JP5702912B2 - Double-sided adhesive tape for fixing adhesive and abrasive cloth - Google Patents
Double-sided adhesive tape for fixing adhesive and abrasive cloth Download PDFInfo
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- JP5702912B2 JP5702912B2 JP2009052312A JP2009052312A JP5702912B2 JP 5702912 B2 JP5702912 B2 JP 5702912B2 JP 2009052312 A JP2009052312 A JP 2009052312A JP 2009052312 A JP2009052312 A JP 2009052312A JP 5702912 B2 JP5702912 B2 JP 5702912B2
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- 239000004744 fabric Substances 0.000 title claims description 131
- 239000000853 adhesive Substances 0.000 title claims description 65
- 230000001070 adhesive effect Effects 0.000 title claims description 65
- 239000002390 adhesive tape Substances 0.000 title description 17
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 196
- 239000010410 layer Substances 0.000 claims description 60
- 239000000178 monomer Substances 0.000 claims description 54
- 229920003067 (meth)acrylic acid ester copolymer Polymers 0.000 claims description 47
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 46
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 40
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 27
- 239000000203 mixture Substances 0.000 claims description 27
- -1 2-ethylhexyl Chemical group 0.000 claims description 26
- 239000003431 cross linking reagent Substances 0.000 claims description 20
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 claims description 20
- 125000003368 amide group Chemical group 0.000 claims description 16
- 125000003277 amino group Chemical group 0.000 claims description 16
- 239000002253 acid Substances 0.000 claims description 15
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 239000000758 substrate Substances 0.000 claims description 12
- 230000009477 glass transition Effects 0.000 claims description 10
- 239000012948 isocyanate Substances 0.000 claims description 8
- 150000002513 isocyanates Chemical class 0.000 claims description 8
- 238000005259 measurement Methods 0.000 claims description 6
- 238000005227 gel permeation chromatography Methods 0.000 claims description 5
- 229920001577 copolymer Polymers 0.000 claims description 4
- 239000004793 Polystyrene Substances 0.000 claims description 3
- 229920002223 polystyrene Polymers 0.000 claims description 3
- WDQMWEYDKDCEHT-UHFFFAOYSA-N 2-ethylhexyl 2-methylprop-2-enoate Chemical compound CCCCC(CC)COC(=O)C(C)=C WDQMWEYDKDCEHT-UHFFFAOYSA-N 0.000 claims 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 238000005498 polishing Methods 0.000 description 129
- 229940048053 acrylate Drugs 0.000 description 35
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 33
- 239000002585 base Substances 0.000 description 31
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 30
- 229920000139 polyethylene terephthalate Polymers 0.000 description 24
- 239000005020 polyethylene terephthalate Substances 0.000 description 24
- 229940114077 acrylic acid Drugs 0.000 description 23
- 239000012790 adhesive layer Substances 0.000 description 23
- 239000000243 solution Substances 0.000 description 23
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 239000003513 alkali Substances 0.000 description 14
- 239000007864 aqueous solution Substances 0.000 description 14
- 239000000463 material Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 238000007654 immersion Methods 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000011347 resin Substances 0.000 description 10
- 239000011521 glass Substances 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 238000001035 drying Methods 0.000 description 7
- 239000003505 polymerization initiator Substances 0.000 description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 5
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 5
- 229920001971 elastomer Polymers 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
- 239000006260 foam Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229920002799 BoPET Polymers 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 4
- 238000013329 compounding Methods 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000011800 void material Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 3
- 238000010528 free radical solution polymerization reaction Methods 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- 239000008096 xylene Substances 0.000 description 3
- FYRCDEARNUVZRG-UHFFFAOYSA-N 1,1,5-trimethyl-3,3-bis(2-methylpentan-2-ylperoxy)cyclohexane Chemical compound CCCC(C)(C)OOC1(OOC(C)(C)CCC)CC(C)CC(C)(C)C1 FYRCDEARNUVZRG-UHFFFAOYSA-N 0.000 description 2
- UAJRSHJHFRVGMG-UHFFFAOYSA-N 1-ethenyl-4-methoxybenzene Chemical compound COC1=CC=C(C=C)C=C1 UAJRSHJHFRVGMG-UHFFFAOYSA-N 0.000 description 2
- RTEZVHMDMFEURJ-UHFFFAOYSA-N 2-methylpentan-2-yl 2,2-dimethylpropaneperoxoate Chemical compound CCCC(C)(C)OOC(=O)C(C)(C)C RTEZVHMDMFEURJ-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- YIVJZNGAASQVEM-UHFFFAOYSA-N Lauroyl peroxide Chemical compound CCCCCCCCCCCC(=O)OOC(=O)CCCCCCCCCCC YIVJZNGAASQVEM-UHFFFAOYSA-N 0.000 description 2
- 229920000459 Nitrile rubber Polymers 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 239000002985 plastic film Substances 0.000 description 2
- 229920006255 plastic film Polymers 0.000 description 2
- 229920001225 polyester resin Polymers 0.000 description 2
- 239000004645 polyester resin Substances 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229920003002 synthetic resin Polymers 0.000 description 2
- 239000000057 synthetic resin Substances 0.000 description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 2
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 description 2
- 239000003643 water by type Substances 0.000 description 2
- FVQMJJQUGGVLEP-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOOC(C)(C)C FVQMJJQUGGVLEP-UHFFFAOYSA-N 0.000 description 1
- HCXVPNKIBYLBIT-UHFFFAOYSA-N (2-methylpropan-2-yl)oxy 3,5,5-trimethylhexaneperoxoate Chemical compound CC(C)(C)CC(C)CC(=O)OOOC(C)(C)C HCXVPNKIBYLBIT-UHFFFAOYSA-N 0.000 description 1
- AYMDJPGTQFHDSA-UHFFFAOYSA-N 1-(2-ethenoxyethoxy)-2-ethoxyethane Chemical compound CCOCCOCCOC=C AYMDJPGTQFHDSA-UHFFFAOYSA-N 0.000 description 1
- JZHGRUMIRATHIU-UHFFFAOYSA-N 1-ethenyl-3-methylbenzene Chemical compound CC1=CC=CC(C=C)=C1 JZHGRUMIRATHIU-UHFFFAOYSA-N 0.000 description 1
- STMDPCBYJCIZOD-UHFFFAOYSA-N 2-(2,4-dinitroanilino)-4-methylpentanoic acid Chemical compound CC(C)CC(C(O)=O)NC1=CC=C([N+]([O-])=O)C=C1[N+]([O-])=O STMDPCBYJCIZOD-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- JKNCOURZONDCGV-UHFFFAOYSA-N 2-(dimethylamino)ethyl 2-methylprop-2-enoate Chemical compound CN(C)CCOC(=O)C(C)=C JKNCOURZONDCGV-UHFFFAOYSA-N 0.000 description 1
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
- XKBHBVFIWWDGQX-UHFFFAOYSA-N 2-bromo-3,3,4,4,5,5,5-heptafluoropent-1-ene Chemical compound FC(F)(F)C(F)(F)C(F)(F)C(Br)=C XKBHBVFIWWDGQX-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
- JLBJTVDPSNHSKJ-UHFFFAOYSA-N 4-Methylstyrene Chemical compound CC1=CC=C(C=C)C=C1 JLBJTVDPSNHSKJ-UHFFFAOYSA-N 0.000 description 1
- NFWPZNNZUCPLAX-UHFFFAOYSA-N 4-methoxy-3-methylaniline Chemical compound COC1=CC=C(N)C=C1C NFWPZNNZUCPLAX-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 description 1
- GAWIXWVDTYZWAW-UHFFFAOYSA-N C[CH]O Chemical group C[CH]O GAWIXWVDTYZWAW-UHFFFAOYSA-N 0.000 description 1
- 241000694440 Colpidium aqueous Species 0.000 description 1
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- JUIBLDFFVYKUAC-UHFFFAOYSA-N [5-(2-ethylhexanoylperoxy)-2,5-dimethylhexan-2-yl] 2-ethylhexaneperoxoate Chemical compound CCCCC(CC)C(=O)OOC(C)(C)CCC(C)(C)OOC(=O)C(CC)CCCC JUIBLDFFVYKUAC-UHFFFAOYSA-N 0.000 description 1
- MZVQCMJNVPIDEA-UHFFFAOYSA-N [CH2]CN(CC)CC Chemical group [CH2]CN(CC)CC MZVQCMJNVPIDEA-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 239000011260 aqueous acid Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 238000005537 brownian motion Methods 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000013522 chelant Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000007720 emulsion polymerization reaction Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 229920003145 methacrylic acid copolymer Polymers 0.000 description 1
- 238000004377 microelectronic Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920005749 polyurethane resin Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 238000007348 radical reaction Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- OPQYOFWUFGEMRZ-UHFFFAOYSA-N tert-butyl 2,2-dimethylpropaneperoxoate Chemical compound CC(C)(C)OOC(=O)C(C)(C)C OPQYOFWUFGEMRZ-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
Images
Description
本発明は、酸及びアルカリへの耐性に優れ、研磨中に剥がれを生ずることなく、かつ、糊残りをほとんど生じさせずに剥離できる粘着剤に関する。また、本発明は、該粘着剤を用いてなる研磨布固定用両面粘着テープに関する。 The present invention relates to a pressure-sensitive adhesive that has excellent resistance to acids and alkalis and can be peeled off without causing peeling during polishing and hardly causing adhesive residue. The present invention also relates to a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth using the pressure-sensitive adhesive.
半導体ウエハを所定の厚さにまで研磨する工程においては、研磨機の定盤に固定された研磨布を用いて研磨が行われる。研磨布を研磨機の定盤に固定するためには、通常、両面テープが使用される。この研磨布固定用両面粘着テープには、研磨中に研磨布が剥離しない程度に充分な接着力を有するとともに、使用した研磨布を交換する際には定盤から糊残りなく剥離できることが求められてきた。 In the step of polishing the semiconductor wafer to a predetermined thickness, polishing is performed using a polishing cloth fixed to a surface plate of a polishing machine. In order to fix the polishing cloth to the surface plate of the polishing machine, a double-sided tape is usually used. This double-sided pressure-sensitive adhesive tape for fixing a polishing cloth is required to have sufficient adhesive strength so that the polishing cloth does not peel off during polishing, and when the used polishing cloth is replaced, it can be peeled off without any adhesive residue from the surface plate. I came.
特許文献１には、プラスチックフィルムの一方の面にニトリルゴム系粘着剤からなる粘着剤層を設け、他方の面に再剥離性の粘着剤層を設けてなる研磨布固定用両面粘着テープが開示されている。特許文献１に開示されている研磨布固定用両面粘着テープは、ニトリルゴム系粘着剤からなる粘着剤層側を研磨布に接着し、再剥離性の粘着剤層側を定盤に接着して使用する。特許文献１の実施例では、再剥離性の粘着剤層を構成する粘着剤として、アクリル酸と、アクリル酸ブチルと、酢酸ビニルとを共重合させてなる共重合体を使用している。特許文献１に開示されている研磨布固定用両面粘着テープは、両面をアクリル粘着剤とした場合に比べて、酸化セリウム微粉末の２０％溶液に５０℃で５日間浸漬した後も高い粘着力を維持できる。 Patent Document 1 discloses a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth in which a pressure-sensitive adhesive layer made of a nitrile rubber-based pressure-sensitive adhesive is provided on one surface of a plastic film and a removable pressure-sensitive adhesive layer is provided on the other surface. Has been. The double-sided pressure-sensitive adhesive tape for fixing a polishing cloth disclosed in Patent Document 1 has a pressure-sensitive adhesive layer side made of a nitrile rubber-based pressure-sensitive adhesive bonded to the polishing cloth and a removable pressure-sensitive adhesive layer side bonded to a surface plate. use. In the Example of patent document 1, the copolymer formed by copolymerizing acrylic acid, butyl acrylate, and vinyl acetate is used as an adhesive which comprises a releasable adhesive layer. The double-sided pressure-sensitive adhesive tape for fixing a polishing cloth disclosed in Patent Document 1 has higher adhesive strength after being immersed in a 20% solution of fine cerium oxide powder at 50 ° C. for 5 days than when both sides are made of an acrylic pressure-sensitive adhesive. Can be maintained.
特許文献２には、プラスチックフィルム支持体の一方の面にアクリル系ポリマーを主成分とする粘着剤層と該粘着剤層上にポリエステル又はポリウレタンからなる熱活性粘着剤層が積層一体化された層を設け、他方の面に再剥離性の粘着剤層を設けてなる研磨布固定用両面粘着テープが開示されている。特許文献２に開示されている研磨布固定用両面粘着テープは、熱活性粘着剤層を研磨材に接着させて使用する。特許文献２に開示されている研磨布固定用両面粘着テープは、両面ともアクリル粘着剤層を用いた場合と比べて、水酸化カリウムでｐＨ１０に調整した５０℃の水溶液に５日間浸漬した場合にも、高い粘着力を維持できる。
しかしながら、近年、半導体ウエハ等を研磨する際に強酸性又は強アルカリ性のスラリー液を使用するため、特許文献１及び２に開示されている研磨布固定用両面粘着テープでは、定盤側の粘着剤層が酸やアルカリの影響で劣化しやすく、研磨中に剥離してしまうことがあるという問題があった。また、仮に特許文献１及び２に記載されている研磨布固定側の粘着剤層を定盤側にも使用した場合には、酸やアルカリに対する耐性は優れるが、使用した研磨布を交換する際に定盤から容易に剥離することができなかった。
However, in recent years, since a strongly acidic or strongly alkaline slurry is used when polishing a semiconductor wafer or the like, the double-sided pressure-sensitive adhesive tape for fixing a polishing cloth disclosed in
耐アルカリ性に優れた粘着剤として、例えば、特許文献３には、スチレンと、環式構造を有する（メタ）アクリル酸エステルと、鎖式構造からなる（メタ）アクリル酸アルキルエステルと、エチレン性二重結合を有するカルボン酸とを共重合したポリマーを主成分とする粘着剤が開示されている。特許文献３に開示されている粘着剤は、２．３８質量％のＴＭＡＨ水溶液に浸漬させても溶解しない。しかしながら、特許文献３に開示されている耐アルカリ性に優れた粘着剤を研磨布固定用両面粘着テープの定盤固定用粘着剤層に使用した場合には、使用した研磨布を交換する際に接着層を溶解し取り除くための剥離液が必要となり、容易に再剥離することができなかった。 As pressure-sensitive adhesives having excellent alkali resistance, for example, Patent Document 3 discloses styrene, (meth) acrylic acid ester having a cyclic structure, (meth) acrylic acid alkyl ester having a chain structure, A pressure-sensitive adhesive mainly comprising a polymer copolymerized with a carboxylic acid having a heavy bond is disclosed. The pressure-sensitive adhesive disclosed in Patent Document 3 does not dissolve even when immersed in a 2.38% by mass TMAH aqueous solution. However, when the adhesive excellent in alkali resistance disclosed in Patent Document 3 is used for the pressure-sensitive adhesive layer for fixing the surface plate of the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth, it adheres when the used polishing cloth is replaced. A stripping solution was required to dissolve and remove the layer, and could not be easily stripped again.
本発明は、酸及びアルカリへの耐性に優れ、研磨中に剥がれを生ずることなく、かつ、糊残りをほとんど生じさせずに剥離できる粘着剤を提供することを目的とする。また、本発明は、該粘着剤を用いてなる研磨布固定用両面粘着テープを提供することを目的とする。 An object of the present invention is to provide a pressure-sensitive adhesive that has excellent resistance to acids and alkalis and can be peeled off without causing peeling during polishing and hardly causing adhesive residue. Another object of the present invention is to provide a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth using the pressure-sensitive adhesive.
本発明は、（メタ）アクリル酸エステル共重合体と、架橋剤とを含有する粘着剤であって、動的粘弾性測定により得られるガラス転移温度（Ｔｇ）が−１０〜２０℃の範囲にあり、上記（メタ）アクリル酸エステル共重合体は、（メタ）アクリル酸ｔ−ブチルと、（メタ）アクリル酸２−エチルヘキシルと、アクリル酸とを含有するモノマー混合物を共重合させてなる共重合体である粘着剤である。
以下に本発明を詳述する。
The present invention is a pressure-sensitive adhesive containing a (meth) acrylic acid ester copolymer and a crosslinking agent, and has a glass transition temperature (Tg) obtained by dynamic viscoelasticity measurement in the range of −10 to 20 ° C. The (meth) acrylic acid ester copolymer is a copolymer obtained by copolymerizing a monomer mixture containing t-butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, and acrylic acid. It is an adhesive that is a coalescence.
The present invention is described in detail below.
研磨布固定用両面粘着テープに用いる粘着剤には、凝集力に優れ、かつ、薬液による分解が起こりにくい粘着剤を用いる必要がある。
本発明者らは、凝集力を向上させる成分としてのアクリル酸と、重量増加率を抑制する成分としての特定の（メタ）アクリル酸エステルとを共重合させて得られる（メタ）アクリル酸エステル共重合体を用いることにより、酸及びアルカリへの耐性に優れるために研磨中に剥がれを生ずることなく、かつ、糊残りをほとんど生じさせずに剥離できる粘着剤が得られることを見出し、本発明を完成させるに至った。
The pressure-sensitive adhesive used for the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth needs to be a pressure-sensitive adhesive that is excellent in cohesive force and hardly decomposes by a chemical solution.
The present inventors have prepared a copolymer of (meth) acrylic acid ester obtained by copolymerizing acrylic acid as a component that improves cohesion and a specific (meth) acrylic acid ester as a component that suppresses the rate of increase in weight. By using a polymer, it has been found that a pressure-sensitive adhesive that can be peeled off without causing peeling during polishing due to excellent resistance to acid and alkali and hardly causing adhesive residue is obtained. It came to complete.
本発明の粘着剤は、（メタ）アクリル酸エステル共重合体を含有する。
上記（メタ）アクリル酸エステル共重合体は、モノマー混合物を共重合させてなる。
上記モノマー混合物は（メタ）アクリル酸ｔ−ブチルを含有する。
上記モノマー混合物が上記（メタ）アクリル酸ｔ−ブチルを含有することにより、本発明の粘着剤は酸スラリー及びアルカリスラリーを用いた際でも加水分解がほとんど進行せず、かつ凝集力に優れる。
The pressure-sensitive adhesive of the present invention contains a (meth) acrylic acid ester copolymer.
The (meth) acrylic acid ester copolymer is obtained by copolymerizing a monomer mixture.
The monomer mixture contains t-butyl (meth) acrylate.
When the monomer mixture contains the t-butyl (meth) acrylate, the pressure-sensitive adhesive of the present invention hardly undergoes hydrolysis even when an acid slurry or an alkali slurry is used, and is excellent in cohesive force.
上記（メタ）アクリル酸ｔ−ブチルの含有量は特に限定されないが、上記モノマー混合物１００重量部に対して、好ましい下限は５重量部、好ましい上限は５０重量部である。上記（メタ）アクリル酸ｔ−ブチルの含有量が５重量部未満であると、得られる粘着剤を研磨布固定用両面粘着テープに用いた場合、凝集力が弱く研磨中にずれ等を引き起こすことがある。上記（メタ）アクリル酸ｔ−ブチルの含有量が５０重量部を超えると、得られる粘着剤を研磨布固定用両面粘着テープに用いた場合、接着力が弱くなり研磨中に剥がれを引き起こすことがある。上記（メタ）アクリル酸ｔ−ブチルの含有量は、上記モノマー混合物１００重量部に対して、より好ましい下限は１０重量部、より好ましい上限は３０重量部である。 Although content of the said (meth) acrylic-acid t-butyl is not specifically limited, A preferable minimum is 5 weight part and a preferable upper limit is 50 weight part with respect to 100 weight part of said monomer mixtures. When the content of the t-butyl (meth) acrylate is less than 5 parts by weight, when the obtained pressure-sensitive adhesive is used for a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth, the cohesive force is weak and causes slippage during polishing. There is. When the content of t-butyl (meth) acrylate is more than 50 parts by weight, when the obtained pressure-sensitive adhesive is used for a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth, the adhesive strength is weakened, which may cause peeling during polishing. is there. The content of the t-butyl (meth) acrylate is more preferably 10 parts by weight and more preferably 30 parts by weight with respect to 100 parts by weight of the monomer mixture.
上記モノマー混合物は（メタ）アクリル酸２−エチルヘキシルを含有する。
上記モノマー混合物が、上記（メタ）アクリル酸２−エチルヘキシルを含有することにより、得られる（メタ）アクリル酸エステル共重合体の疎水性が高くなり、酸性水溶液やアルカリ性水溶液の粘着剤中への浸透が抑制され、加水分解の影響を受けにくくなるため、本発明の粘着剤は耐酸性及び耐アルカリ性に優れる。また、上記（メタ）アクリル酸２−エチルヘキシルを用いることにより、得られる（メタ）アクリル酸エステル共重合体のガラス転移温度（Ｔｇ）が低くなり、本発明の粘着剤は、流動性及び密着性に優れる。
The monomer mixture contains 2-ethylhexyl (meth) acrylate.
When the monomer mixture contains 2-ethylhexyl (meth) acrylate, the resulting (meth) acrylic acid ester copolymer becomes highly hydrophobic, and an aqueous acid solution or an aqueous alkaline solution penetrates into the adhesive. The pressure-sensitive adhesive of the present invention is excellent in acid resistance and alkali resistance. Moreover, the glass transition temperature (Tg) of the (meth) acrylic acid ester copolymer obtained becomes low by using the said (meth) acrylic-acid 2-ethylhexyl, and the adhesive of this invention has fluidity | liquidity and adhesiveness. Excellent.
上記（メタ）アクリル酸２−エチルヘキシルの含有量は特に限定されないが、上記モノマー混合物１００重量部に対して、好ましい下限は４２重量部、好ましい上限は８９重量部である。上記（メタ）アクリル酸２−エチルヘキシルの含有量が４２重量部未満であると、得られる粘着剤の粘着性が低くなり、研磨布固定用両面粘着テープに用いた場合、研磨時に研磨布が剥がれることがある。上記（メタ）アクリル酸２−エチルヘキシルの含有量が８９重量部を超えると、得られる粘着剤の凝集性が低くなり、研磨布固定用両面粘着テープに用いた場合、研磨時に粘着剤に加わるせん断力に耐えられずに研磨布が剥がれたり、使用した研磨布を交換するために再剥離する際に凝集破壊して糊残りが生じたりすることがある。上記（メタ）アクリル酸２−エチルヘキシルの含有量は、上記モノマー混合物１００重量部に対して、より好ましい下限は５０重量部、より好ましい上限は８０重量部である。 Although content of the said (meth) acrylic-acid 2-ethylhexyl is not specifically limited, A preferable minimum is 42 weight part with respect to 100 weight part of said monomer mixtures, A preferable upper limit is 89 weight part. When the content of 2-ethylhexyl (meth) acrylate is less than 42 parts by weight, the pressure-sensitive adhesive obtained has low adhesiveness, and when used for a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth, the polishing cloth peels off during polishing. Sometimes. When the content of 2-ethylhexyl (meth) acrylate exceeds 89 parts by weight, the cohesiveness of the resulting pressure-sensitive adhesive is reduced, and when used for a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth, shear applied to the pressure-sensitive adhesive during polishing. In some cases, the polishing cloth may not be able to withstand the force, and the polishing cloth may be peeled off, or when the used polishing cloth is re-separated to replace the polishing cloth, cohesive failure may occur and adhesive residue may be generated. The content of the 2-ethylhexyl (meth) acrylate is more preferably 50 parts by weight and more preferably 80 parts by weight with respect to 100 parts by weight of the monomer mixture.
上記モノマー混合物はアクリル酸を含有する。
上記モノマー混合物が、上記アクリル酸を含有することにより、本発明の粘着剤は凝集性に優れ、かつ、高い界面接着力を有する。そのため、本発明の粘着剤を研磨布固定用両面粘着テープに用いた場合、再剥離する際の糊残りの発生を防止することができ、かつ、研磨時に回転方向のモーメントとして接着面に対して加わる力による粘着剤層又は接着界面でのボイドの発生を抑制し、ボイドに酸又はアルカリスラリー液が浸透し、接着面積が低下することによる研磨布の剥離を効果的に防止することができる。
The monomer mixture contains acrylic acid.
When the monomer mixture contains the acrylic acid, the pressure-sensitive adhesive of the present invention has excellent cohesiveness and high interfacial adhesion. Therefore, when the pressure-sensitive adhesive of the present invention is used for a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth, it is possible to prevent the occurrence of adhesive residue when re-peeling, and to the adhesive surface as a moment in the rotational direction during polishing. Generation | occurrence | production of the void in the adhesive layer or the adhesion interface by the applied force can be suppressed, and peeling of the polishing cloth due to the acid or alkali slurry liquid penetrating into the void and reducing the adhesion area can be effectively prevented.
上記アクリル酸の含有量は特に限定されないが、上記（メタ）アクリル酸ｔ−ブチルと上記（メタ）アクリル酸２−エチルヘキシルとの合計１００重量部に対して、好ましい下限は５重量部、好ましい上限は１０重量部である。上記アクリル酸の含有量が５重量部未満であると、粘着剤の凝集性や定盤に対する界面粘着力が低くなり、研磨布固定用両面粘着テープに用いた場合、使用した研磨布を交換するために再剥離する際に凝集破壊して糊残りが生じたり、研磨時に研磨布が剥がれたりすることがある。上記アクリル酸の含有量が１０重量部を超えると、粘着剤のタックが低下し初期接着性が悪くなり、研磨時に研磨布が剥がれることがある。上記アクリル酸の含有量は、上記（メタ）アクリル酸ｔ−ブチルと上記（メタ）アクリル酸２−エチルヘキシルとの合計１００重量部に対して、より好ましい下限は６重量部、より好ましい上限は８重量部である。 Although content of the said acrylic acid is not specifically limited, A preferable minimum is 5 weight part and a preferable upper limit with respect to a total of 100 weight part of the said (meth) acrylic-acid t-butyl and the said (meth) acrylic-acid 2-ethylhexyl. Is 10 parts by weight. When the acrylic acid content is less than 5 parts by weight, the cohesiveness of the adhesive and the interfacial adhesive force to the surface plate are reduced, and when used for a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth, the used polishing cloth is replaced. For this reason, cohesive failure may occur when re-peeling, and adhesive residue may be generated, or the polishing cloth may be peeled off during polishing. When the content of the acrylic acid exceeds 10 parts by weight, the tackiness of the pressure-sensitive adhesive is lowered, initial adhesiveness is deteriorated, and the polishing cloth may be peeled off during polishing. The content of the acrylic acid is more preferably a lower limit of 6 parts by weight and a more preferable upper limit of 8 with respect to a total of 100 parts by weight of the t-butyl (meth) acrylate and the 2-ethylhexyl (meth) acrylate. Parts by weight.
上記モノマー混合物は、アミノ基及び／又はアミド基を有するモノマーを含有することが好ましい。
上記モノマー混合物が、上記アミノ基及び／又はアミド基を有するモノマーを含有することにより、本発明の粘着剤は高い凝集性を有する。これは、上記アクリル酸と上記アミノ基及び／又はアミド基を有するモノマーとが、イオン結合又は水素結合を形成することによって擬似的に架橋しているためであると推定される。そのため、発明の粘着剤を研磨布固定用両面粘着テープに用いた場合、再剥離する際の糊残りの発生を防止することができ、かつ、研磨時に回転方向のモーメントとして接着面に対して加わる力による粘着剤層又は接着界面でのボイドの発生を抑制し、ボイドに酸又はアルカリスラリー液が浸透して接着面積が低下することによる研磨布の剥離を効果的に防止することができる。
The monomer mixture preferably contains a monomer having an amino group and / or an amide group.
When the monomer mixture contains a monomer having the amino group and / or amide group, the pressure-sensitive adhesive of the present invention has high cohesiveness. This is presumably because the acrylic acid and the monomer having the amino group and / or amide group are pseudo-crosslinked by forming an ionic bond or a hydrogen bond. Therefore, when the pressure-sensitive adhesive of the invention is used for the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth, it is possible to prevent the occurrence of adhesive residue when re-peeling and to apply to the adhesive surface as a moment in the rotational direction during polishing. Generation | occurrence | production of the void in the adhesive layer or adhesion | attachment interface by force can be suppressed, and peeling of the polishing cloth by an acid or alkali slurry liquid osmose | permeating a void and a bonding area falling can be prevented effectively.
上記アミノ基及び／又はアミド基を有するモノマーは特に限定されず、例えば、アクリルアミド、メタクリルアミド、（メタ）アクリル酸アミノエチル、（メタ）アクリル酸ジメチルアミノエチル、（メタ）アクリル酸ジエチルアミノエチル等が挙げられる。これらのアミノ基及び／又はアミド基を有するモノマーは単独で用いてもよいし、２種以上を併用してもよい。なかでも、加水分解を受けにくく、また、上記（メタ）アクリル酸ｔ−ブチル、上記（メタ）アクリル酸２−エチルヘキシル及び／又は上記アクリル酸と共重合しやすいことから、アクリルアミドが好適である。 The monomer having the amino group and / or amide group is not particularly limited, and examples thereof include acrylamide, methacrylamide, aminoethyl (meth) acrylate, dimethylaminoethyl (meth) acrylate, diethylaminoethyl (meth) acrylate, and the like. Can be mentioned. These monomers having an amino group and / or an amide group may be used alone or in combination of two or more. Among them, acrylamide is preferable because it is difficult to undergo hydrolysis and is easily copolymerized with the t-butyl (meth) acrylate, the 2-ethylhexyl (meth) acrylate and / or the acrylic acid.
上記アミノ基及び／又はアミド基を有するモノマーの含有量は特に限定されないが、上記（メタ）アクリル酸ｔ−ブチルと上記（メタ）アクリル酸２−エチルヘキシルとの合計１００重量部に対して、好ましい下限は０．１重量部、好ましい上限は２重量部である。上記アミノ基及び／又はアミド基を有するモノマーの含有量が０．１重量部未満であると、粘着剤の凝集性が低くなり、研磨布固定用両面粘着テープに用いた場合、使用した研磨布を交換するために再剥離する際に凝集破壊して糊残りが生じたり、研磨時に研磨布が剥がれたりすることがある。上記アミノ基及び／又はアミド基を有するモノマーの含有量が２重量部を超えると、粘着剤のタックが低下して初期接着性が悪くなり、研磨布が剥がれることがある。また、上記アミノ基及び／又はアミド基を有するモノマーの含有量が２重量部を超えると、得られる（メタ）アクリル酸エステル共重合体の吸水性が高くなるため、共重合体内部へ酸性水溶液やアルカリ性水溶液が浸透しやすくなることがある。浸透した酸やアルカリは、触媒として作用して（メタ）アクリル酸エステル共重合体のエステル部位の加水分解反応を引き起こし、（メタ）アクリル酸エステル共重合体の化学劣化が発生することがある。
上記アミノ基及び／又はアミド基を有するモノマーの含有量は、上記（メタ）アクリル酸ｔ−ブチルと上記（メタ）アクリル酸２−エチルヘキシルとの合計１００重量部に対して、より好ましい下限は０．２重量部、より好ましい上限は１．５重量部である。
Although content of the monomer which has the said amino group and / or amide group is not specifically limited, It is preferable with respect to a total of 100 weight part of said (meth) acrylate t-butyl and said (meth) acrylate 2-ethylhexyl. The lower limit is 0.1 parts by weight, and the preferred upper limit is 2 parts by weight. When the content of the monomer having an amino group and / or amide group is less than 0.1 parts by weight, the cohesiveness of the pressure-sensitive adhesive is lowered, and when used for a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth, the used polishing cloth When re-peeling to replace the adhesive, there may be a cohesive failure resulting in adhesive residue, or the polishing cloth may be peeled off during polishing. When the content of the monomer having an amino group and / or amide group exceeds 2 parts by weight, tackiness of the pressure-sensitive adhesive is lowered, initial adhesiveness is deteriorated, and the polishing cloth may be peeled off. In addition, when the content of the monomer having an amino group and / or amide group exceeds 2 parts by weight, the resulting (meth) acrylic acid ester copolymer has high water absorption, so that an acidic aqueous solution is introduced into the copolymer. Or an alkaline aqueous solution may easily penetrate. The permeated acid or alkali acts as a catalyst to cause a hydrolysis reaction of the ester site of the (meth) acrylic acid ester copolymer, and chemical deterioration of the (meth) acrylic acid ester copolymer may occur.
The content of the monomer having an amino group and / or amide group is more preferably 0 with respect to a total of 100 parts by weight of the t-butyl (meth) acrylate and the 2-ethylhexyl (meth) acrylate. .2 parts by weight, and a more preferred upper limit is 1.5 parts by weight.
上記モノマー混合物は、上記（メタ）アクリル酸ｔ−ブチル、上記（メタ）アクリル酸２−エチルヘキシル、又は、アクリル酸と共重合可能な他のモノマーを含有してもよい。更に、上記アミノ基及び／又はアミド基を有するモノマーを含有する場合には、上記モノマー混合物は、上記（メタ）アクリル酸ｔ−ブチル、上記（メタ）アクリル酸２−エチルヘキシル、上記アクリル酸、或いは、上記アミノ基及び／又はアミド基を有するモノマーと共重合可能な他のモノマーを含有してもよい。なお、本明細書中、このようなモノマーを、単に「他のモノマー」ともいう。
上記他のモノマーを含有することにより、本発明の粘着剤の凝集力を高めることや、濡れ性を増大させることができる。
The monomer mixture may contain the t-butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, or other monomer copolymerizable with acrylic acid. Furthermore, when the monomer having the amino group and / or the amide group is contained, the monomer mixture is composed of t-butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, acrylic acid, or In addition, other monomers copolymerizable with the monomer having the amino group and / or amide group may be contained. In the present specification, such a monomer is also simply referred to as “other monomer”.
By containing the other monomer, the cohesive force of the pressure-sensitive adhesive of the present invention can be increased and wettability can be increased.
上記他のモノマーは特に限定されず、例えば、（メタ）アクリル酸２−ヒドロキシエチル、（メタ）アクリル酸グリシジル、アリルグリシジルエーテル、酢酸ビニル、スチレン、α−メチルスチレン、ｍ−メチルスチレン、ｐ−メチルスチレン、ビニルトルエン、ｐ−メトキシスチレン、塩化ビニル、塩化ビニリデン、酢酸ビニル等が挙げられる。 The other monomers are not particularly limited. For example, 2-hydroxyethyl (meth) acrylate, glycidyl (meth) acrylate, allyl glycidyl ether, vinyl acetate, styrene, α-methylstyrene, m-methylstyrene, p- Examples include methyl styrene, vinyl toluene, p-methoxy styrene, vinyl chloride, vinylidene chloride, and vinyl acetate.
上記他のモノマーの含有量は特に限定されないが、上記（メタ）アクリル酸ｔ−ブチルと上記（メタ）アクリル酸２−エチルヘキシルとの合計１００重量部に対して、好ましい上限は１０重量部である。上記他のモノマーの含有量が１０重量部を超えると、得られる粘着剤の粘着性が低くなり、研磨布固定用両面粘着テープに用いた場合、研磨時に研磨布が剥がれることがある。上記他のモノマーの含有量は、上記（メタ）アクリル酸ｔ−ブチルと上記（メタ）アクリル酸２−エチルヘキシルとの合計１００重量部に対して、より好ましい上限は８重量部である。 The content of the other monomer is not particularly limited, but a preferable upper limit is 10 parts by weight with respect to a total of 100 parts by weight of the t-butyl (meth) acrylate and 2-ethylhexyl (meth) acrylate. . When the content of the other monomer exceeds 10 parts by weight, the pressure-sensitive adhesive obtained has low adhesiveness, and when used for a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth, the polishing cloth may be peeled off during polishing. The content of the other monomer is more preferably 8 parts by weight with respect to 100 parts by weight in total of the t-butyl (meth) acrylate and the 2-ethylhexyl (meth) acrylate.
上記（メタ）アクリル酸エステル共重合体を製造する方法は特に限定されず、例えば、上記（メタ）アクリル酸ｔ−ブチル、上記（メタ）アクリル酸２−エチルヘキシル、及び、上記アクリル酸と、必要に応じて、上記アミノ基及び／又はアミド基を有するモノマーと、他のモノマーとを含有するモノマー混合物を、重合開始剤の存在下にてラジカル反応させる重合方法等が挙げられる。
上記重合方法は特に限定されず、例えば、溶液重合、乳化重合、懸濁重合、塊状重合等の従来公知の重合方法を用いることができる。
The method for producing the (meth) acrylic acid ester copolymer is not particularly limited. For example, the t-butyl (meth) acrylate, the 2-ethylhexyl (meth) acrylate, and the acrylic acid are necessary. Depending on the above, there may be mentioned a polymerization method in which a monomer mixture containing the monomer having the amino group and / or amide group and another monomer is subjected to a radical reaction in the presence of a polymerization initiator.
The said polymerization method is not specifically limited, For example, conventionally well-known polymerization methods, such as solution polymerization, emulsion polymerization, suspension polymerization, and block polymerization, can be used.
上記溶液重合に用いる溶媒は特に限定されず、例えば、酢酸エチル、トルエン、ジメチルスルホキシド、エタノール、アセトン、ジエチルエーテル等が挙げられる。 The solvent used for the solution polymerization is not particularly limited, and examples thereof include ethyl acetate, toluene, dimethyl sulfoxide, ethanol, acetone, diethyl ether and the like.
上記溶液重合に用いる溶媒の配合量は特に限定されないが、上記モノマー混合物１００重量部に対して、好ましい下限は２５重量部、好ましい上限は３００重量部である。上記溶媒の配合量が２５重量部未満であると、得られるポリマーの分子量分布が広くなり、得られる粘着剤の粘着性や凝集性が低くなり、研磨布固定用両面粘着テープに用いた場合、研磨時に粘着剤に加わるせん断力に耐えられずに研磨布が剥がれたり、使用した研磨布を交換するために再剥離する際に凝集破壊して糊残りが生じたりすることがある。上記溶媒の配合量が３００重量部を超えると、研磨布固定用両面粘着テープを作成する際に粘着層厚みを均一にすることが困難になったり、溶剤を除去する手間が必要となったりすることがある。 Although the compounding quantity of the solvent used for the said solution polymerization is not specifically limited, A preferable minimum is 25 weight part and a preferable upper limit is 300 weight part with respect to 100 weight part of said monomer mixtures. When the blending amount of the solvent is less than 25 parts by weight, the molecular weight distribution of the obtained polymer is broadened, the adhesiveness and cohesiveness of the resulting adhesive is reduced, and when used for a double-sided adhesive tape for fixing an abrasive cloth, The polishing cloth may not be able to withstand the shearing force applied to the pressure-sensitive adhesive during polishing, and the adhesive residue may be generated due to cohesive failure when re-peeling to replace the used polishing cloth. If the amount of the solvent exceeds 300 parts by weight, it may be difficult to make the thickness of the adhesive layer uniform when preparing a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth, or it may be necessary to remove the solvent. Sometimes.
上記重合開始剤は特に限定されず、例えば、１，１−ビス（ｔ−ヘキシルパーオキシ）−３，３，５−トリメチルシクロヘキサン、ｔ−ヘキシルパーオキシピバレート、ｔ−ブチルパーオキシピバレート、ラウロイルパーオキシド、２，５−ジメチル−２，５−ビス（２−エチルヘキサノイルパーオキシ）ヘキサン、ｔ−ヘキシルパーオキシ−２−エチルヘキサノエート、ｔ−ブチルパーオキシ−２−エチルヘキサノエート、ｔ−ブチルパーオキシイソブチレート、ｔ−ブチルパーオキシ−３，５，５−トリメチルヘキサノエート、ｔ−ブチルパーオキシラウレート等が挙げられる。これらの重合開始剤は単独で用いてもよく、２種以上を併用してもよい。なかでも、１，１−ビス（ｔ−ヘキシルパーオキシ）−３，３，５−トリメチルシクロヘキサン、ｔ−ヘキシルパーオキシピバレートが好適である。 The polymerization initiator is not particularly limited. For example, 1,1-bis (t-hexylperoxy) -3,3,5-trimethylcyclohexane, t-hexylperoxypivalate, t-butylperoxypivalate, Lauroyl peroxide, 2,5-dimethyl-2,5-bis (2-ethylhexanoylperoxy) hexane, t-hexylperoxy-2-ethylhexanoate, t-butylperoxy-2-ethylhexanoate And t-butyl peroxyisobutyrate, t-butyl peroxy-3,5,5-trimethylhexanoate, t-butyl peroxylaurate and the like. These polymerization initiators may be used alone or in combination of two or more. Of these, 1,1-bis (t-hexylperoxy) -3,3,5-trimethylcyclohexane and t-hexylperoxypivalate are preferable.
上記重合開始剤の配合量は特に限定されないが、上記モノマー混合物１００重量部に対して、好ましい下限は０．０５重量部、好ましい上限は０．５重量部である。上記重合開始剤の配合量が０．０５重量部未満であると、重合反応が不充分となったり、重合反応に長時間を要したりすることがある。上記重合開始剤の配合量が０．５重量部を超えると、得られる（メタ）アクリル酸エステル共重合体の重量平均分子量が低くなりすぎたり、分子量分布が広くなりすぎたりすることがあり、その結果、研磨布固定用両面粘着テープに用いた場合、研磨時に粘着剤に加わるせん断力に耐えられずに研磨布が剥がれたり、使用した研磨布を交換するために再剥離する際に凝集破壊して糊残りが生じたりすることがある。 Although the compounding quantity of the said polymerization initiator is not specifically limited, A preferable minimum is 0.05 weight part and a preferable upper limit is 0.5 weight part with respect to 100 weight part of said monomer mixtures. When the blending amount of the polymerization initiator is less than 0.05 parts by weight, the polymerization reaction may be insufficient, or the polymerization reaction may take a long time. If the amount of the polymerization initiator exceeds 0.5 parts by weight, the weight average molecular weight of the resulting (meth) acrylic acid ester copolymer may be too low, or the molecular weight distribution may be too wide. As a result, when used for double-sided pressure-sensitive adhesive tape for fixing abrasive cloth, the abrasive cloth peels off without being able to withstand the shearing force applied to the adhesive during polishing, or cohesive failure occurs when re-peeling to replace the used abrasive cloth As a result, adhesive residue may occur.
上記（メタ）アクリル酸エステル共重合体の重量平均分子量は特に限定されないが、好ましい下限は２０万、好ましい上限は１００万である。上記（メタ）アクリル酸エステル共重合体の重量平均分子量が２０万未満であると、得られる粘着剤の凝集性が低くなり、使用した研磨布を交換するために再剥離する際に凝集破壊して糊残りが生じることがある。上記（メタ）アクリル酸エステル共重合体の重量平均分子量が１００万を超えると、得られる粘着剤の接着力やタックが低下し、得られる粘着剤を研磨布固定用両面粘着テープに用いた場合、研磨時に研磨布が剥がれることがある。
なお、本明細書において上記重量平均分子量は、ゲルパーミエーションクロマトグラフィー（ＧＰＣ）法により、ポリスチレン換算して測定した値を意味する。具体的には、例えば、上記（メタ）アクリル酸エステル共重合体をテトラヒドロフラン（ＴＨＦ）により１００倍に希釈して得られた希釈液をフィルターで濾過し、得られた濾液をカラム（例えば、Ｗａｔｅｒｓ社製の商品名「２６９０ Ｓｅｐａｒａｔｉｏｎｓ Ｍｏｄｅｌ」等）を用いてＧＰＣ法により測定することができる。
Although the weight average molecular weight of the said (meth) acrylic acid ester copolymer is not specifically limited, A preferable minimum is 200,000 and a preferable upper limit is 1 million. When the weight average molecular weight of the (meth) acrylic acid ester copolymer is less than 200,000, the cohesiveness of the resulting pressure-sensitive adhesive is lowered, and cohesive failure occurs when re-peeling to replace the used polishing cloth. Adhesive residue may occur. When the weight average molecular weight of the (meth) acrylic acid ester copolymer exceeds 1,000,000, the adhesive strength and tack of the resulting pressure-sensitive adhesive are reduced, and the resulting pressure-sensitive adhesive is used for a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth. The polishing cloth may be peeled off during polishing.
In addition, in this specification, the said weight average molecular weight means the value measured in polystyrene conversion by the gel permeation chromatography (GPC) method. Specifically, for example, a diluted solution obtained by diluting the (meth) acrylic acid ester copolymer with tetrahydrofuran (THF) 100 times is filtered through a filter, and the obtained filtrate is filtered with a column (for example, Waters It can be measured by the GPC method using a trade name “2690 Separations Model” manufactured by the company.
本発明の粘着剤は、架橋剤を含有する。
上記架橋剤を含有することにより、上記（メタ）アクリル酸エステル共重合体に架橋構造を形成することができる。また、上記架橋剤の種類や量を適宜調整することによって、本発明の粘着剤のゲル分率を調整することが容易になる。
The pressure-sensitive adhesive of the present invention contains a crosslinking agent.
By containing the crosslinking agent, a crosslinked structure can be formed in the (meth) acrylic acid ester copolymer. Moreover, it becomes easy to adjust the gel fraction of the adhesive of this invention by adjusting suitably the kind and quantity of the said crosslinking agent.
上記架橋剤は特に限定されず、例えば、イソシアネート系架橋剤、アジリジン系架橋剤、エポキシ系架橋剤、金属キレート型架橋剤等が挙げられる。なかでも、耐熱性及び耐久性等の性能を発現しやすいことから、イソシアネート系架橋剤が好適である。 The said crosslinking agent is not specifically limited, For example, an isocyanate type crosslinking agent, an aziridine type crosslinking agent, an epoxy-type crosslinking agent, a metal chelate type crosslinking agent etc. are mentioned. Among these, an isocyanate-based crosslinking agent is preferable because it easily exhibits performance such as heat resistance and durability.
上記架橋剤の配合量は特に限定されないが、上記（メタ）アクリル酸エステル共重合体１００重量部に対して、好ましい下限は０．１重量部、好ましい上限は４．０重量部である。上記架橋剤の配合量が０．１重量部未満であると、上記（メタ）アクリル酸エステル共重合体の架橋が不充分となり、得られる粘着剤を研磨布固定用両面粘着テープに用いた場合、使用した研磨布を交換するために再剥離する際に凝集破壊して糊残りが生じることがある。上記架橋剤の配合量が２．０重量部を超えると、得られる粘着剤の粘着力やタックが低下することがある。上記架橋剤の配合量は、上記（メタ）アクリル酸エステル共重合体１００重量部に対して、より好ましい下限は０．３重量部、より好ましい上限は２．５重量部である。 Although the compounding quantity of the said crosslinking agent is not specifically limited, A preferable minimum is 0.1 weight part and a preferable upper limit is 4.0 weight part with respect to 100 weight part of the said (meth) acrylic acid ester copolymers. When the amount of the crosslinking agent is less than 0.1 parts by weight, the (meth) acrylic acid ester copolymer is insufficiently crosslinked, and the resulting adhesive is used for a double-sided adhesive tape for fixing an abrasive cloth. When re-peeling to replace the used polishing cloth, cohesive failure may occur and adhesive residue may be generated. If the amount of the crosslinking agent exceeds 2.0 parts by weight, the adhesive strength and tack of the resulting adhesive may be reduced. The blending amount of the crosslinking agent is more preferably 0.3 parts by weight and more preferably 2.5 parts by weight with respect to 100 parts by weight of the (meth) acrylic acid ester copolymer.
本発明の粘着剤は、更に、粘着付与樹脂を含有してもよい。
上記粘着付与樹脂は特に限定されず、例えば、キシレン樹脂、フェノール樹脂、ロジン系樹脂、テルペン系樹脂等が挙げられる。これらの粘着付与樹脂は、単独で用いてもよいし、２種以上を併用してもよい。なかでも、キシレン樹脂が好適であり、キシレン樹脂のアルキルフェノール反応物がより好適である。
The pressure-sensitive adhesive of the present invention may further contain a tackifier resin.
The tackifying resin is not particularly limited, and examples thereof include a xylene resin, a phenol resin, a rosin resin, and a terpene resin. These tackifier resins may be used alone or in combination of two or more. Among these, a xylene resin is preferable, and an alkylphenol reaction product of the xylene resin is more preferable.
本発明の粘着剤は、更に、必要に応じて着色剤、充てん剤、老化防止剤等の従来公知の添加剤を含有してもよい。 The pressure-sensitive adhesive of the present invention may further contain conventionally known additives such as a colorant, a filler and an anti-aging agent as necessary.
本発明の粘着剤のガラス転移温度の下限は−１０℃、上限は２０℃である。上記ガラス転移温度が−１０℃未満であると、凝集力が低すぎ、研磨布固定用両面粘着テープに用いた場合、テープが定盤からずれて剥がれることがある。上記ガラス転移温度が２０℃を超えると、凝集力が高くなりすぎて粘着力が不充分となることがある。
なお、本明細書においてガラス転移温度とは、動的粘弾性測定により得られる損失正接（ｔａｎδ）の極大のうち、ミクロブラウン運動に起因する極大が現れる温度を意味する。上記ガラス転移温度は、粘弾性スペクトロメーター等を用いた従来公知の方法により測定することができる。
The lower limit of the glass transition temperature of the pressure-sensitive adhesive of the present invention is −10 ° C., and the upper limit is 20 ° C. When the glass transition temperature is less than −10 ° C., the cohesive force is too low, and when used for a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth, the tape may be displaced from the surface plate and peeled off. When the glass transition temperature exceeds 20 ° C., the cohesive force becomes too high, and the adhesive strength may be insufficient.
In the present specification, the glass transition temperature means a temperature at which a maximum due to micro-Brownian motion appears among the maximum of loss tangent (tan δ) obtained by dynamic viscoelasticity measurement. The glass transition temperature can be measured by a conventionally known method using a viscoelastic spectrometer or the like.
本発明の粘着剤を含有する粘着剤層を、基材の少なくとも一方の面に積層一体化してなる研磨布固定用両面粘着テープもまた、本発明の１つである。
本発明の研磨布固定用両面粘着テープは、基材フィルム支持体の少なくとも一方の面に本発明の粘着剤を含有する粘着剤層が積層一体化されて設けられる。上記粘着剤層が研磨機定盤との貼り合わせ面となることにより、使用後に定盤から剥離しやすく、また、研磨布の位置調整が容易になる。また、上記粘着剤層は酸およびアルカリスラリー液の浸透性が低いため、酸性又はアルカリ性条件での研磨において粘着力の低下が起こりにくい。
A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth, in which the pressure-sensitive adhesive layer containing the pressure-sensitive adhesive of the present invention is laminated and integrated on at least one surface of the substrate, is also one aspect of the present invention.
The double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth of the present invention is provided by laminating and integrating a pressure-sensitive adhesive layer containing the pressure-sensitive adhesive of the present invention on at least one surface of a substrate film support. When the pressure-sensitive adhesive layer becomes a bonding surface with the polishing machine surface plate, it is easy to peel off from the surface plate after use, and the position of the polishing cloth can be easily adjusted. Moreover, since the said adhesive layer has the low permeability | transmittance of an acid and an alkali slurry liquid, the fall of adhesive force does not occur easily in grinding | polishing on acidic or alkaline conditions.
上記基材は特に限定されず、例えば、ポリエステル系樹脂、ポリプロピレン系樹脂等からなる合成樹脂フィルムや、ポリウレタン系樹脂、ポリプロピレン系樹脂等のポリオレフィン系樹脂等からなる発泡シート等が挙げられる。なかでも、平坦であり、厚みのぶれが小さく、一定の強度を有することから、ポリエステル系樹脂からなる合成樹脂フィルムが好適である。 The said base material is not specifically limited, For example, the synthetic resin film which consists of polyester resin, a polypropylene resin, etc., the foamed sheet etc. which consist of polyolefin resin, such as a polyurethane resin and a polypropylene resin, etc. are mentioned. Among them, a synthetic resin film made of a polyester resin is preferable because it is flat, has little thickness fluctuation, and has a certain strength.
上記基材の厚みは特に限定されないが、非発泡体である場合には、好ましい下限は１５μｍ、好ましい上限は３００μｍである。上記非発泡体である基材の厚みが１５μｍ未満であると、得られる研磨布固定用両面粘着テープを研磨機の定盤から剥離させる際に基材が破断して綺麗に剥離させることができないことがある。上記非発泡体である基材の厚みが３００μｍを超えると、研磨布と得られる研磨布固定用両面粘着テープとを圧着させる際の圧力の調整が困難となり、研磨布と得られる研磨布固定用両面粘着テープとの接着強度が低下することがある。上記非発泡体である基材の厚みのより好ましい下限は２０μｍ、より好ましい上限は２００μｍである。 The thickness of the substrate is not particularly limited, but when it is a non-foamed material, the preferred lower limit is 15 μm and the preferred upper limit is 300 μm. When the thickness of the non-foam base material is less than 15 μm, the base material breaks when the resulting double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth is peeled off from the surface plate of the polishing machine, and cannot be peeled cleanly. Sometimes. When the thickness of the non-foamed substrate exceeds 300 μm, it is difficult to adjust the pressure when the abrasive cloth and the resulting double-sided adhesive tape for fixing the abrasive cloth are pressure-bonded, and for fixing the abrasive cloth and the obtained abrasive cloth. The adhesive strength with the double-sided pressure-sensitive adhesive tape may decrease. The minimum with more preferable thickness of the base material which is the said non-foaming body is 20 micrometers, and a more preferable upper limit is 200 micrometers.
上記基材が発泡体である場合には、上記基材の厚みの好ましい下限は５０μｍ、好ましい上限は３０００μｍである。上記発泡体である基材の厚みが５０μｍ未満であると、得られる研磨布固定用両面粘着テープを研磨機の定盤から剥離させる際に基材が破断して綺麗に剥離させることができないことがある。上記発泡体である基材の厚みが３０００μｍを超えると、研磨の際の圧力により基材が押し込まれるように変形し、研磨物の研磨精度が低下することがある。上記発泡体である基材の厚みのより好ましい下限は１００μｍ、より好ましい上限は２０００μｍである。 When the said base material is a foam, the preferable minimum of the thickness of the said base material is 50 micrometers, and a preferable upper limit is 3000 micrometers. When the thickness of the base material that is the foam is less than 50 μm, the base material breaks when the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth obtained is peeled off from the surface plate of the polishing machine, and cannot be peeled cleanly. There is. When the thickness of the base material which is the foam exceeds 3000 μm, the base material is deformed so as to be pushed in by the pressure during polishing, and the polishing accuracy of the polished article may be lowered. The minimum with more preferable thickness of the base material which is the said foam is 100 micrometers, and a more preferable upper limit is 2000 micrometers.
上記粘着剤層を構成する粘着剤中における上記（メタ）アクリル酸エステル系共重合体の含有量は特に限定されないが、好ましい下限は７０重量％である。上記（メタ）アクリル酸エステル系共重合体の含有量が７０重量％未満であると、接着力が低くなり研磨時に研磨布が剥がれることがある。 The content of the (meth) acrylic acid ester copolymer in the pressure-sensitive adhesive constituting the pressure-sensitive adhesive layer is not particularly limited, but a preferred lower limit is 70% by weight. When the content of the (meth) acrylic acid ester copolymer is less than 70% by weight, the adhesive strength is lowered and the polishing cloth may be peeled off during polishing.
上記粘着剤層の厚みは特に限定されないが、好ましい下限は２０μｍ、好ましい上限は１００μｍである。上記粘着剤層の厚みが２０μｍ未満であると、粘着力が不充分となり、研磨中に研磨布が剥がれることがある。上記粘着剤層の厚みが１００μｍを超えると、保持力が低くなり、研磨中に研磨布が剥がれることがある。上記粘着剤層の厚みのより好ましい下限は２５μｍ、より好ましい上限は８０μｍであり、更に好ましい下限は３０μｍ、更に好ましい上限は６０μｍである。 Although the thickness of the said adhesive layer is not specifically limited, A preferable minimum is 20 micrometers and a preferable upper limit is 100 micrometers. When the thickness of the pressure-sensitive adhesive layer is less than 20 μm, the adhesive strength becomes insufficient, and the polishing cloth may be peeled off during polishing. When the thickness of the pressure-sensitive adhesive layer exceeds 100 μm, the holding power becomes low, and the polishing cloth may be peeled off during polishing. The more preferable lower limit of the thickness of the pressure-sensitive adhesive layer is 25 μm, the more preferable upper limit is 80 μm, the still more preferable lower limit is 30 μm, and the still more preferable upper limit is 60 μm.
上記粘着剤層のゲル分率は特に限定されないが、好ましい下限は３０重量％、好ましい上限は８０重量％である。上記ゲル分率が３０重量％未満であると、上記（メタ）アクリル酸エステル系共重合体の架橋が不充分であり、研磨中に研磨布が剥がれたり、使用した研磨布を交換するために再剥離する際に凝集破壊して糊残りが生じたりすることがある。上記ゲル分率が８０重量％を超えると、ゾル分の分子量が下がり粘着剤の粘着力が低下し、研磨中に研磨布が剥がれることがある。上記ゲル分率のより好ましい下限は４５重量％、より好ましい上限は７５重量％である。 Although the gel fraction of the said adhesive layer is not specifically limited, A preferable minimum is 30 weight% and a preferable upper limit is 80 weight%. When the gel fraction is less than 30% by weight, the (meth) acrylic acid ester copolymer is not sufficiently crosslinked, and the polishing cloth is peeled off during polishing or the used polishing cloth is replaced. When re-peeling, adhesive breakage may occur due to cohesive failure. When the gel fraction exceeds 80% by weight, the molecular weight of the sol decreases and the adhesive strength of the adhesive decreases, and the polishing cloth may peel off during polishing. A more preferable lower limit of the gel fraction is 45% by weight, and a more preferable upper limit is 75% by weight.
なお、上記ゲル分率は、下記の方法により測定することができる。
まず、本発明の研磨布固定用両面粘着テープを５０ｍｍ×２５ｍｍの平面長方形状に切断して試験片を作製する。得られた試験片を酢酸エチル中に２３℃にて２４時間浸漬した後、２００メッシュのステンレスメッシュを介して試験片を酢酸エチルから取り出して、１１０℃の条件下で１時間乾燥させる。そして、乾燥後の試験片の重量を測定し、下記式（１）を用いてゲル分率を算出する。なお、試験片に用いた研磨布固定用両面粘着テープには、後述する離型フィルム及び剥離紙は積層されていない。
ゲル分率（重量％）＝１００×（Ｗ２−Ｗ０）／（Ｗ１−Ｗ０） （１）
式（１）中、Ｗ０は基材の重量を表し、Ｗ１は浸漬前の試験片の重量を表し、Ｗ２は浸漬し乾燥した後の試験片の重量を表す。
The gel fraction can be measured by the following method.
First, the double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth of the present invention is cut into a flat rectangular shape of 50 mm × 25 mm to produce a test piece. After immersing the obtained test piece in ethyl acetate at 23 ° C. for 24 hours, the test piece is taken out from ethyl acetate through a 200-mesh stainless steel mesh and dried at 110 ° C. for 1 hour. And the weight of the test piece after drying is measured, and a gel fraction is computed using following formula (1). In addition, the release film and release paper which are mentioned later are not laminated | stacked on the double-sided adhesive tape for polishing cloth fixation used for the test piece.
Gel fraction (% by weight) = 100 × (W 2 −W 0 ) / (W 1 −W 0 ) (1)
In formula (1), W 0 represents the weight of the substrate, W 1 represents the weight of the test piece before immersion, and W 2 represents the weight of the test piece after immersion and drying.
本発明の研磨布固定用両面粘着テープの製造方法は特に限定されず、例えば、以下の方法が挙げられる。 The manufacturing method of the double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth of the present invention is not particularly limited, and examples thereof include the following methods.
まず、本発明の粘着剤に溶剤を加えて粘着剤溶液を調製し、得られた粘着剤溶液を基材の表面に塗布し、粘着剤溶液中の溶剤を完全に乾燥除去して粘着剤層を形成する。次に、形成した粘着剤層の上に離型フィルムを、離型処理面が粘着剤層に対向した状態になるように重ね合わせる。 First, a solvent is added to the pressure-sensitive adhesive of the present invention to prepare a pressure-sensitive adhesive solution, and the resulting pressure-sensitive adhesive solution is applied to the surface of the substrate, and the solvent in the pressure-sensitive adhesive solution is completely removed by drying. Form. Next, the release film is overlaid on the formed pressure-sensitive adhesive layer so that the release treatment surface faces the pressure-sensitive adhesive layer.
上記溶剤は特に限定されず、例えば、酢酸エチル、アセトン、シクロヘキサン、ジエチルエーテル、エタノール、ジメチルスルホキシド等が挙げられる。 The solvent is not particularly limited, and examples thereof include ethyl acetate, acetone, cyclohexane, diethyl ether, ethanol, dimethyl sulfoxide and the like.
次いで、新たに用意した離型フィルムの離型処理面に粘着剤溶液（本発明の粘着剤でもよいし、本発明の粘着剤と異なる粘着剤でもよい）を塗布し、粘着剤溶液中の溶剤を完全に乾燥除去することにより、離型フィルムの表面に粘着剤層が形成された積層フィルムを作製する。 Next, a pressure-sensitive adhesive solution (the pressure-sensitive adhesive of the present invention or a pressure-sensitive adhesive different from the pressure-sensitive adhesive of the present invention) may be applied to the release treatment surface of the newly prepared release film, and the solvent in the pressure-sensitive adhesive solution Is completely removed by drying to produce a laminated film in which a pressure-sensitive adhesive layer is formed on the surface of the release film.
基材における粘着剤層を形成した側と反対側の面に対して、得られた積層フィルムの粘着剤層が対向した状態になるように重ね合わせて積層体を作製する。
得られた積層体を、ゴムローラ等を用いて加圧することで、基材の両面に粘着剤層が積層一体化され、かつ、粘着剤層の表面に離型フィルムが剥離可能に積層されてなる研磨布固定用両面粘着テープを得ることができる。
A laminated body is produced by superposing the obtained laminated film so that the pressure-sensitive adhesive layer of the laminated film faces the surface opposite to the side on which the pressure-sensitive adhesive layer is formed.
By pressing the obtained laminate using a rubber roller or the like, the adhesive layer is laminated and integrated on both surfaces of the base material, and the release film is laminated on the surface of the adhesive layer in a peelable manner. A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth can be obtained.
また、同様の要領で離型フィルムの表面に粘着剤層が形成された積層フィルムを２組作製し、得られた２組の積層フィルムを基材の両面に、積層フィルムの粘着剤層を基材に対向させた状態になるように重ね合わせて積層体を作製し、得られた積層体を、ゴムローラ等を用いて加圧することで、基材の両面に粘着剤層が積層一体化され、かつ、粘着剤層の表面に離型フィルムが剥離可能に積層されてなる研磨布固定用両面粘着テープを得ることができる。 In addition, in the same manner, two sets of laminated films having a pressure-sensitive adhesive layer formed on the surface of the release film were prepared, and the two sets of laminated films thus obtained were formed on both sides of the substrate, and the pressure-sensitive adhesive layer of the laminated film was used as a base. A laminate is produced by superimposing them so as to face the material, and the resulting laminate is pressurized using a rubber roller or the like, whereby the adhesive layer is laminated and integrated on both surfaces of the substrate, And the double-sided adhesive tape for polishing cloth fixation by which a release film is laminated | stacked on the surface of an adhesive layer so that peeling is possible can be obtained.
本発明の研磨布固定用両面粘着テープにおいて、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液又は０．１ｍｏｌ／Ｌの塩酸に、３０℃で、１７０時間浸漬した後の上記粘着剤層の重量増加率は特に限定されないが、１０％未満であることが好ましい。上記重量増加率が１０％以上であると、粘着剤層に酸又はアルカリスラリー液が染み込みやすくなり、粘着剤の化学的分解が起こり、研磨時に研磨布が剥がれることがある。上記重量増加率は、７％未満であることがより好ましい。
なお、上記重量増加率は、下記式（２）を用いて求めることができる。
重量増加率（％）＝１００×（Ｗ４−Ｗ３）／（Ｗ３−Ｗ０） （２）
式（２）中、Ｗ０は基材の重量を表し、Ｗ３は浸漬前の試験片の重量を表し、Ｗ４は浸漬後の試験片の重量を表す。
In the double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth of the present invention, the weight increase rate of the pressure-sensitive adhesive layer after being immersed in a 0.1 mol / L sodium hydroxide aqueous solution or 0.1 mol / L hydrochloric acid at 30 ° C. for 170 hours. Is not particularly limited, but is preferably less than 10%. When the weight increase rate is 10% or more, the pressure-sensitive adhesive layer is likely to soak the acid or alkali slurry liquid, the pressure-sensitive adhesive is chemically decomposed, and the polishing cloth may be peeled off during polishing. The weight increase rate is more preferably less than 7%.
In addition, the said weight increase rate can be calculated | required using following formula (2).
Weight increase rate (%) = 100 × (W 4 −W 3 ) / (W 3 −W 0 ) (2)
In formula (2), W 0 represents the weight of the substrate, W 3 represents the weight of the test piece before immersion, and W 4 represents the weight of the test piece after immersion.
本発明の研磨布固定用両面粘着テープにおいて、１００ｍｍ×２５ｍｍの試験片を用いて、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液又は０．１ｍｏｌ／Ｌの塩酸に３０℃で２４時間浸漬した後に、ＪＩＳ Ｚ０２３７に準拠して測定した、ＳＵＳに対する１８０°引き剥がし粘着力は特に限定されないが、好ましい下限は１０．０Ｎ／２５ｍｍ、好ましい上限は２３．０Ｎ／２５ｍｍである。上記１８０°引き剥がし粘着力が１０．０Ｎ／２５ｍｍ未満であると、研磨時に研磨布が剥がれることがある。上記１８０°引き剥がし粘着力が２３．０Ｎ／２５ｍｍを超えると、使用した研磨布を交換する際に再剥離することが困難となることがある。 In the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth of the present invention, using a 100 mm × 25 mm test piece, after being immersed in a 0.1 mol / L sodium hydroxide aqueous solution or 0.1 mol / L hydrochloric acid at 30 ° C. for 24 hours, The 180 ° peel adhesion to SUS, measured according to JIS Z0237, is not particularly limited, but a preferred lower limit is 10.0 N / 25 mm and a preferred upper limit is 23.0 N / 25 mm. If the 180 ° peeling adhesion is less than 10.0 N / 25 mm, the polishing cloth may be peeled off during polishing. If the 180 ° peeling adhesive strength exceeds 23.0 N / 25 mm, it may be difficult to re-peel when replacing the used polishing cloth.
本発明の研磨布固定用両面粘着テープにおいて、一辺２０ｍｍの平面正方形状の試験片を用いて、ＪＩＳ Ｚ０２３７に準拠した保持力試験を、６０℃、１ｋｇｆ、１時間の条件で行った際の剥離長さは特に限定されないが、好ましい上限は０．５ｍｍである。上記剥離長さが０．５ｍｍを超えると、粘着剤の凝集力が小さすぎて研磨時に加わるせん断力に対する応力が弱く、研磨布固定用両面粘着テープの接着面でずれが生じ、研磨布の平坦性が低下して研磨精度が低下することがある。また、研磨布固定用両面粘着テープの接着面にずれが発生した状態で研磨使用を続けると研磨布が剥がれることがある。 In the double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth of the present invention, peeling when a holding force test according to JIS Z0237 is performed under conditions of 60 ° C., 1 kgf, 1 hour using a flat square test piece having a side of 20 mm. The length is not particularly limited, but a preferred upper limit is 0.5 mm. When the peeling length exceeds 0.5 mm, the cohesive force of the adhesive is too small, the stress against the shearing force applied during polishing is weak, and the adhesive surface of the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth is displaced, and the polishing cloth is flat. In some cases, the polishing accuracy may be reduced due to a decrease in the performance. Further, if polishing is continued in a state where the adhesive surface of the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth is displaced, the polishing cloth may be peeled off.
本発明の研磨布固定用両面粘着テープは、以下の方法により測定したねじりせん断試験において、剥離までの時間が２０分以上であることが好ましい。
まず、１０ｍｍ×１０ｍｍの大きさに切断した研磨布固定用両面粘着テープを用いて、１００ｍｍ×５０ｍｍ×１．８ｍｍの大きさのガラス板と５０ｍｍ×１５ｍｍ×２ｍｍの大きさのアクリル板とを、ガラス板の短辺の端から２０ｍｍかつ長辺の端から２０ｍｍの位置を粘着剤層の中心となるようにし、アクリル板の短辺の端から７．５ｍｍかつ長辺の端から７．５ｍｍの位置を他方の粘着剤層側の中心となるようにして貼り合わせる。
次いで、アクリル板における研磨布固定用両面粘着テープの中心から３０ｍｍ離れた位置に２００ｇの錘を垂下させ、２３℃、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液、又は、２３℃、０．１ｍｏｌ／Ｌの塩酸中に浸漬させる。
水酸化ナトリウム水溶液又は塩酸中への浸漬の開始から、ガラス板からアクリル板が研磨布固定用両面粘着テープごと剥離するまでにかかる剥離時間を測定する。
図１にねじりせん断試験の測定方法を表す模式図を示した。
上記剥離までの時間が２０分未満であると、研磨時に研磨布が剥がれることがある。
The double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth of the present invention preferably has a time until peeling of 20 minutes or more in a torsional shear test measured by the following method.
First, using a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth cut to a size of 10 mm × 10 mm, a glass plate having a size of 100 mm × 50 mm × 1.8 mm and an acrylic plate having a size of 50 mm × 15 mm × 2 mm, The position of 20 mm from the end of the short side of the glass plate and 20 mm from the end of the long side is the center of the adhesive layer, 7.5 mm from the end of the short side of the acrylic plate and 7.5 mm from the end of the long side Bonding is performed so that the position is the center of the other pressure-sensitive adhesive layer.
Next, a 200 g weight is suspended at a position 30 mm away from the center of the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth on the acrylic plate, and 23 ° C., 0.1 mol / L sodium hydroxide aqueous solution, or 23 ° C., 0.1 mol / Immerse in L hydrochloric acid.
From the start of immersion in a sodium hydroxide aqueous solution or hydrochloric acid, the peeling time required from the glass plate to the peeling of the acrylic plate together with the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth is measured.
FIG. 1 is a schematic diagram showing the measurement method of the torsional shear test.
If the time until peeling is less than 20 minutes, the polishing cloth may be peeled off during polishing.
本発明によれば、酸及びアルカリへの耐性に優れ、研磨中に剥がれを生ずることなく、かつ、糊残りをほとんど生じさせずに剥離できる粘着剤を提供することができる。また、本発明によれば、該粘着剤を用いてなる研磨布固定用両面粘着テープを提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the adhesive which is excellent in the tolerance to an acid and an alkali, can be peeled without producing peeling during grinding | polishing, and producing almost no adhesive residue can be provided. Moreover, according to this invention, the double-sided adhesive tape for polishing cloth fixation which uses this adhesive can be provided.
以下に実施例を掲げて本発明を更に詳しく説明するが、本発明はこれら実施例のみに限定されない。 Hereinafter, the present invention will be described in more detail with reference to examples. However, the present invention is not limited to these examples.
（実施例１）
温度計、攪拌機、冷却管を備えた反応器内に、アクリル酸ｔ−ブチル３４．３重量部と、アクリル酸２−エチルヘキシル５７．４重量部と、アクリル酸８重量部と、アクリル酸２−ヒドロキシエチル０．３重量部と、酢酸エチル８０重量部とを加え、窒素置換した後、反応器を加熱して還流を開始した。次いで、上記反応器内に、重合開始剤としてラウロイルパーオキシド０．１重量部を添加した。その後、７０℃にて、５時間還流させて、固形分５５％の（メタ）アクリル酸エステル共重合体溶液を得た。
得られた（メタ）アクリル酸エステル共重合体について、カラムとしてＷａｔｅｒｓ社製「２６９０ Ｓｅｐａｒａｔｉｏｎｓ Ｍｏｄｅｌ」を用いてＧＰＣ法によって測定したポリスチレン換算による重量平均分子量は３３万であった。
Example 1
In a reactor equipped with a thermometer, a stirrer, and a condenser tube, 34.3 parts by weight of t-butyl acrylate, 57.4 parts by weight of 2-ethylhexyl acrylate, 8 parts by weight of acrylic acid, and 2-acrylic acid 2- After 0.3 parts by weight of hydroxyethyl and 80 parts by weight of ethyl acetate were added and purged with nitrogen, the reactor was heated to start refluxing. Next, 0.1 part by weight of lauroyl peroxide was added as a polymerization initiator in the reactor. Thereafter, the mixture was refluxed at 70 ° C. for 5 hours to obtain a (meth) acrylic acid ester copolymer solution having a solid content of 55%.
About the obtained (meth) acrylic acid ester copolymer, the weight average molecular weight by polystyrene conversion measured by GPC method using "2690 Separations Model" made from Waters as a column was 330,000.
得られた（メタ）アクリル酸エステル共重合体１００重量部に対して、酢酸エチル（和光純薬工業社製）１２５重量部、イソシアネート系架橋剤（積水フーラー社製「硬化剤 ＵＡ」）を１．０重量部添加し、攪拌して、粘着剤溶液を得た。 125 parts by weight of ethyl acetate (manufactured by Wako Pure Chemical Industries, Ltd.) and 1 isocyanate crosslinking agent (“curing agent UA” manufactured by Sekisui Fuller) are added to 100 parts by weight of the obtained (meth) acrylic acid ester copolymer. 0.0 part by weight was added and stirred to obtain an adhesive solution.
厚み２３μｍのポリエチレンテレフタレート（ＰＥＴ）基材フィルムの表面に、得られた粘着剤溶液を塗布し、１００℃で５分間乾燥させることにより粘着剤溶液中の酢酸エチルを除去し、厚み３０μｍの粘着剤層（ａ）を形成した。形成した粘着剤層（ａ）上に、離型処理が施された厚み５０μｍのＰＥＴ離型フィルムを離型処理面が粘着剤層（ａ）に対向するように重ね合わせ、フィルム（Ｘ）を得た。
一方、離型処理が施された厚み５０μｍのＰＥＴ離型フィルムを新たに用意し、このＰＥＴ離型フィルムの離型処理面に、得られた粘着剤溶液を塗布し、１００℃で５分間乾燥させることにより、厚み５０μｍの粘着剤層（ｂ）を形成したフィルム（Ｙ）を得た。
フィルム（Ｘ）の粘着剤層（ａ）を形成した側と反対側の面に、フィルム（Ｙ）の粘着剤層（ｂ）が対向するようにフィルム（Ｘ）とフィルム（Ｙ）とを重ね合わせて積層体を作製した。得られた積層体上に３００ｍｍ／分の速度で２ｋｇのゴムローラを１往復させた後、２３℃で７日間養生することにより、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
The obtained pressure-sensitive adhesive solution is applied to the surface of a polyethylene terephthalate (PET) base film having a thickness of 23 μm, and the ethyl acetate in the pressure-sensitive adhesive solution is removed by drying at 100 ° C. for 5 minutes, resulting in a pressure-sensitive adhesive having a thickness of 30 μm. Layer (a) was formed. On the formed pressure-sensitive adhesive layer (a), a 50 μm-thick PET release film subjected to a release treatment is overlaid so that the release treatment surface faces the pressure-sensitive adhesive layer (a), and the film (X) is laminated. Obtained.
On the other hand, a 50 μm-thick PET release film that has been subjected to a release treatment is newly prepared, and the obtained adhesive solution is applied to the release treatment surface of this PET release film and dried at 100 ° C. for 5 minutes. By doing, the film (Y) in which the 50-micrometer-thick adhesive layer (b) was formed was obtained.
The film (X) and the film (Y) are overlapped so that the pressure-sensitive adhesive layer (b) of the film (Y) faces the surface opposite to the side where the pressure-sensitive adhesive layer (a) of the film (X) is formed. Together, a laminate was produced. Polishing with the adhesive layer laminated on both sides of the PET base film by reciprocating a 2 kg rubber roller once at a speed of 300 mm / min on the resulting laminate, followed by curing at 23 ° C. for 7 days A double-sided adhesive tape for fixing cloth was obtained.
（実施例２）
アクリル酸の配合量を６重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例２で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は３３万であった。
(Example 2)
Except having changed the compounding quantity of acrylic acid into 6 weight part, it carried out similarly to Example 1, and obtained the double-sided adhesive tape for polishing cloth fixing by which the adhesive layer was laminated | stacked and integrated on both surfaces of PET base film.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 2 was 330,000.
（実施例３）
アクリル酸ｔ−ブチルの配合量を１８．４重量部に変更し、アクリル酸２−エチルヘキシルの配合量を７３．３重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例３で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は３５万であった。
(Example 3)
PET base film in the same manner as in Example 1 except that the amount of t-butyl acrylate was changed to 18.4 parts by weight and the amount of 2-ethylhexyl acrylate was changed to 73.3 parts by weight. A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which pressure-sensitive adhesive layers were laminated and integrated on both sides was obtained.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 3 was 350,000.
（実施例４）
アクリル酸ｔ−ブチルの配合量を３５．７重量部に変更し、アクリル酸２−エチルヘキシルの配合量を６０．０重量部に変更し、アクリル酸の配合量を４重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例４で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は３０万であった。
Example 4
Other than changing the amount of t-butyl acrylate to 35.7 parts by weight, changing the amount of 2-ethylhexyl acrylate to 60.0 parts by weight, and changing the amount of acrylic acid to 4 parts by weight In the same manner as in Example 1, a double-sided pressure-sensitive adhesive tape for fixing a polishing cloth in which pressure-sensitive adhesive layers were laminated and integrated on both sides of a PET base film was obtained.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 4 was 300,000.
（実施例５）
イソシアネート系架橋剤（積水フーラー社製「硬化剤 ＵＡ」）の配合量を２．０重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例５で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は３３万であった。
(Example 5)
Adhesive layers are laminated on both sides of the PET base film in the same manner as in Example 1 except that the blending amount of the isocyanate-based crosslinking agent (“curing agent UA” manufactured by Sekisui Fuller) is changed to 2.0 parts by weight. An integrated double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth was obtained.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 5 was 330,000.
（実施例６）
イソシアネート系架橋剤（積水フーラー社製「硬化剤 ＵＡ」）の配合量を０．３重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例６で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は３３万であった。
(Example 6)
Adhesive layers are laminated on both sides of the PET base film in the same manner as in Example 1 except that the blending amount of the isocyanate-based crosslinking agent (“curing agent UA” manufactured by Sekisui Fuller Co., Ltd.) is changed to 0.3 parts by weight. An integrated double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth was obtained.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 6 was 330,000.
（実施例７）
アクリル酸ｔ−ブチルの配合量を２０．０重量部に変更し、アクリル酸２−エチルヘキシルの配合量を７５．５重量部に変更し、アクリル酸の配合量を４重量部に変更し、更に、アクリルアミドを０．５重量部添加したこと以外は実施例１と同様にして、（メタ）アクリル酸エステル共重合体溶液を得た。
得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は５２万であった。
(Example 7)
The amount of t-butyl acrylate is changed to 20.0 parts by weight, the amount of 2-ethylhexyl acrylate is changed to 75.5 parts by weight, the amount of acrylic acid is changed to 4 parts by weight, and A (meth) acrylic acid ester copolymer solution was obtained in the same manner as in Example 1 except that 0.5 part by weight of acrylamide was added.
The weight average molecular weight of the obtained (meth) acrylic acid ester copolymer was 520,000.
得られた（メタ）アクリル酸エステル共重合体を用い、イソシアネート系架橋剤（積水フーラー社製「硬化剤 ＵＡ」）の配合量を０．３重量部に変更したこと以外は実施例１と同様にして、粘着剤溶液を得た。 Using the obtained (meth) acrylic acid ester copolymer, the same as Example 1 except that the amount of the isocyanate-based crosslinking agent (“Curing Agent UA” manufactured by Sekisui Fuller Co., Ltd.) was changed to 0.3 parts by weight. Thus, an adhesive solution was obtained.
得られた粘着剤溶液を用いて粘着剤層（ａ）を形成し、形成した粘着剤層（ａ）上に、離型処理が施された剥離紙を離型処理面が粘着剤層（ａ）に対向するように重ね合わせたこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
なお、粘着剤層（ｂ）については、実施例１で得られた粘着剤溶液を用いて形成されている。
A pressure-sensitive adhesive layer (a) is formed using the obtained pressure-sensitive adhesive solution, and a release paper subjected to a release treatment is formed on the formed pressure-sensitive adhesive layer (a). A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which a pressure-sensitive adhesive layer was laminated and integrated on both sides of a PET base film was obtained in the same manner as in Example 1 except that they were superposed so as to face each other.
The pressure-sensitive adhesive layer (b) is formed using the pressure-sensitive adhesive solution obtained in Example 1.
（実施例８）
アクリル酸ｔ−ブチルの配合量を１４．７重量部に変更し、アクリル酸２−エチルヘキシルの配合量を８０．４重量部に変更し、アクリルアミドの配合量を０．２重量部に変更したこと以外は実施例７と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例８で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は５２万であった。
(Example 8)
The amount of t-butyl acrylate was changed to 14.7 parts by weight, the amount of 2-ethylhexyl acrylate was changed to 80.4 parts by weight, and the amount of acrylamide was changed to 0.2 parts by weight. Except for the above, a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which pressure-sensitive adhesive layers were laminated and integrated on both surfaces of a PET base film was obtained in the same manner as Example 7.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 8 was 520,000.
（実施例９）
アクリル酸ｔ−ブチルの配合量を５重量部に変更し、アクリル酸２−エチルヘキシルの配合量を８６．２重量部に変更し、アクリル酸の配合量を８重量部に変更し、アクリルアミドの配合量を０．５重量部に変更したこと以外は実施例７と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例９で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は５０万であった。
Example 9
The amount of t-butyl acrylate was changed to 5 parts by weight, the amount of 2-ethylhexyl acrylate was changed to 86.2 parts by weight, the amount of acrylic acid was changed to 8 parts by weight, and acrylamide was added. A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which pressure-sensitive adhesive layers were laminated and integrated on both sides of a PET base film was obtained in the same manner as Example 7 except that the amount was changed to 0.5 parts by weight.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 9 was 500,000.
（実施例１０）
アクリル酸ｔ−ブチルの配合量を１０．５重量部に変更し、アクリル酸２−エチルヘキシルの配合量を８５．７重量部に変更し、アクリル酸の配合量を２重量部に変更し、アクリルアミドの配合量を１．５重量部に変更したこと以外は実施例７と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例１０で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は５１万であった。
(Example 10)
The amount of t-butyl acrylate was changed to 10.5 parts by weight, the amount of 2-ethylhexyl acrylate was changed to 85.7 parts by weight, the amount of acrylic acid was changed to 2 parts by weight, and acrylamide A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which pressure-sensitive adhesive layers were laminated and integrated on both surfaces of a PET base film was obtained in the same manner as in Example 7 except that the blending amount of was changed to 1.5 parts by weight.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 10 was 510,000.
（実施例１１）
アクリル酸ｔ−ブチルの配合量を２０．２重量部に変更し、アクリル酸２−エチルヘキシルの配合量を７５．５重量部に変更し、アクリル酸を２重量部に変更し、アクリルアミドの配合量を２．０重量部に変更したこと以外は実施例７と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例１１で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は５３万であった。
(Example 11)
The amount of t-butyl acrylate is changed to 20.2 parts by weight, the amount of 2-ethylhexyl acrylate is changed to 75.5 parts by weight, acrylic acid is changed to 2 parts by weight, and the amount of acrylamide is changed. A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which a pressure-sensitive adhesive layer was laminated and integrated on both sides of a PET base film was obtained in the same manner as in Example 7 except that was changed to 2.0 parts by weight.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 11 was 530,000.
（実施例１２）
アクリル酸ｔ−ブチルの配合量を１９．７重量部に変更し、アクリル酸２−エチルヘキシルの配合量を７５．５重量部に変更し、アクリルアミドをメタクリル酸ジメチルアミノエチルに変更し、アクリル酸の配合量を２重量部に変更したこと以外は実施例７と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
実施例１２で得られた（メタ）アクリル酸エステル共重合体の重量平均分子量は５１万であった。
(Example 12)
The amount of t-butyl acrylate was changed to 19.7 parts by weight, the amount of 2-ethylhexyl acrylate was changed to 75.5 parts by weight, acrylamide was changed to dimethylaminoethyl methacrylate, A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which a pressure-sensitive adhesive layer was laminated and integrated on both sides of a PET base film was obtained in the same manner as in Example 7 except that the blending amount was changed to 2 parts by weight.
The weight average molecular weight of the (meth) acrylic acid ester copolymer obtained in Example 12 was 510,000.
（比較例１）
アクリル酸ｔ−ブチルの配合量を５１．８重量部に変更し、アクリル酸２−エチルヘキシルの配合量を３９．９重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
比較例１で得られた（メタ）アクリル酸エステル共重合体の固形分は４５％であり、重量平均分子量は３６万であった。
(Comparative Example 1)
PET base film in the same manner as in Example 1 except that the amount of t-butyl acrylate was changed to 51.8 parts by weight and the amount of 2-ethylhexyl acrylate was changed to 39.9 parts by weight. A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which pressure-sensitive adhesive layers were laminated and integrated on both sides was obtained.
The solid content of the (meth) acrylic acid ester copolymer obtained in Comparative Example 1 was 45%, and the weight average molecular weight was 360,000.
（比較例２）
アクリル酸ｔ−ブチルの配合量を２．０重量部に変更し、アクリル酸２−エチルヘキシルの配合量を８９．７重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
比較例２で得られた（メタ）アクリル酸エステル共重合体の固形分は４５％であり、重量平均分子量は３６万であった。
(Comparative Example 2)
PET base film in the same manner as in Example 1 except that the amount of t-butyl acrylate was changed to 2.0 parts by weight and the amount of 2-ethylhexyl acrylate was changed to 89.7 parts by weight. A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which pressure-sensitive adhesive layers were laminated and integrated on both sides was obtained.
The solid content of the (meth) acrylic acid ester copolymer obtained in Comparative Example 2 was 45%, and the weight average molecular weight was 360,000.
（比較例３）
アクリル酸ｔ−ブチル３４．３重量部の代わりにアクリル酸ｎ−ブチル３４．３重量部を用い、アクリル酸２−エチルヘキシルの配合量を５７．３重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
比較例３で得られた（メタ）アクリル酸エステル共重合体の固形分は５０％であり、重量平均分子量は３２万であった。
（比較例４）
アクリル酸を用いず、アクリル酸２−エチルヘキシルの配合量を７２．１重量部に変更し、アクリル酸ｔ−ブチルの配合量を２７．６重量部に変更したこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
比較例４で得られた（メタ）アクリル酸エステル共重合体の固形分は５０％であり、重量平均分子量は３４万であった。
（比較例５）
アクリル酸２−エチルヘキシル５７．４重量部の代わりにアクリル酸ｎ−ブチル５７．４重量部を用いたこと以外は実施例１と同様にして、ＰＥＴ基材フィルムの両面に粘着剤層が積層一体化された研磨布固定用両面粘着テープを得た。
比較例５で得られた（メタ）アクリル酸エステル共重合体の固形分は５０％であり、重量平均分子量は３５万であった。
(Comparative Example 3)
Example 1 except that 34.3 parts by weight of n-butyl acrylate was used instead of 34.3 parts by weight of t-butyl acrylate, and the blending amount of 2-ethylhexyl acrylate was changed to 57.3 parts by weight. Similarly, a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which pressure-sensitive adhesive layers were laminated and integrated on both sides of a PET base film was obtained.
The solid content of the (meth) acrylic acid ester copolymer obtained in Comparative Example 3 was 50%, and the weight average molecular weight was 320,000.
(Comparative Example 4)
Example 1 was used except that acrylic acid was not used, the amount of 2-ethylhexyl acrylate was changed to 72.1 parts by weight, and the amount of t-butyl acrylate was changed to 27.6 parts by weight. Thus, a double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth in which pressure-sensitive adhesive layers were laminated and integrated on both surfaces of a PET base film was obtained.
The solid content of the (meth) acrylic acid ester copolymer obtained in Comparative Example 4 was 50%, and the weight average molecular weight was 340,000.
(Comparative Example 5)
A pressure-sensitive adhesive layer is laminated and integrated on both sides of the PET base film in the same manner as in Example 1 except that 57.4 parts by weight of n-butyl acrylate is used instead of 57.4 parts by weight of 2-ethylhexyl acrylate. A double-sided pressure-sensitive adhesive tape for fixing an abrasive cloth was obtained.
The solid content of the (meth) acrylic acid ester copolymer obtained in Comparative Example 5 was 50%, and the weight average molecular weight was 350,000.
＜評価＞
実施例１〜１２及び比較例１〜５で得られた粘着剤溶液及び研磨布固定用両面粘着テープについて以下の評価を行った。結果を表１及び表２に示した。
<Evaluation>
The following evaluation was performed about the adhesive solution obtained in Examples 1-12 and Comparative Examples 1-5 and the double-sided adhesive tape for polishing cloth fixation. The results are shown in Tables 1 and 2.
（１）ゲル分率の測定
得られた研磨布固定用両面粘着テープを５０ｍｍ×２５ｍｍの平面長方形状に切断して試験片を作製し、この重量Ｗ１を測定した。試験片を酢酸エチル中に２３℃にて２４時間浸漬した後、２００メッシュのステンレスメッシュを介して試験片を酢酸エチルから取り出して、１１０℃の条件下で１時間乾燥させた。乾燥後の試験片の重量Ｗ２を測定した。基材として用いたＰＥＴフィルムの重量Ｗ０を用いて、式（１）によりゲル分率を算出した。
(1) Measurement of gel fraction The obtained double-sided pressure-sensitive adhesive tape for fixing abrasive cloth was cut into a flat rectangular shape of 50 mm x 25 mm to prepare a test piece, and the weight W 1 was measured. After immersing the test piece in ethyl acetate at 23 ° C. for 24 hours, the test piece was taken out from ethyl acetate through a 200-mesh stainless steel mesh and dried at 110 ° C. for 1 hour. The weight W 2 after drying the test piece was measured. The gel fraction was calculated by the formula (1) using the weight W 0 of the PET film used as the substrate.
（２）薬液浸漬後の重量増加率
得られた研磨布固定用両面粘着テープを縦５０ｍｍ×横５０ｍｍの試験片に切り出した後、粘着面上に設けたＰＥＴ離型フィルム（実施例７〜１２においては、粘着剤層（ａ）側は剥離紙、粘着剤層（ｂ）側はＰＥＴ離型フィルム）を両面とも剥離し、浸漬前の粘着テープの重量を測定した。その後、離型紙及び離型フィルムが剥離された粘着テープを３０℃、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液中に粘着面が容器に触れないよう浸漬させ、１７０時間放置した。所定時間経過後、上記粘着テープを水酸化ナトリウム水溶液中から取り出し、表面に付着した水を圧縮空気で除去した後、浸漬後の上記粘着テープの重量を測定した。その後、酢酸エチルを用いて両面の粘着剤を完全に除去し基材の重量を測定し、式（２）より重量増加率を算出した。
また、３０℃、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液の代わりに、３０℃、０．１ｍｏｌ／Ｌの塩酸を用いて同様の評価を行った。
(2) Weight increase rate after immersion in chemical solution The obtained double-sided pressure-sensitive adhesive tape for fixing polishing cloth was cut into a test piece of 50 mm length x 50 mm width, and then a PET release film provided on the pressure-sensitive adhesive surface (Examples 7 to 12) , The pressure-sensitive adhesive layer (a) side was peeled from the release paper and the pressure-sensitive adhesive layer (b) side was the PET release film), and the weight of the pressure-sensitive adhesive tape before immersion was measured. Thereafter, the pressure-sensitive adhesive tape from which the release paper and the release film were peeled was immersed in a 0.1 mol / L sodium hydroxide aqueous solution at 30 ° C. so that the pressure-sensitive adhesive surface did not touch the container, and left for 170 hours. After a predetermined time, the pressure-sensitive adhesive tape was taken out from the aqueous sodium hydroxide solution, water attached to the surface was removed with compressed air, and the weight of the pressure-sensitive adhesive tape after immersion was measured. Thereafter, the pressure-sensitive adhesive on both sides was completely removed using ethyl acetate, the weight of the substrate was measured, and the weight increase rate was calculated from the formula (2).
Further, the same evaluation was performed using 30 mol C and 0.1 mol / L hydrochloric acid instead of 30 mol C and 0.1 mol / L sodium hydroxide aqueous solution.
（３）薬液浸漬後の１８０°引き剥がし粘着力
得られた研磨布固定用両面粘着テープの研磨布用粘着剤層（粘着剤層（ｂ））上に３８μｍ厚みのＰＥＴフィルムを裏打ちし、縦１００ｍｍ×横２５ｍｍの平面長方形状の試験片を切り出した。切り出した試験片を２ｋｇのローラで押圧し、ステンレス板上に貼り着けてから、温度２３℃、相対湿度５０％の雰囲気下にて３０分間放置した。次いで、試験片を貼り付けたステンレス板を３０℃、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液中に浸漬させ、２４時間放置した。その後、ステンレス板を取り出して軽く水洗した後、圧縮空気で付着した水を除去し、引張試験機を用いてＪＩＳ Ｚ０２３７に準拠して１８０°引き剥がし粘着力を測定した。
また、３０℃、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液の代わりに、３０℃、０．１ｍｏｌ／Ｌの塩酸を用いて同様の評価を行った。
(3) A 180 μm-stretch PET film with a 38 μm thickness is lined on the adhesive layer for the abrasive cloth (adhesive layer (b)) of the double-sided adhesive tape for fixing the abrasive cloth obtained after 180 ° peeling adhesion after chemical immersion. A 100 mm × 25 mm horizontal rectangular test piece was cut out. The cut test piece was pressed with a 2 kg roller and stuck on a stainless steel plate, and then left for 30 minutes in an atmosphere of a temperature of 23 ° C. and a relative humidity of 50%. Next, the stainless steel plate to which the test piece was attached was immersed in a 0.1 mol / L sodium hydroxide aqueous solution at 30 ° C. and left for 24 hours. Thereafter, the stainless steel plate was taken out and lightly washed with water, then the water adhering to the compressed air was removed, and the adhesive strength was measured by peeling it 180 ° according to JIS Z0237 using a tensile tester.
Further, the same evaluation was performed using 30 mol C and 0.1 mol / L hydrochloric acid instead of 30 mol C and 0.1 mol / L sodium hydroxide aqueous solution.
（４）保持力
得られた研磨布固定用両面粘着テープの研磨布用粘着剤層（粘着剤層（ｂ））上に３８μｍ厚みのＰＥＴフィルムを裏打ちし、一辺２０ｍｍの平面正方形状の試験片を切り出した。切り出した試験片を２ｋｇのローラで押圧し、粘着テープの粘着剤層をステンレス板上に貼り着けた後、４０℃で、６０分間養生させた。
次いで、ＰＥＴフィルムの下面に試験片が水平に位置した状態となるように配設し、６０℃において、試験片の長さ方向の端部に１ｋｇｆの荷重を垂直方向に付加し、試験片に荷重を付加してから１時間後の剥離長さを、ルーペを用いて測定した。
(4) Retaining force A 38 μm-thick PET film is lined on the abrasive cloth pressure-sensitive adhesive layer (adhesive layer (b)) of the obtained double-sided pressure-sensitive adhesive tape for fixing the abrasive cloth, and a flat square test piece having a side of 20 mm. Was cut out. The cut test piece was pressed with a 2 kg roller, and an adhesive layer of an adhesive tape was attached on a stainless steel plate, and then cured at 40 ° C. for 60 minutes.
Next, the test piece is placed on the lower surface of the PET film so that the test piece is positioned horizontally, and at 60 ° C., a 1 kgf load is applied to the end of the test piece in the longitudinal direction in the vertical direction, The peel length 1 hour after applying the load was measured using a magnifying glass.
（５）ねじりせん断試験
得られた研磨布固定用両面粘着テープを１０ｍｍ×１０ｍｍの大きさに切断し、１００ｍｍ×５０ｍｍ×１．８ｍｍの大きさのガラス板と５０ｍｍ×１５ｍｍ×２ｍｍの大きさのアクリル板とを、ガラス板の短辺の端から２０ｍｍ、かつ、長辺の端から２０ｍｍの位置に研磨布固定用両面粘着テープの定盤固定用粘着剤層（粘着層（ａ））側の中心がきて、アクリル板の短辺の端から７．５ｍｍ、かつ、長辺の端から７．５ｍｍの位置に研磨布固定用両面粘着テープの研磨布固定用粘着剤層（粘着層（ｂ））側の中心がくるようにして貼り合わせた。次いで、アクリル板の両面テープの中心から３０ｍｍの位置に２００ｇの錘を垂下させた。錘を垂下させた状態で、２３℃、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液中に浸漬した。浸漬の開始から、ガラス板からアクリル板が研磨布固定用両面粘着テープごと剥離するまでにかかる剥離時間を測定した。
また、２３℃、０．１ｍｏｌ／Ｌの水酸化ナトリウム水溶液の代わりに、２３℃、０．１ｍｏｌ／Ｌの塩酸を用いて同様の評価を行った。
(5) Torsional shear test The obtained double-sided pressure-sensitive adhesive tape for fixing abrasive cloth is cut into a size of 10 mm x 10 mm, and a glass plate of a size of 100 mm x 50 mm x 1.8 mm and a size of 50 mm x 15 mm x 2 mm. The acrylic plate is placed 20 mm from the short side end of the glass plate and 20 mm from the long side end of the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth on the side of the pressure-sensitive adhesive layer (adhesive layer (a)). Abrasive cloth fixing pressure-sensitive adhesive layer (adhesive layer (b)) of the double-sided pressure-sensitive adhesive tape for fixing the abrasive cloth at a position 7.5 mm from the short side end of the acrylic plate and 7.5 mm from the long side end. ) Bonding was done so that the center of the side came. Next, a 200 g weight was suspended at a position 30 mm from the center of the double-sided tape on the acrylic plate. It was immersed in a 0.1 mol / L sodium hydroxide aqueous solution at 23 ° C. with the weight suspended. From the start of the immersion, the peeling time required for the acrylic plate to peel from the glass plate together with the double-sided pressure-sensitive adhesive tape for fixing the polishing cloth was measured.
Further, the same evaluation was performed using 23 ° C. and 0.1 mol / L hydrochloric acid instead of 23 ° C. and 0.1 mol / L sodium hydroxide aqueous solution.
（６）ガラス転移温度
動的粘弾性測定装置（ＩＴ計測制御社製、「ＤＶＡ−２００」）による測定において、実施例及び比較例で得られた粘着剤溶液を乾燥させて得られた１ｍｍ厚の粘着剤試料を用い、−８０〜２００℃、１０Ｈｚにおいて動的粘弾性を測定し、損失正接（ｔａｎδ）の極大値の温度をガラス転移温度（Ｔｇ）として測定した。
(6) 1 mm thickness obtained by drying the adhesive solutions obtained in Examples and Comparative Examples in the measurement with a glass transition temperature dynamic viscoelasticity measuring apparatus ("DVA-200" manufactured by IT Measurement Control Co., Ltd.) The viscoelasticity was measured at −80 to 200 ° C. and 10 Hz, and the maximum temperature of loss tangent (tan δ) was measured as the glass transition temperature (Tg).
（７）研磨中はがれの有無
得られた研磨布固定用両面粘着テープを、ゴムロールを用いて研磨布に貼り着けた。次いで、研磨布側からゴムロールを押し当てることにより、研磨装置の定盤に研磨布固定用両面粘着テープを介して研磨布を固定した。
ガラス板を被研磨試験体とし、研磨スラリー（Ｃａｂｏｔ Ｍｉｃｒｏｅｌｅｃｔｒｏｎｉｃｓ社製、「ＳＳ２５」又は「Ｗ２０００」）を用い、研磨圧力４９．０ｋＰａ、回転数１００ｒｐｍで５分間研磨を行った。その後、研磨布固定用両面粘着テープと定盤の界面について、剥離状態を目視にて観察した。同様にして研磨と観察とを１０回行った結果、１０回中、１回も剥がれがなかった場合を「○」と、１０回中、１回も剥がれがなかったものの、浮きが発生した場合を「△」と、１０回中、１回以上剥がれが見られた場合を「×」と評価した。
(7) The double-sided pressure-sensitive adhesive tape for fixing a polishing cloth obtained by the presence or absence of peeling during polishing was attached to the polishing cloth using a rubber roll. Next, by pressing a rubber roll from the polishing cloth side, the polishing cloth was fixed to the surface plate of the polishing apparatus via a double-sided adhesive tape for fixing the polishing cloth.
Using a glass plate as a specimen to be polished, polishing was performed for 5 minutes at a polishing pressure of 49.0 kPa and a rotation speed of 100 rpm using a polishing slurry (manufactured by Cabot Microelectronics, “SS25” or “W2000”). Then, the peeling state was observed visually about the interface of the double-sided adhesive tape for polishing cloth fixation, and a surface plate. Similarly, when 10 times of polishing and observation were performed, “○” indicates that no peeling occurred once in 10 times, and no occurrence of peeling once in 10 times, but floating occurred Was evaluated as “X” when “Δ” was observed and peeling occurred 10 times or more in 10 times.
（８）再剥離性
（７）に記載した研磨中はがれの有無の評価後、更に２４時間放置し、充分に接着力が昂進した後、定盤から粘着テープを剥離し、定盤上に粘着剤が残っているか否か確認した。容易に剥離でき、かつ、粘着剤残りが認められなかった場合を「◎」と、粘着剤残りが認められなかった場合を「○」と、一部に粘着剤残りが認められた場合を「△」と、全面に粘着剤残りが認められた場合を「×」と評価した。
(8) Re-peelability After evaluating the presence or absence of peeling during polishing as described in (7), the film is left for another 24 hours, and after sufficient adhesive strength has been developed, the adhesive tape is peeled off from the surface plate and adhered onto the surface plate. It was confirmed whether the agent remained. When it is easy to peel off and there is no adhesive residue, `` ◎ '', when there is no adhesive residue `` ○ '', when there is some adhesive residue `` A case where an adhesive residue was observed on the entire surface was evaluated as “×”.
本発明によれば、酸及びアルカリへの耐性に優れ、研磨中に剥がれを生ずることなく、かつ、糊残りをほとんど生じさせずに剥離できる粘着剤を提供することができる。また、本発明によれば、該粘着剤を用いてなる研磨布固定用両面粘着テープを提供することができる。 ADVANTAGE OF THE INVENTION According to this invention, the adhesive which is excellent in the tolerance to an acid and an alkali, can be peeled without producing peeling during grinding | polishing, and producing almost no adhesive residue can be provided. Moreover, according to this invention, the double-sided adhesive tape for polishing cloth fixation which uses this adhesive can be provided.
１ ガラス板
２ 両面粘着テープ
３ アクリル板
４ 錘
1
Claims (8)
動的粘弾性測定により得られるガラス転移温度（Ｔｇ）が−１０〜２０℃の範囲にあり、
前記（メタ）アクリル酸エステル共重合体は、（メタ）アクリル酸ｔ−ブチルと、（メタ）アクリル酸２−エチルヘキシルと、アクリル酸とを含有するモノマー混合物を共重合させてなる共重合体であり、
前記モノマー混合物は、前記モノマー混合物１００重量部に対して（メタ）アクリル酸ｔ−ブチルを５〜５０重量部、（メタ）アクリル酸２−エチルヘキシルを４２〜８９重量部、かつ、前記（メタ）アクリル酸ｔ−ブチルと前記（メタ）アクリル酸２−エチルヘキシルとの合計１００重量部に対して１０重量部以下のアクリル酸を含有するものであり、
前記イソシアネート系架橋剤を前記（メタ）アクリル酸エステル共重合体１００重量部に対して０．１〜４．０重量部含有する
ことを特徴とする粘着剤。 A pressure-sensitive adhesive containing a (meth) acrylic acid ester copolymer and an isocyanate-based crosslinking agent,
The glass transition temperature (Tg) obtained by dynamic viscoelasticity measurement is in the range of −10 to 20 ° C.,
The (meth) acrylic acid ester copolymer is a copolymer obtained by copolymerizing a monomer mixture containing t-butyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, and acrylic acid. Yes,
The monomer mixture is 5 to 50 parts by weight of t-butyl (meth) acrylate, 42 to 89 parts by weight of 2-ethylhexyl (meth) acrylate, and 100 parts by weight of the above (meth). Containing 10 parts by weight or less of acrylic acid with respect to a total of 100 parts by weight of t-butyl acrylate and 2-ethylhexyl (meth) acrylate,
A pressure-sensitive adhesive comprising 0.1 to 4.0 parts by weight of the isocyanate-based crosslinking agent with respect to 100 parts by weight of the (meth) acrylic acid ester copolymer.
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| JP5604398B2 (en) * | 2011-09-30 | 2014-10-08 | 富士フイルム株式会社 | Planographic printing plate precursor and lithographic printing plate preparation method |
| WO2013099684A1 (en) * | 2011-12-28 | 2013-07-04 | 綜研化学株式会社 | Optical member adhesive composition, adhesive sheet using same, optical member provided with adhesive layer, and flat panel display |
| JP6412873B2 (en) * | 2013-09-27 | 2018-10-24 | リンテック株式会社 | Adhesive sheet |
| JP2016125026A (en) * | 2015-01-07 | 2016-07-11 | 日東電工株式会社 | Pressure-sensitive adhesive tape |
| JP6523125B2 (en) * | 2015-09-30 | 2019-05-29 | 積水化学工業株式会社 | Double-sided adhesive tape, double-sided adhesive tape for fixing electronic device parts and double-sided adhesive tape for fixing automotive parts |
| WO2019143076A1 (en) * | 2018-01-22 | 2019-07-25 | 주식회사 엘지화학 | Back grinding tape |
| CN113214763B (en) * | 2020-01-21 | 2023-01-10 | 3M创新有限公司 | Pressure-sensitive adhesive composition and pressure-sensitive adhesive tape |
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