and the like can be appropriately blended as necessary in addition to the above-described blending components that are essential components.
上記離型剤としては、例えば、ステアリン酸、ベヘニン酸等の長鎖脂肪酸、ステアリン酸亜鉛、ステアリン酸カルシウム等に代表される長鎖脂肪酸の金属塩、カルナバワックス、モンタンワックス、モンタン酸の部分ケン化エステル等に代表されるエステル系ワックス、ステアリルエチレンジアミド等に代表される長鎖脂肪酸アミド、ポリエチレンワックス等に代表されるパラフィン類等があげられる。これらは単独でもしくは２種以上併せて用いられる。 Examples of the release agent include long chain fatty acids such as stearic acid and behenic acid, metal salts of long chain fatty acids represented by zinc stearate, calcium stearate, carnauba wax, montan wax, and partial saponification of montanic acid. Examples thereof include ester waxes typified by esters, long chain fatty acid amides typified by stearylethylenediamide, paraffins typified by polyethylene waxes, and the like. These may be used alone or in combination of two or more.
上記離型剤の含有量は、母材となる合成ゴムおよび合成樹脂の少なくとも一方１００部に対して５〜２０部の範囲に設定することが好ましく、特に好ましくは８〜１６部である。すなわち、含有量が少な過ぎると、充分な離型効果を発揮することが困難となり、逆に多過ぎると、洗浄力が低下するとともに再生後の金型を用いて成形品を製造した際にその成形品の外観が悪化する傾向がみられるからである。 The content of the release agent is preferably set in a range of 5 to 20 parts, particularly preferably 8 to 16 parts, relative to 100 parts of at least one of a synthetic rubber and a synthetic resin as a base material. That is, if the content is too small, it will be difficult to exert a sufficient releasing effect, and conversely if too much, the cleaning power will be reduced and when a molded product is produced using a recycled mold, This is because the appearance of the molded product tends to deteriorate.
上記補強剤としては、例えば、シリカ粉末、タルク粉末、アルミナ、炭酸カルシウム、水酸化アルミニウム、酸化チタン等の無機質充填剤があげられる。これらは単独でもしくは２種以上併せて用いられる。上記補強剤としては、平均粒径０．０１〜１００μｍ程度のものを用いることが好ましい Examples of the reinforcing agent include inorganic fillers such as silica powder, talc powder, alumina, calcium carbonate, aluminum hydroxide, and titanium oxide. These may be used alone or in combination of two or more. As the reinforcing agent, one having an average particle size of about 0.01 to 100 μm is preferably used.
上記補強剤の含有量は、母材となる合成ゴムおよび合成樹脂の少なくとも一方１００部に対して１０〜５０部の範囲に設定することが好ましく、特に好ましくは１５〜４０部である。すなわち、含有量が少な過ぎると、補強性が低下することにより機械的強度の低下を招く傾向がみられ、逆に多過ぎると、脆くなってやはり機械的強度が低下する傾向がみられるからである。 The content of the reinforcing agent is preferably set in a range of 10 to 50 parts, particularly preferably 15 to 40 parts, with respect to at least one part of 100 parts of synthetic rubber and synthetic resin as a base material. In other words, if the content is too small, the reinforcing property tends to decrease, leading to a decrease in mechanical strength. On the other hand, if the content is too large, the mechanical strength tends to decrease. is there.
さらに、本発明の金型洗浄剤組成物には、上記以外の添加剤としては、例えば、アロマオイル、ナフテニックオイル等の軟化剤、硫黄等の加硫剤や加硫促進剤、老化防止剤、亜鉛華等を必要に応じて適宜配合することができる。 Furthermore, in the mold cleaning composition of the present invention, as additives other than those described above, for example, softeners such as aroma oil and naphthenic oil, vulcanizing agents such as sulfur, vulcanization accelerators, and antiaging agents In addition, zinc white or the like can be appropriately blended as necessary.
本発明の金型洗浄剤組成物は、例えば、つぎのようにして製造することができる。すなわち、上記各必須成分を含む各配合成分を、バンバリーミキサー、ニーダー、ロールミキサー、押出機等を用いて機械的に混練することにより製造することができる。 The mold cleaning composition of the present invention can be produced, for example, as follows. That is, it can be produced by mechanically kneading each compounding component including the above essential components using a Banbury mixer, a kneader, a roll mixer, an extruder, or the like.
このようにして製造される本発明の金型洗浄剤組成物は、例えば、粉末状、タブレット状、シート状あるいは短冊状に形成された金型洗浄材として金型洗浄に供される。このシート状にして用いる場合のシートの厚みは、通常、３〜１０ｍｍに設定される。 The mold cleaning composition of the present invention produced in this way is used for mold cleaning as a mold cleaning material formed in, for example, powder, tablet, sheet or strip. The thickness of the sheet when used in this sheet form is usually set to 3 to 10 mm.
そして、本発明の金型洗浄剤組成物としては、白色ないしこれに近い灰色のような淡色とすることが好ましい。このように設定することにより、金型洗浄後に、金型から除去されて金型洗浄剤組成物に付着した汚れを目視にて容易に確認することが可能となり、金型洗浄の状況を容易に確認することができるようになるという効果を奏する。 And as a metal mold | die cleaning composition of this invention, it is preferable to set it as light color like white thru | or the gray near this. By setting in this way, after cleaning the mold, it becomes possible to easily visually check the dirt removed from the mold and attached to the mold cleaning composition. There is an effect that it can be confirmed.
本発明の金型洗浄剤組成物から得られる金型洗浄材の使用に際しては、母材が合成ゴムの場合は、一般にシート状に成形して用いることが好ましい。また、母材が合成樹脂の場合は、例えば、熱硬化性メラミン樹脂では、粉末状やタブレット状にして用いることが好ましい。 When using the mold cleaning material obtained from the mold cleaning composition of the present invention, when the base material is a synthetic rubber, it is generally preferable to use it molded into a sheet. When the base material is a synthetic resin, for example, a thermosetting melamine resin is preferably used in the form of powder or tablet.
本発明のシート状に形成された金型洗浄剤組成物を用いての金型のクリーニング方法は、半導体装置成形用金型に装填して行われる。例えば、上記シートは、母材が合成ゴムの場合、当然、未加硫状態であって、これを成形用金型に装填し加熱加硫させることによりシートに汚染物を付着一体化させる。ついで、加硫のなされたシートを金型から取り出すことにより金型の洗浄が行われる。 The mold cleaning method using the mold detergent composition formed in the sheet form of the present invention is carried out by loading the mold for molding a semiconductor device. For example, when the base material is synthetic rubber, the sheet is naturally in an unvulcanized state, and this is loaded into a molding die and heated and vulcanized to attach and integrate contaminants on the sheet. Next, the mold is cleaned by removing the vulcanized sheet from the mold.
母材が合成ゴムの場合となる上記シート状の金型洗浄剤組成物を用いた金型のクリーニング方法を、順を追ってより詳しく説明する。 A mold cleaning method using the above-described sheet-shaped mold cleaning composition, in which the base material is a synthetic rubber, will be described in detail step by step.
まず、本発明の金型洗浄剤組成物からなるシート状の金型洗浄材を準備する。ついで、上記シート状の金型洗浄材（クリーニングシート）を、金型のそれぞれ凹部が形成された上型と下型の間に配置し、その状態から、上型と下型を締めてシート状金型洗浄材を挟み、圧縮成形する。そして、成形時の圧力によって、上記シート状金型洗浄材が、上型に形成された凹部および下型に形成された凹部からなるキャビティ内に充填されるとともに、金型表面に圧接される。その状態で成形時の熱により、合成ゴム（未加硫ゴム）が加熱加硫されて加硫ゴム化し、その際にキャビティ内に形成されている離型剤の酸化劣化層等を加硫ゴムに一体化させる。このとき、場合によってはキャビティ回りに形成されたバリも一体化させる。ついで、所定時間経過後に上型と下型を開き、加硫ゴム化されたシート状金型洗浄材を上下両金型から剥離することにより、上記シート状金型洗浄材と一体化された酸化劣化層等（汚染物）を上下両金型表面から剥離させる。このようにして、金型のクリーニングが行われる。 First, a sheet-shaped mold cleaning material comprising the mold cleaning composition of the present invention is prepared. Next, the above-described sheet-shaped mold cleaning material (cleaning sheet) is placed between the upper mold and the lower mold in which the concave portions of the mold are formed, and from this state, the upper mold and the lower mold are tightened to form a sheet The mold cleaning material is sandwiched and compression molded. And by the pressure at the time of shaping | molding, the said sheet-like metal mold | die cleaning material is filled in the cavity which consists of the recessed part formed in the upper mold | type, and the recessed part formed in the lower mold | type, and is press-contacted to the metal mold | die surface. In this state, synthetic rubber (unvulcanized rubber) is heated and vulcanized by heat during molding to form vulcanized rubber, and the oxidative degradation layer of the release agent formed in the cavity at that time is vulcanized rubber. To be integrated. At this time, a burr formed around the cavity is also integrated in some cases. Next, after the predetermined time has elapsed, the upper mold and the lower mold are opened, and the vulcanized rubber sheet-shaped mold cleaning material is peeled off from both the upper and lower molds, thereby integrating the sheet-shaped mold cleaning material. The deteriorated layer or the like (contaminant) is peeled off from the upper and lower mold surfaces. In this way, the mold is cleaned.
上記シート状金型洗浄材を挟み、圧縮成形し加熱する際の条件としては、母材の種類等により適宜に設定されるが、例えば、合成ゴムの場合、１６０〜１９０℃×１〜５分間の範囲に設定することが好ましく、合成樹脂として熱硬化性樹脂を用いた場合、１６０〜１９０℃×１〜５分間の範囲に設定することが好ましい。 The conditions for sandwiching the sheet-shaped mold cleaning material, compression molding and heating are appropriately set according to the type of the base material and the like. For example, in the case of synthetic rubber, 160 to 190 ° C. × 1 to 5 minutes It is preferable to set in the range of 160 to 190 ° C. × 1 to 5 minutes when a thermosetting resin is used as the synthetic resin.
本発明の金型洗浄剤組成物の使用対象となる金型の一例として、例えば、熱硬化性樹脂組成物を用いて繰り返し成形が行われる半導体装置封止用の成形用金型があげられる。 As an example of the metal mold | die used as the usage object of the metal mold | die cleaning composition of this invention, the metal mold | die for semiconductor device sealing which is repeatedly shape | molded using a thermosetting resin composition is mention | raise | lifted, for example.
本発明の金型洗浄剤組成物の使用対象の一例である半導体装置成形用金型において、封止用樹脂材料として用いられる熱硬化性樹脂組成物としては、例えば、エポキシ樹脂を主剤とするエポキシ樹脂組成物があげられる。 As a thermosetting resin composition used as a sealing resin material in a mold for molding a semiconductor device, which is an example of an object to be used for the mold cleaning composition of the present invention, for example, an epoxy having an epoxy resin as a main component is used. Examples thereof include resin compositions.
そして、熱硬化性樹脂組成物としては、上記主剤となるエポキシ樹脂とともに、通常、硬化剤、さらには必要に応じて、無機質充填剤、硬化促進剤等の添加剤が適宜配合される。 And as a thermosetting resin composition, additives, such as a hardening | curing agent and also an inorganic filler and a hardening accelerator, are suitably mix | blended with the epoxy resin used as the said main ingredient normally as needed.
つぎに、本発明の金型洗浄剤組成物により洗浄された金型は、汚染物が除去され、初期状態の金型表面に戻っているため、通常、成形材料である熱硬化性樹脂組成物を用いた半導体パッケージの成形を行う際に、予め金型表面に離型剤を塗布する。例えば、離型剤としてモンタン酸ワックスを含有してなる成形材料の成形に際しては、同じモンタン酸ワックスを、またカルナバワックスを含有してなる成形材料の成形に際しては、同じカルナバワックスを塗布することが好ましい。そして、金型表面への離型剤の塗布方法としては、離型剤を含有した未加硫ゴム組成物を準備し、これをシート状に形成したものを用いるのが好ましい。例えば、先に述べた未加硫ゴムとともに、離型剤を配合して得られるシートがあげられる。そして、この離型剤を含有した未加硫ゴム組成物からなるシートを上記シート状金型洗浄剤組成物を用いた洗浄工程と同様、金型に装填して加熱することにより含有された離型剤が金型表面に塗布される。これは、加熱加硫の際に未加硫ゴム組成物中の離型剤が溶融し、金型面に滲出して表面に均一な離型剤膜が形成されるものと考えられる。 Next, since the mold cleaned by the mold cleaning composition of the present invention is removed from the contaminants and returned to the initial mold surface, the thermosetting resin composition, which is usually a molding material, is used. When molding a semiconductor package using a mold, a mold release agent is applied to the mold surface in advance. For example, when molding a molding material containing montanic acid wax as a release agent, the same montanic acid wax may be applied, and when molding a molding material containing carnauba wax, the same carnauba wax may be applied. preferable. And as a coating method of the mold release agent to the metal mold | die surface, it is preferable to use the thing which prepared the unvulcanized rubber composition containing the mold release agent, and formed this in the sheet form. For example, the sheet | seat obtained by mix | blending a mold release agent with the unvulcanized rubber mentioned above is mention | raise | lifted. Then, in the same manner as the cleaning step using the sheet-shaped mold cleaning composition, a sheet made of an unvulcanized rubber composition containing the release agent is loaded into a mold and heated to contain the release agent. A mold is applied to the mold surface. It is considered that this is because the release agent in the unvulcanized rubber composition melts during heat vulcanization and exudes to the mold surface to form a uniform release agent film on the surface.
なお、上記離型剤の含有量は、例えば、未加硫ゴム組成物中のゴム材料１００部に対して１５〜３５部の割合に設定することが好ましく、特に好ましくは２０〜３０部である。すなわち、モンタン酸ワックスの含有量が１５部未満では充分な離型効果が発揮されず、逆に３５部を超えると金型表面に過剰塗布されるとともに、洗浄，再生後の金型を用いて成形品を形成した場合にその成形品の外観が劣化する傾向がみられるからである。 In addition, it is preferable to set content of the said mold release agent to the ratio of 15-35 parts with respect to 100 parts of rubber materials in an unvulcanized rubber composition, for example, Most preferably, it is 20-30 parts. . That is, when the content of the montanic acid wax is less than 15 parts, a sufficient releasing effect is not exerted. On the contrary, when the content exceeds 35 parts, it is overcoated on the mold surface, and the mold after cleaning and regeneration is used. This is because when the molded product is formed, the appearance of the molded product tends to deteriorate.
つぎに、実施例について比較例と併せて説明する。ただし、本発明は、これら実施例に限定されるものではない。 Next, examples will be described together with comparative examples. However, the present invention is not limited to these examples.
まず、金型洗浄剤組成物を構成する各成分を準備した。 First, each component which comprises a metal mold | die cleaning composition was prepared.
１）ＢＲ：〔ブタジエンゴム：ＪＳＲ社製、ＢＲ−０１（シス１，４結合：９５％）〕
２）ＥＰＲ：〔エチレン−プロピレン−ジエンゴム：三井化学社製、ＥＰＴ４０４５（エチレン含有量：５４モル％、ジエン成分含有量：８．１モル％）〕
３）タルク粉末：平均粒径９μｍ
４）シリカ粉末：平均粒径９μｍ
５）酸化チタン：平均粒径０．２５μｍ
６）カルナバワックス：カルナバ１号（日興リカ社製）
７）イミダゾール：２，４−ジアミノ−６−［２′−メチルイミダゾリル−（１′）］エチル−ｓ−トリアジン
８）有機過酸化物：ｎ−ブチル−４，４−ビス（ｔ−ブチルパーオキシ）バレレート
９）水：イオン交換水
1) BR: [Butadiene rubber: manufactured by JSR, BR-01 (cis 1,4 bond: 95%)]
2) EPR: [Ethylene-propylene-diene rubber: Mitsui Chemicals, EPT4045 (ethylene content: 54 mol%, diene component content: 8.1 mol%)]
3) Talc powder: average particle size 9μm
4) Silica powder: Average particle size 9 μm
5) Titanium oxide: Average particle size 0.25 μm
6) Carnauba wax: Carnauba No. 1 (manufactured by Nikko Rica)
7) Imidazole: 2,4-diamino-6- [2'-methylimidazolyl- (1 ')] ethyl-s-triazine 8) Organic peroxide: n-butyl-4,4-bis (t-butylper) Oxy) valerate 9) Water: Ion exchange water
〔実施例１〜８、比較例１〜２〕
後記の表１〜表２に示す各成分を同表に示す割合で配合し、これを混練ロールを用いて混練した。ついで、圧延ロールを用いてシート状（厚み５ｍｍ）に成形して目的とするシート状の金型洗浄剤組成物（金型洗浄材）を作製した。
[Examples 1-8, Comparative Examples 1-2]
The components shown in Tables 1 and 2 to be described later were blended in the proportions shown in the same table and kneaded using a kneading roll. Subsequently, it was formed into a sheet shape (thickness 5 mm) using a rolling roll to produce a target sheet-shaped mold cleaning composition (mold cleaning material).
〔実施例９〕
市販の金型クリーニング用熱硬化性メラミン樹脂（日本カーバイト工業社製、ニカレットＥＣＲ−Ｔ）を粉砕したもの１００部に、洗浄剤成分であるＫ3ＰＯ4１部と水４部を噴霧して付着させることにより、粉末状の金型洗浄剤組成物（金型洗浄材）を得た。
Example 9
Spray 100 parts of a commercially available thermosetting melamine resin for mold cleaning (Nicarette ECR-T, manufactured by Nippon Carbide Industries Co., Ltd.) with 1 part of K 3 PO 4 and 4 parts of water. To obtain a powdery mold cleaning composition (mold cleaning material).
〔比較例３〕
市販の金型クリーニング用熱硬化性メラミン樹脂（日本カーバイト工業社製、ニカレットＥＣＲ−Ｔ）のタブレットを用いて、タブレット状の金型洗浄剤組成物（金型洗浄材）とした。
[Comparative Example 3]
A commercially available thermosetting melamine resin for mold cleaning (Nicarette ECR-T, manufactured by Nippon Carbide Industries Co., Ltd.) was used as a tablet-shaped mold cleaning composition (mold cleaning material).
このようにして得られた実施例品および比較例品の各金型洗浄剤組成物（金型洗浄材）を用い、金型に形成された汚染物の除去性をつぎのようにして評価した。すなわち、封止材料である環境対応エポキシ樹脂（日東電工社製、ＧＥ−７４７０）を用いた繰り返し成形を行ない、８００ショット後の、表面が汚染された成形用金型において、上記各金型洗浄剤組成物（金型洗浄材）を用いたクリーニング成形を行なった。そして、クリーニング成形により形成された成形物を金型から取り出し、金型表面における汚染物の除去性を目視にて評価した。この評価において、汚染物を完全に除去することのできた成形作業回数が５回以下であった場合を良、汚染物の除去に６回以上の成形作業を要した場合を不良とした。
Using the mold cleaning compositions (mold cleaning materials) of the example product and the comparative example product thus obtained, the removability of contaminants formed on the mold was evaluated as follows. . That is, repeated molding using an environmentally friendly epoxy resin (manufactured by Nitto Denko Corporation, GE-7470) which is a sealing material, and after each 800 shots, in the molding mold whose surface is contaminated, Cleaning molding was performed using the agent composition (mold cleaning material). Then, the molded product formed by the cleaning molding was taken out from the mold, and the removal of contaminants on the mold surface was visually evaluated. In this evaluation, the case where the number of molding operations in which the contaminants could be completely removed was 5 times or less was judged good, and the case where 6 or more molding operations were required to remove the contaminants was judged as bad.
なお、実施例１〜８品および比較例１〜２品の評価では、シート状の金型洗浄剤組成物（金型洗浄材）を成形用金型に挟み、１７５℃で５分間加熱成形を行なった。一方、実施例９品の評価では、粉末状の金型洗浄剤組成物（金型洗浄材）を用い、比較例３品の評価では、タブレット状の金型洗浄剤組成物（金型洗浄材）を用いてトランスファー成形を行ない、１７５℃で３分間の加熱成形を行なった。 In the evaluation of the products of Examples 1 to 8 and Comparative Examples 1 to 2, the sheet-shaped mold cleaning composition (mold cleaning material) was sandwiched between the molding dies, and heat molding was performed at 175 ° C. for 5 minutes. I did it. On the other hand, in the evaluation of the product of Example 9, a powdery mold cleaning composition (mold cleaning material) was used, and in the evaluation of the product of Comparative Example 3, a tablet-shaped mold cleaning composition (mold cleaning material) was used. ) Was used to carry out transfer molding, followed by heat molding at 175 ° C. for 3 minutes.
上記評価結果を下記の表１〜表２に示す。 The evaluation results are shown in Tables 1 and 2 below.
上記結果から、洗浄剤成分であるアルカリ金属塩およびアルカリ金属水酸化物の少なくとも一方と、水の両方を含有していない比較例品は金型の洗浄性評価が不良であったのに対して、全ての実施例品では金型の洗浄性に関して良の評価が得られた。 From the above results, the comparative example product that does not contain both the alkali metal salt and alkali metal hydroxide, which are the detergent components, and water has a poor mold detergency evaluation. In all of the examples, good evaluation was obtained regarding the cleaning property of the mold.
＜封止材料の変更（１）＞
さらに、封止材料である上記環境対応エポキシ樹脂（日東電工社製、ＧＥ−７４７０）を、同じく日東電工社製の環境対応エポキシ樹脂：ＧＥ−１０３０に代え、上記と同様に繰り返し成形した成形用金型（８００ショット後）に対して、上記と同様の方法にて、実施例１〜９品および比較例１〜３品の各金型洗浄剤組成物（金型洗浄材）を用いた汚染物の除去性を目視にて評価した。その結果、上記と同様、比較例品は金型の洗浄性評価が不良であったのに対して、全ての実施例品では金型の洗浄性に関して良の評価が得られた。
<Change of sealing material (1)>
Further, the above-mentioned environmentally friendly epoxy resin (manufactured by Nitto Denko Corporation, GE-7470), which is a sealing material, is replaced with an environmentally friendly epoxy resin: GE-1030, also produced by Nitto Denko Corporation. Contamination using mold cleaning compositions (mold cleaning materials) of Examples 1 to 9 and Comparative Examples 1 to 3 for the mold (after 800 shots) in the same manner as above. The removable property was visually evaluated. As a result, in the same manner as described above, the comparative example product had a poor mold cleaning property evaluation, whereas all of the example products had good evaluations regarding the mold cleaning property.
＜封止材料の変更（２）＞
また、封止材料である上記環境対応エポキシ樹脂（日東電工社製、ＧＥ−７４７０）を、同じく日東電工社製の環境対応エポキシ樹脂：ＧＥ−１００に代え、上記と同様に繰り返し成形した成形用金型（８００ショット後）に対して、上記と同様の方法にて、実施例１〜９品および比較例１〜３品の各金型洗浄剤組成物（金型洗浄材）を用いた汚染物の除去性を目視にて評価した。その結果、上記と同様、比較例品は金型の洗浄性評価が不良であったのに対して、全ての実施例品では金型の洗浄性に関して良の評価が得られた。
<Change of sealing material (2)>
Further, the above-mentioned environmentally friendly epoxy resin (manufactured by Nitto Denko Corporation, GE-7470), which is a sealing material, is replaced with Nitto Denko Corporation's environmentally friendly epoxy resin: GE-100, and is molded repeatedly in the same manner as described above. Contamination using mold cleaning compositions (mold cleaning materials) of Examples 1 to 9 and Comparative Examples 1 to 3 for the mold (after 800 shots) in the same manner as above. The removable property was visually evaluated. As a result, in the same manner as described above, the comparative example product had a poor mold cleaning property evaluation, whereas all of the example products had good evaluations regarding the mold cleaning property.
本発明の金型洗浄剤組成物は、熱硬化性樹脂成形材料用等の各種成形金型、例えば、エポキシ樹脂成形材料を用いて、半導体素子を射出成形またはトランスファー成形によって繰り返し樹脂封止して成形する際に用いる成形用金型の洗浄再生等に用いられる。 The mold cleaning composition of the present invention is obtained by repeatedly sealing a semiconductor element by injection molding or transfer molding using various molding dies for a thermosetting resin molding material, for example, an epoxy resin molding material. Used for cleaning and regeneration of a molding die used for molding.
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| JP2009169330A JP6116789B2 (en) | 2009-07-17 | 2009-07-17 | Semiconductor device molding die cleaning sheet and semiconductor device molding die cleaning method using the same |
| SG201005167-0A SG168489A1 (en) | 2009-07-17 | 2010-07-16 | Mold cleaning composition and mold cleaning material, and method for cleaning mold using the same |
| TW099123559A TWI499668B (en) | 2009-07-17 | 2010-07-16 | Mold cleaning composition and mold cleaning material, and method for cleaning mold using the same |
| KR1020100069108A KR101788859B1 (en) | 2009-07-17 | 2010-07-16 | Mold cleaner composition and mold cleaning material, and method of cleaning using the same |
| CN201010233007XA CN101955858B (en) | 2009-07-17 | 2010-07-16 | Mold cleaner composition and mold cleaning material, and method of cleaning using the same |
| MYPI2010003374A MY177272A (en) | 2009-07-17 | 2010-07-16 | Mold cleaner composition and mold cleaning material, and mold cleaning method using the same |
| KR1020170096473A KR20170091558A (en) | 2009-07-17 | 2017-07-28 | Mold cleaner composition and mold cleaning material, and method of cleaning using the same |
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