JP5795472B2 - Adhesive for attaching conductive film and adhesive sheet for attaching conductive film - Google Patents
Adhesive for attaching conductive film and adhesive sheet for attaching conductive film Download PDFInfo
- Publication number
- JP5795472B2 JP5795472B2 JP2010264208A JP2010264208A JP5795472B2 JP 5795472 B2 JP5795472 B2 JP 5795472B2 JP 2010264208 A JP2010264208 A JP 2010264208A JP 2010264208 A JP2010264208 A JP 2010264208A JP 5795472 B2 JP5795472 B2 JP 5795472B2
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- JP
- Japan
- Prior art keywords
- conductive film
- adhesive
- sensitive adhesive
- mass
- pressure
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000000853 adhesive Substances 0.000 title claims description 84
- 230000001070 adhesive effect Effects 0.000 title claims description 84
- 239000004820 Pressure-sensitive adhesive Substances 0.000 claims description 78
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 55
- 239000000178 monomer Substances 0.000 claims description 46
- 229920005989 resin Polymers 0.000 claims description 30
- 239000011347 resin Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 27
- 125000000217 alkyl group Chemical group 0.000 claims description 26
- 229920006243 acrylic copolymer Polymers 0.000 claims description 25
- 239000003431 cross linking reagent Substances 0.000 claims description 23
- 239000012790 adhesive layer Substances 0.000 claims description 15
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 14
- 229910052731 fluorine Inorganic materials 0.000 claims description 14
- 239000011737 fluorine Substances 0.000 claims description 14
- 125000004432 carbon atom Chemical group C* 0.000 claims description 12
- 239000003208 petroleum Substances 0.000 claims description 11
- 125000003709 fluoroalkyl group Chemical group 0.000 claims description 10
- 229920002367 Polyisobutene Polymers 0.000 claims description 8
- PJXISJQVUVHSOJ-UHFFFAOYSA-N indium(iii) oxide Chemical compound [O-2].[O-2].[O-2].[In+3].[In+3] PJXISJQVUVHSOJ-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 229910003437 indium oxide Inorganic materials 0.000 claims description 6
- -1 2-ethylhexyl Chemical group 0.000 description 36
- 239000010410 layer Substances 0.000 description 19
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 18
- 239000007787 solid Substances 0.000 description 15
- 239000000463 material Substances 0.000 description 14
- 239000012948 isocyanate Substances 0.000 description 12
- 229920001577 copolymer Polymers 0.000 description 11
- 238000005259 measurement Methods 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 229920000139 polyethylene terephthalate Polymers 0.000 description 10
- 239000005020 polyethylene terephthalate Substances 0.000 description 10
- 239000000758 substrate Substances 0.000 description 10
- 239000000123 paper Substances 0.000 description 9
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 8
- 125000002723 alicyclic group Chemical group 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 125000000524 functional group Chemical group 0.000 description 7
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 6
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 6
- 238000000576 coating method Methods 0.000 description 6
- 150000002513 isocyanates Chemical class 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 5
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 description 4
- 239000004925 Acrylic resin Substances 0.000 description 4
- 229920000178 Acrylic resin Polymers 0.000 description 4
- 239000004593 Epoxy Substances 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000011787 zinc oxide Substances 0.000 description 4
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 3
- 239000004971 Cross linker Substances 0.000 description 3
- 229920005987 OPPANOL® Polymers 0.000 description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 3
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- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 3
- 229910001887 tin oxide Inorganic materials 0.000 description 3
- QTKPMCIBUROOGY-UHFFFAOYSA-N 2,2,2-trifluoroethyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OCC(F)(F)F QTKPMCIBUROOGY-UHFFFAOYSA-N 0.000 description 2
- 229920002126 Acrylic acid copolymer Polymers 0.000 description 2
- 229920002284 Cellulose triacetate Polymers 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- VZCYOOQTPOCHFL-OWOJBTEDSA-N Fumaric acid Chemical compound OC(=O)\C=C\C(O)=O VZCYOOQTPOCHFL-OWOJBTEDSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 239000004793 Polystyrene Substances 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- NNLVGZFZQQXQNW-ADJNRHBOSA-N [(2r,3r,4s,5r,6s)-4,5-diacetyloxy-3-[(2s,3r,4s,5r,6r)-3,4,5-triacetyloxy-6-(acetyloxymethyl)oxan-2-yl]oxy-6-[(2r,3r,4s,5r,6s)-4,5,6-triacetyloxy-2-(acetyloxymethyl)oxan-3-yl]oxyoxan-2-yl]methyl acetate Chemical compound O([C@@H]1O[C@@H]([C@H]([C@H](OC(C)=O)[C@H]1OC(C)=O)O[C@H]1[C@@H]([C@@H](OC(C)=O)[C@H](OC(C)=O)[C@@H](COC(C)=O)O1)OC(C)=O)COC(=O)C)[C@@H]1[C@@H](COC(C)=O)O[C@@H](OC(C)=O)[C@H](OC(C)=O)[C@H]1OC(C)=O NNLVGZFZQQXQNW-ADJNRHBOSA-N 0.000 description 2
- 125000001931 aliphatic group Chemical group 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 description 2
- 239000012964 benzotriazole Substances 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000013522 chelant Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- KBLWLMPSVYBVDK-UHFFFAOYSA-N cyclohexyl prop-2-enoate Chemical compound C=CC(=O)OC1CCCCC1 KBLWLMPSVYBVDK-UHFFFAOYSA-N 0.000 description 2
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
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- 150000002466 imines Chemical class 0.000 description 2
- 229920000554 ionomer Polymers 0.000 description 2
- 229920000092 linear low density polyethylene Polymers 0.000 description 2
- 239000004707 linear low-density polyethylene Substances 0.000 description 2
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- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
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- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
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- DTGKSKDOIYIVQL-WEDXCCLWSA-N (+)-borneol Chemical group C1C[C@@]2(C)[C@@H](O)C[C@@H]1C2(C)C DTGKSKDOIYIVQL-WEDXCCLWSA-N 0.000 description 1
- QERNPKXJOBLNFM-UHFFFAOYSA-N 1,1,2,2,3,3,4,4-octafluoropentane Chemical compound CC(F)(F)C(F)(F)C(F)(F)C(F)F QERNPKXJOBLNFM-UHFFFAOYSA-N 0.000 description 1
- VIPLBNSVTIFFDD-UHFFFAOYSA-N 1,2,2,3-tetrafluoropropyl prop-2-enoate Chemical compound C(C=C)(=O)OC(C(CF)(F)F)F VIPLBNSVTIFFDD-UHFFFAOYSA-N 0.000 description 1
- OHLKMGYGBHFODF-UHFFFAOYSA-N 1,4-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=C(CN=C=O)C=C1 OHLKMGYGBHFODF-UHFFFAOYSA-N 0.000 description 1
- FWWWRCRHNMOYQY-UHFFFAOYSA-N 1,5-diisocyanato-2,4-dimethylbenzene Chemical compound CC1=CC(C)=C(N=C=O)C=C1N=C=O FWWWRCRHNMOYQY-UHFFFAOYSA-N 0.000 description 1
- LFSYUSUFCBOHGU-UHFFFAOYSA-N 1-isocyanato-2-[(4-isocyanatophenyl)methyl]benzene Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=CC=C1N=C=O LFSYUSUFCBOHGU-UHFFFAOYSA-N 0.000 description 1
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- WWUCYCYSEUEANO-UHFFFAOYSA-N 2-(aziridin-1-yl)acetamide Chemical compound NC(=O)CN1CC1 WWUCYCYSEUEANO-UHFFFAOYSA-N 0.000 description 1
- 125000000954 2-hydroxyethyl group Chemical group [H]C([*])([H])C([H])([H])O[H] 0.000 description 1
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- DKGCZVJEVNZACI-UHFFFAOYSA-N n-[[5-[[bis(oxiran-2-ylmethyl)amino]methyl]-5-methylcyclohexa-1,3-dien-1-yl]methyl]-1-(oxiran-2-yl)-n-(oxiran-2-ylmethyl)methanamine Chemical compound C1C(CN(CC2OC2)CC2OC2)=CC=CC1(C)CN(CC1OC1)CC1CO1 DKGCZVJEVNZACI-UHFFFAOYSA-N 0.000 description 1
- 125000001280 n-hexyl group Chemical group C(CCCCC)* 0.000 description 1
- RPQRDASANLAFCM-UHFFFAOYSA-N oxiran-2-ylmethyl prop-2-enoate Chemical compound C=CC(=O)OCC1CO1 RPQRDASANLAFCM-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 229920001643 poly(ether ketone) Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920002530 polyetherether ketone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920000307 polymer substrate Polymers 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 239000013464 silicone adhesive Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 238000010897 surface acoustic wave method Methods 0.000 description 1
- 238000010345 tape casting Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- IUCJMVBFZDHPDX-UHFFFAOYSA-N tretamine Chemical compound C1CN1C1=NC(N2CC2)=NC(N2CC2)=N1 IUCJMVBFZDHPDX-UHFFFAOYSA-N 0.000 description 1
- 229950001353 tretamine Drugs 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
Images
Landscapes
- Adhesives Or Adhesive Processes (AREA)
- Position Input By Displaying (AREA)
- Laminated Bodies (AREA)
- Adhesive Tapes (AREA)
Description
本発明は導電膜に対して貼付する粘着剤、特に静電容量方式タッチパネルや液晶ディスプレイ、電子ペーパーなどの部材の一部として用いられる導電膜に対して貼付する粘着剤及び粘着シートに関する。 The present invention relates to a pressure-sensitive adhesive to be attached to a conductive film, and particularly to a pressure-sensitive adhesive and a pressure-sensitive adhesive sheet to be attached to a conductive film used as a part of a member such as a capacitive touch panel, a liquid crystal display, or electronic paper.
透明な高分子基板やガラス上に、スズを添加した酸化インジウムや酸化亜鉛、酸化スズなどの導電性材料からなる透明導電膜を形成した積層体は、タッチパネル、液晶ディスプレイ、電子ペーパーなどの情報端末機器における透明電極として広く用いられている。
このような透明電極が用いられる情報端末機器は近年、小型化、薄型化が進んでおり、製品内部は複雑かつ緻密な設計が行われる。例えば表示装置や基板などの部材と、透明電極を有する積層体とを粘着シートを介して直接固定し、無駄な空間を省略する工夫がなされている。このような場合は透明電極と粘着剤が直接接触する。
Laminates in which a transparent conductive film made of a conductive material such as indium oxide, zinc oxide, or tin oxide with tin added is formed on a transparent polymer substrate or glass is an information terminal such as a touch panel, liquid crystal display, or electronic paper Widely used as a transparent electrode in equipment.
In recent years, information terminal devices using such transparent electrodes have been reduced in size and thickness, and the interior of products is designed to be complicated and precise. For example, a device has been devised in which a member such as a display device or a substrate and a laminated body having a transparent electrode are directly fixed via an adhesive sheet to eliminate useless space. In such a case, the transparent electrode and the adhesive are in direct contact.
また、透明電極と粘着剤が直接接触する他の例として、静電容量方式タッチパネルが挙げられる。静電容量方式タッチパネルは、例えば、図1の断面図に示すように、表面から、ハードコート層1、樹脂フィルム層2、化粧印刷層3、埋め込み用粘着剤層4、ガラス層5、透明導電膜6、粘着剤層7、表示装置8がこの順に積層されている。透明導電膜6には微弱な電圧が印加され、その表面に電荷が蓄えられることにより、電界が形成された状態が維持されている。樹脂フィルム層2のハードコート層1側を指やタッチペンなどの導体で接触すると電界の状態が変化し、放電される。透明導電膜6の四隅に流れる微弱な電流変化を計算処理し、接触位置の検出を行う。
Another example of direct contact between the transparent electrode and the adhesive is a capacitive touch panel. For example, as shown in the cross-sectional view of FIG. 1, the capacitive touch panel includes a hard coat layer 1, a
前述の情報端末機器のように、内部部材において粘着剤が導電膜に直接接触する場合、従来の粘着剤では高温高湿の環境下で貼付対象である導電膜の電気抵抗値を増加させる傾向にあるため、情報端末機器の故障の原因となる。
特に静電容量方式タッチパネルの場合、前記位置検出の高精度化を実現するため、透明導電膜6と表示装置8を固定する粘着剤層7には、透明導電膜6の電気容量(静電容量)を変化させない性能が要求される。
このような要求に対して、金属層の腐食を有効に防止する粘着剤が提案されている(例えば、特許文献1参照)。
When the adhesive directly contacts the conductive film in the internal member as in the information terminal device described above, the conventional adhesive tends to increase the electrical resistance value of the conductive film to be applied in a high temperature and high humidity environment. For this reason, it may cause a failure of the information terminal device.
In particular, in the case of a capacitive touch panel, in order to realize high accuracy of the position detection, the
In response to such demands, an adhesive that effectively prevents corrosion of the metal layer has been proposed (see, for example, Patent Document 1).
特許文献1記載の粘着剤組成物は、金属腐食防止効果を目的としてベンゾトリアゾールやその誘導体を粘着剤組成物の必須成分としているが、ベンゾトリアゾールおよびその誘導体のブリードによって粘着力が変動する問題や、当該成分の経時変化による変色が懸念される。さらに粘着剤と前記電気抵抗値の増加との関係が示されてなく、スズ添加酸化インジウム(Indium Tin Oxide、以下、ITO)やAgナノワイヤーなどの導電膜と、LCDなど精密な表示装置を固定する粘着剤としては、さらに性質向上の余地が残されている。 The pressure-sensitive adhesive composition described in Patent Document 1 uses benzotriazole or a derivative thereof as an essential component of the pressure-sensitive adhesive composition for the purpose of preventing metal corrosion, but there is a problem that the adhesive force varies depending on the bleeding of benzotriazole and its derivatives. There is a concern about discoloration due to aging of the component. Furthermore, the relationship between the pressure-sensitive adhesive and the increase in the electrical resistance value is not shown, and a conductive film such as indium tin oxide (ITO) or Ag nanowire and a precise display device such as an LCD are fixed. As a pressure-sensitive adhesive, there is still room for property improvement.
本発明は、上記事情に鑑みてなされたものであって、高温高湿の環境下で貼付対象である導電膜の抵抗値増加率を大幅に抑制し、前記環境下においても情報端末機器の故障の原因となる前記導電膜の劣化を生じさせない導電膜貼付用粘着シート及び前記導電膜貼付用粘着シートに用いられる粘着剤を提供することを目的とする。 The present invention has been made in view of the above circumstances, and greatly suppresses the rate of increase in the resistance value of a conductive film to be applied in a high-temperature and high-humidity environment. It aims at providing the adhesive used for the electrically conductive film sticking adhesive sheet and the electrically conductive film sticking adhesive sheet which do not produce the deterioration of the said electrically conductive film which causes the above.
本発明者らは上記の課題を解決するため、鋭意研究を行った結果、粘着剤の含水率を低減することにより課題を解決できることを見出した。すなわち本発明は、下記(1)〜(9)を提供するものである。
(1)本発明の第2の態様の導電膜貼付用粘着剤は、カールフィッシャー法による含水率が0〜0.2%であり、フルオロアルキル(メタ)アクリレートモノマー由来の構成単位(a3)を含むフッ素含有アクリル系共重合体(A2)および架橋剤(B)を含有することを特徴とする。
(2)本発明の第2の態様の導電膜貼付用粘着剤は、フルオロアルキル(メタ)アクリレートモノマー由来の構成単位(a3)を3〜30質量%、アルキル基の炭素数が4〜20のアルキル(メタ)アクリレートモノマー由来の構成単位(a4)を60〜95質量%含むフッ素含有アクリル系共重合体(A2’)および架橋剤(B)を含有することが好ましい。
(3)本発明の第3の態様の導電膜貼付用粘着シートは、カールフィッシャー法による含水率が0〜0.2%であり、ポリイソブチレン系樹脂と水素化石油樹脂からなることを特徴とする。
(4)本発明の第4の態様の導電膜貼付用粘着シートは、前記本発明の粘着剤からなる粘着剤層の両面に剥離シートが積層されているものである。
(5)本発明の第5の態様の導電膜貼付用粘着シートは、前記本発明の粘着剤からなる粘着剤層が基材フィルムの少なくとも一方の面に積層されているものである。
(6)本発明の第4の態様または第5の態様の導電膜貼付用粘着シートは、貼付対象の導電膜が透明であることが好ましい。
(7)本発明の第4の態様または第5の態様の導電膜貼付用粘着シートは、貼付対象の導電膜がスズ添加酸化インジウムであることが好ましい。
(8)本発明の第4の態様または第5の態様の導電膜貼付用粘着シートは、タッチパネルの部材として使用されることが好ましい。
(9)本発明の第4の態様または第5の態様の導電膜貼付用粘着シートにおいて、前記タッチパネルが静電容量方式であることが好ましい。
In order to solve the above-mentioned problems, the present inventors have conducted extensive research and found that the problems can be solved by reducing the moisture content of the pressure-sensitive adhesive. That is, the present invention provides the following (1) to ( 9 ).
( 1 ) The adhesive for attaching a conductive film according to the second aspect of the present invention has a moisture content of 0 to 0.2% according to the Karl Fischer method, and includes a structural unit (a3) derived from a fluoroalkyl (meth) acrylate monomer. It contains a fluorine-containing acrylic copolymer (A2) and a crosslinking agent (B).
( 2 ) The adhesive for electrically conductive film sticking of the 2nd aspect of this invention is 3-30 mass% of structural units (a3) derived from a fluoroalkyl (meth) acrylate monomer, and the carbon number of an alkyl group is 4-20. It is preferable to contain the fluorine-containing acrylic copolymer (A2 ′) containing 60 to 95% by mass of the structural unit (a4) derived from the alkyl (meth) acrylate monomer and the crosslinking agent (B).
( 3 ) The adhesive sheet for attaching a conductive film according to the third aspect of the present invention has a water content of 0 to 0.2% according to the Karl Fischer method, and is characterized by comprising a polyisobutylene resin and a hydrogenated petroleum resin. To do.
( 4 ) The adhesive sheet for electrically conductive film sticking of the 4th aspect of this invention has a peeling sheet laminated | stacked on both surfaces of the adhesive layer which consists of an adhesive of the said this invention.
( 5 ) The pressure-sensitive adhesive sheet for attaching a conductive film according to the fifth aspect of the present invention is such that a pressure-sensitive adhesive layer made of the pressure-sensitive adhesive of the present invention is laminated on at least one surface of a substrate film.
( 6 ) In the adhesive sheet for attaching a conductive film according to the fourth aspect or the fifth aspect of the present invention, the conductive film to be attached is preferably transparent.
( 7 ) As for the adhesive sheet for electrically conductive film sticking of the 4th aspect or the 5th aspect of this invention, it is preferable that the electrically conductive film of sticking object is a tin addition indium oxide.
( 8 ) It is preferable that the adhesive sheet for electrically conductive film sticking of the 4th aspect or the 5th aspect of this invention is used as a member of a touch panel.
( 9 ) In the adhesive sheet for attaching a conductive film according to the fourth aspect or the fifth aspect of the present invention, it is preferable that the touch panel is a capacitance type.
本発明の導電膜貼付用粘着シートによれば、高温高湿の環境下での粘着シートが貼付された導電膜の抵抗値増加率を大幅に抑制できるため、前記環境下においても本発明の導電膜貼付用粘着シートを用いた情報端末機器を良好な状態で用いることができる。 According to the pressure-sensitive adhesive sheet for attaching a conductive film of the present invention, the resistance increase rate of the conductive film to which the pressure-sensitive adhesive sheet is attached in a high-temperature and high-humidity environment can be significantly suppressed. The information terminal device using the adhesive sheet for film sticking can be used in a good state.
本明細書および特許請求の範囲において、「構成単位」とは、樹脂成分(重合体、共重合体)を構成するモノマー単位(単量体単位)を意味する。
「(メタ)アクリレート」とは、α位に水素原子が結合したアクリレートと、α位にメチル基が結合したメタクリレートの一方あるいは両方を意味する。
In the present specification and claims, the “structural unit” means a monomer unit (monomer unit) constituting a resin component (polymer, copolymer).
“(Meth) acrylate” means one or both of an acrylate having a hydrogen atom bonded to the α-position and a methacrylate having a methyl group bonded to the α-position.
本発明の導電膜貼付用粘着剤は、カールフィッシャー法による含水率が0〜0.2%である。
カールフィッシャー法とは、水の定量用試薬であるカールフィッシャー試薬を使用して、水の量を求める方法であり、カールフィッシャー試薬とは、ヨウ素、二酸化硫黄、塩基、及び、アルコール等の溶剤より構成される試薬である。この試薬中のI21モルとH2O1モルとが反応することを利用して、試料をカールフィッシャー試薬で滴定することより、試料中の水の量を精度よく求めることができる。尚、ここで示す水分含量は、カールフィッシャー法の方法原理を用いた装置で測定した値であれば、測定装置については特に限定されない。
また、粘着剤の水分量を測定する際には、精度を向上させる上で、測定に供する粘着剤を、たとえば、23℃、50%相対湿度の環境下に24時間放置しておく等、予め決めておいた環境下に所定時間保管しておいてから測定することが好ましい。
The adhesive for attaching a conductive film of the present invention has a water content of 0 to 0.2% according to the Karl Fischer method.
The Karl Fischer method is a method for determining the amount of water using the Karl Fischer reagent, which is a reagent for quantifying water. The Karl Fischer reagent is obtained from a solvent such as iodine, sulfur dioxide, base, and alcohol. It is a configured reagent. By utilizing the reaction between 1 mol of I 2 and 1 mol of H 2 O in this reagent, the amount of water in the sample can be accurately determined by titrating the sample with a Karl Fischer reagent. The moisture content shown here is not particularly limited as long as it is a value measured by an apparatus using the Karl Fischer method principle.
Further, when measuring the moisture content of the pressure-sensitive adhesive, in order to improve accuracy, the pressure-sensitive adhesive to be used for measurement is allowed to stand for 24 hours in an environment of 23 ° C. and 50% relative humidity. It is preferable to perform measurement after storing for a predetermined time in the determined environment.
本発明の導電膜貼付用粘着剤は、カールフィッシャー法による含水率が0〜0.2%であることが必須である。含水率が0.2%以下の場合、本発明の導電膜貼付用粘着シートは、粘着剤の種類に依存することなく、高温高湿下においても粘着シートが貼付された導電膜の電気抵抗値増加率を10%以下に抑えることができる。
含水率と電気抵抗値の増加率との間には、相関関係が見られ、粘着シートの含水率の上昇に従い、高温高湿の環境下においた粘着シート付き導電膜の電気抵抗値増加率が上昇する。電気抵抗値増加率が20%を超える場合、タッチパネルの操作において、機器が指の動きについていけなるという不都合が生じる。従って、電気抵抗値の増加率に相関する含水率を一定に抑える必要がある。
It is essential that the adhesive for attaching a conductive film of the present invention has a moisture content of 0 to 0.2% according to the Karl Fischer method. When the moisture content is 0.2% or less, the adhesive sheet for attaching a conductive film of the present invention does not depend on the type of adhesive, and the electrical resistance value of the conductive film to which the adhesive sheet is attached even under high temperature and high humidity The increase rate can be suppressed to 10% or less.
There is a correlation between the moisture content and the increase rate of the electrical resistance value, and as the moisture content of the adhesive sheet increases, the electrical resistance value increase rate of the conductive film with the adhesive sheet in a high temperature and high humidity environment increases. To rise. When the electrical resistance value increase rate exceeds 20%, there is a disadvantage that the device can follow the movement of the finger in the operation of the touch panel. Therefore, it is necessary to keep the moisture content correlated with the increasing rate of the electrical resistance value constant.
本発明の導電膜貼付用粘着剤の材質としては、カールフィッシャー法による含水率が0〜0.2%であれば特に限定されないが、アルキル基の炭素数が5〜20のアルキル(メタ)アクリレートモノマー由来の構成単位(a1)を30〜99質量%含むアクリル系共重合体(A1)および架橋剤(B)を含有するアクリル系樹脂や、フルオロアルキル(メタ)アクリレートモノマー由来の構成単位(a3)を含むフッ素含有アクリル系共重合体(A2)および架橋剤(B)を含有するフッ素含有アクリル系樹脂が好ましい。 The material of the adhesive for attaching a conductive film of the present invention is not particularly limited as long as the moisture content by the Karl Fischer method is 0 to 0.2%, but the alkyl (meth) acrylate having 5 to 20 carbon atoms in the alkyl group. An acrylic resin containing 30 to 99% by mass of the monomer-derived structural unit (a1) and an acrylic resin containing the crosslinking agent (B), or a structural unit derived from a fluoroalkyl (meth) acrylate monomer (a3 ) Containing a fluorine-containing acrylic copolymer (A2) and a crosslinking agent (B).
アクリル系共重合体(A1)中の構成単位(a1)はアルキル基の炭素数が5〜20のアルキル(メタ)アクリレートモノマーである。
アルキル基の炭素数が5〜20のアルキル(メタ)アクリレートモノマーは、直鎖状又は分岐鎖状のアルキル基含有アクリレートモノマーであり、n−ヘキシル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、イソオクチル(メタ)アクリレート、ラウリル(メタ)アクリレート、ステアリル(メタ)アクリレートなどが挙げられるが、粘着剤の粘着力を高める観点から2−エチルヘキシルアクリレートがより好ましい。なおここでいうアルキル基とは、IUPAC命名法に則りアルカンの末端から水素を1つ取り除いた置換基であり、一般式−CnH2n+1で示されるものを指す。
The structural unit (a1) in the acrylic copolymer (A1) is an alkyl (meth) acrylate monomer having 5 to 20 carbon atoms in the alkyl group.
The alkyl (meth) acrylate monomer having 5 to 20 carbon atoms in the alkyl group is a linear or branched alkyl group-containing acrylate monomer, and includes n-hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, Although isooctyl (meth) acrylate, lauryl (meth) acrylate, stearyl (meth) acrylate, etc. are mentioned, 2-ethylhexyl acrylate is more preferable from the viewpoint of increasing the adhesive strength of the adhesive. The alkyl group here is a substituent obtained by removing one hydrogen from the end of the alkane in accordance with the IUPAC nomenclature, and refers to a group represented by the general formula —C n H 2n + 1 .
前記アルキルアクリレートモノマー由来の構成単位(a1)の含有量は、モノマー全量を100質量%としたときに、30〜99質量%であることが好ましく、40〜84質量%であることがより好ましく、50〜69質量%であることが最も好ましい。 The content of the structural unit (a1) derived from the alkyl acrylate monomer is preferably 30 to 99% by mass, more preferably 40 to 84% by mass, when the total amount of monomers is 100% by mass. Most preferably, it is 50-69 mass%.
また、前記アクリル系共重合体(A1)は、前記アルキル基の炭素数が5〜20のアルキル(メタ)アクリレートモノマー由来の構成単位(a1)と、脂環式基含有(メタ)アクリレートモノマーの由来の構成単位(a2)の両方を含有することが好ましく、アルキル基の炭素数が5〜20のアルキル(メタ)アクリレートモノマー由来の構成単位(a1)を50〜69質量%、炭素数が5〜20の脂環式基含有(メタ)アクリレートモノマー由来の構成単位(a2)を30〜49質量%含むアクリル系共重合体(A1’)であることがより好ましい。 The acrylic copolymer (A1) is composed of a structural unit (a1) derived from an alkyl (meth) acrylate monomer having 5 to 20 carbon atoms in the alkyl group and an alicyclic group-containing (meth) acrylate monomer. It is preferable to contain both the structural unit (a2) derived from 50 to 69% by mass of the structural unit (a1) derived from an alkyl (meth) acrylate monomer having 5 to 20 carbon atoms in the alkyl group and 5 carbon atoms. It is more preferable that it is an acrylic copolymer (A1 ′) containing 30 to 49% by mass of the structural unit (a2) derived from ˜20 alicyclic group-containing (meth) acrylate monomers.
アクリル系共重合体(A1’)中の構成単位(a2)は、炭素数が5〜20の脂環式基含有(メタ)アクリレートモノマーである。
脂環式基含有(メタ)アクリレートモノマーの「脂環式基」とは、環状の脂肪族基(シクロアルキル基)であって芳香族性を持たないことを意味する。脂環式基含有(メタ)アクリレートモノマーは単環状化合物であっても多環式状化合物であってもよい。脂環式基含有(メタ)アクリレートモノマーとしては、シクロヘキシル(メタ)アクリレート、イソボニル(メタ)アクリレート、トリシクロデカン(メタ)アクリレートなどが好ましいが、粘着剤の粘着力を高める観点からシクロヘキシルアクリレートがより好ましい。
また前述のように脂環式基含有(メタ)アクリレートモノマーは、アルキル(メタ)アクリレートモノマーに該当しないため、構成単位(a2)と構成単位(a1)は完全に区別される。
The structural unit (a2) in the acrylic copolymer (A1 ′) is an alicyclic group-containing (meth) acrylate monomer having 5 to 20 carbon atoms.
The “alicyclic group” of the alicyclic group-containing (meth) acrylate monomer means a cyclic aliphatic group (cycloalkyl group) and has no aromaticity. The alicyclic group-containing (meth) acrylate monomer may be a monocyclic compound or a polycyclic compound. As the alicyclic group-containing (meth) acrylate monomer, cyclohexyl (meth) acrylate, isobornyl (meth) acrylate, tricyclodecane (meth) acrylate, and the like are preferable, but cyclohexyl acrylate is more preferable from the viewpoint of increasing the adhesive strength of the pressure-sensitive adhesive. preferable.
Moreover, since the alicyclic group-containing (meth) acrylate monomer does not correspond to the alkyl (meth) acrylate monomer as described above, the structural unit (a2) and the structural unit (a1) are completely distinguished.
フッ素含有アクリル系共重合体(A2)中の構成単位(a3)は、フルオロアルキル(メタ)アクリレートモノマーが好ましい。
フルオロアルキル(メタ)アクリレートモノマーとしては、フルオロ基を分子中に有するものであれば特に制限無く用いられ、2,2,2−トリフルオロエチルアクリレート、2,2,2−トリフルオロエチルメタクリレート、2,2,2,3−テトラフルオロプロピルアクリレート、1H,1H,5H−オクタフルオロペンチルアクリレート、1H,1H,5H−オクタフルオロペンチルメタクリレート等が挙げられるが、2,2,2−トリフルオロエチルメタクリレートが好ましい。
The structural unit (a3) in the fluorine-containing acrylic copolymer (A2) is preferably a fluoroalkyl (meth) acrylate monomer.
The fluoroalkyl (meth) acrylate monomer is not particularly limited as long as it has a fluoro group in the molecule, and includes 2,2,2-trifluoroethyl acrylate, 2,2,2-trifluoroethyl methacrylate, 2 1,2,2,3-tetrafluoropropyl acrylate, 1H, 1H, 5H-octafluoropentyl acrylate, 1H, 1H, 5H-octafluoropentyl methacrylate, etc. preferable.
前記フルオロアルキル(メタ)アクリレートモノマー由来の構成単位(a3)の含有量は、モノマー全量を100質量%としたときに、1〜50質量%であることが好ましく、2〜40質量%であることが好ましく、3〜30質量%であることが最も好ましい。 The content of the structural unit (a3) derived from the fluoroalkyl (meth) acrylate monomer is preferably 1 to 50% by mass, and 2 to 40% by mass when the total amount of the monomers is 100% by mass. Is preferable, and it is most preferable that it is 3-30 mass%.
また、フッ素含有アクリル系共重合体(A2)は、前記フルオロアルキル(メタ)アクリレートモノマー由来の構成単位(a3)と、アルキル基の炭素数が4〜20のアルキル(メタ)アクリレートモノマー由来の構成単位(a4)の両方を含有することが好ましく、フルオロアルキル(メタ)アクリレートモノマー由来の構成単位(a3)を3〜30質量%、アルキル基の炭素数が4〜20のアルキル(メタ)アクリレートモノマー由来の構成単位(a4)を60〜95質量%含むアクリル系共重合体(A2’)であることがより好ましい。 In addition, the fluorine-containing acrylic copolymer (A2) is composed of the structural unit (a3) derived from the fluoroalkyl (meth) acrylate monomer and the alkyl (meth) acrylate monomer having 4 to 20 carbon atoms in the alkyl group. It is preferable to contain both of the unit (a4), the alkyl (meth) acrylate monomer having 3 to 30% by mass of the structural unit (a3) derived from the fluoroalkyl (meth) acrylate monomer and the alkyl group having 4 to 20 carbon atoms. The acrylic copolymer (A2 ′) containing 60 to 95% by mass of the derived structural unit (a4) is more preferable.
フッ素含有アクリル系共重合体(A2’)中の構成単位(a4)は、炭素数が4〜20のアルキル(メタ)アクリレートモノマーである。
アルキル基の炭素数が4〜20のアルキル(メタ)アクリレートモノマーとしては、直鎖状又は分岐鎖状のアルキル基含有アクリレートモノマーが好ましく、n−ブチル(メタ)アクリレート、イソブチル(メタ)アクリレート、n−ヘキシル(メタ)アクリレート、2−エチルヘキシル(メタ)アクリレート、イソオクチル(メタ)アクリレート、ラウリル(メタ)アクリレート、ステアリル(メタ)アクリレートなどが挙げられるが、粘着剤の粘着力を出す観点からn−ブチルアクリレート、2−エチルヘキシルアクリレートがより好ましい。
The structural unit (a4) in the fluorine-containing acrylic copolymer (A2 ′) is an alkyl (meth) acrylate monomer having 4 to 20 carbon atoms.
As the alkyl (meth) acrylate monomer having 4 to 20 carbon atoms in the alkyl group, a linear or branched alkyl group-containing acrylate monomer is preferable, and n-butyl (meth) acrylate, isobutyl (meth) acrylate, n -Hexyl (meth) acrylate, 2-ethylhexyl (meth) acrylate, isooctyl (meth) acrylate, lauryl (meth) acrylate, stearyl (meth) acrylate and the like, n-butyl from the viewpoint of exerting the adhesive strength of the adhesive An acrylate and 2-ethylhexyl acrylate are more preferable.
前記アクリル系共重合体(A1)および(A1’)、フッ素含有アクリル系共重合体(A2)および(A2’)は、官能基含有モノマーを含有しても良い。
官能基含有モノマーの「官能基」とは、水酸基、カルボキシル基等の、架橋剤と反応して結合可能な反応性官能基を意味する。
水酸基含有モノマーとしては、2-ヒドロキシエチル(メタ)アクリレート、2-ヒドロキシプロピル(メタ)アクリレート、3-ヒドロキシプロピル(メタ)アクリレート、2-ヒドロキシブチル(メタ)アクリレート、3-ヒドロキシブチル(メタ)アクリレート、4-ヒドロキシブチル(メタ)アクリレート等のヒドロキシアルキル(メタ)アクリレート等が挙げられる。
カルボキシル基含有モノマーとしては、アクリル酸、メタクリル酸、クロトン酸、フマル酸、イタコン酸、マレイン酸、2−カルボキシエチルメタクリレート等が挙げられる。
粘着力を高める観点から水酸基含有モノマーが好ましく、2-ヒドロキシエチルアクリレートがより好ましい。
官能基含有モノマー由来の構成単位の含有量は、粘着力を高める観点から0.01〜20質量%が好ましく、0.05〜10質量%がより好ましく、0.1〜5質量%が特に好ましい。
The acrylic copolymers (A1) and (A1 ′) and the fluorine-containing acrylic copolymers (A2) and (A2 ′) may contain a functional group-containing monomer.
The “functional group” of the functional group-containing monomer means a reactive functional group that can be bonded by reacting with a crosslinking agent, such as a hydroxyl group or a carboxyl group.
As the hydroxyl group-containing monomer, 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, 3-hydroxypropyl (meth) acrylate, 2-hydroxybutyl (meth) acrylate, 3-hydroxybutyl (meth) acrylate Examples include hydroxyalkyl (meth) acrylates such as 4-hydroxybutyl (meth) acrylate.
Examples of the carboxyl group-containing monomer include acrylic acid, methacrylic acid, crotonic acid, fumaric acid, itaconic acid, maleic acid, and 2-carboxyethyl methacrylate.
From the viewpoint of increasing the adhesive strength, a hydroxyl group-containing monomer is preferable, and 2-hydroxyethyl acrylate is more preferable.
The content of the structural unit derived from the functional group-containing monomer is preferably 0.01 to 20% by mass, more preferably 0.05 to 10% by mass, and particularly preferably 0.1 to 5% by mass from the viewpoint of increasing the adhesive strength. .
前記アクリル系共重合体(A1)(A1’)中、および、フッ素含有アクリル系共重合体(A2)(A2’)中の構成単位として、粘着力制御や凝集力の制御を目的にその他のモノマーを任意で含んでもよい。その他のモノマーとしては、スチレン、α-メチルスチレン、ビニルトルエン、蟻酸ビニル、酢酸ビニル、アクリロニトリル、グリシジルアクリレート、グリシジルメタクリレート等のモノマーが挙げられる。 As a structural unit in the acrylic copolymer (A1) (A1 ′) and in the fluorine-containing acrylic copolymer (A2) (A2 ′), other components are used for the purpose of controlling adhesive force and cohesive force. Monomers may optionally be included. Examples of other monomers include monomers such as styrene, α-methylstyrene, vinyl toluene, vinyl formate, vinyl acetate, acrylonitrile, glycidyl acrylate, and glycidyl methacrylate.
本発明の導電膜貼付用粘着剤の材質となる前記アクリル系樹脂およびフッ素含有アクリル系樹脂は、これらと共に架橋剤(B)を含むことが好ましい。架橋剤(B)は、前述の官能基含有モノマーの「官能基」と反応して架橋し、粘着剤として必要な凝集力を発現する。架橋剤(B)としては、例えば、有機多価イソシアネート化合物、有機多価エポキシ化合物、有機多価イミン化合物が挙げられる。これらの中で入手しやすさなどの観点から、有機多価イソシアネート化合物が好ましい。 It is preferable that the acrylic resin and the fluorine-containing acrylic resin used as the material for the adhesive for attaching a conductive film of the present invention contain a crosslinking agent (B) together with them. The crosslinking agent (B) reacts with the “functional group” of the functional group-containing monomer described above to crosslink, and expresses the cohesive force necessary as an adhesive. Examples of the crosslinking agent (B) include organic polyvalent isocyanate compounds, organic polyvalent epoxy compounds, and organic polyvalent imine compounds. Among these, an organic polyvalent isocyanate compound is preferable from the viewpoint of availability.
有機多価イソシアネート化合物としては、2,4−トリレンジイソシアネート、2,6−トリレンジイソシアネート、1,3−キシリレンジイソシアネート、1,4−キシリレンジイソシアネート、ジフェニルメタン−4,4’−ジイソシアネート、ジフェニルメタン−2,4’−ジイソシアネート、3−メチルジフェニルメタンジイソシアネート、ヘキサメチレンジイソシアネート、イソホロンジイソシアネート、ジシクロヘキシルメタン−4,4’−ジイソシアネート、ジシクロヘキシルメタン−2,4’−ジイソシアネート、リジンイソシアネートなどが挙げられる。これらの多価イソシアネート化合物の三量体、ならびにこれら多価イソシアネート化合物とポリオール化合物とを反応させて得られる末端イソシアネートレタンプレポリマー等も使用することができる。 As organic polyvalent isocyanate compounds, 2,4-tolylene diisocyanate, 2,6-tolylene diisocyanate, 1,3-xylylene diisocyanate, 1,4-xylylene diisocyanate, diphenylmethane-4,4′-diisocyanate, diphenylmethane -2,4'-diisocyanate, 3-methyldiphenylmethane diisocyanate, hexamethylene diisocyanate, isophorone diisocyanate, dicyclohexylmethane-4,4'-diisocyanate, dicyclohexylmethane-2,4'-diisocyanate, lysine isocyanate and the like. Trimers of these polyvalent isocyanate compounds, terminal isocyanate-retane prepolymers obtained by reacting these polyvalent isocyanate compounds and polyol compounds, and the like can also be used.
有機多価エポキシ化合物としては、ビスフェノールA型エポキシ化合物、ビスフェノールF型エポキシ化合物、1,3−ビス(N,N−ジグリシジルアミノメチル)トルエン、N,N,N’,N’−テトラグリシジル−4,4−ジアミノジフェニルメタン等が挙げられる。 Examples of organic polyvalent epoxy compounds include bisphenol A type epoxy compounds, bisphenol F type epoxy compounds, 1,3-bis (N, N-diglycidylaminomethyl) toluene, N, N, N ′, N′-tetraglycidyl- Examples include 4,4-diaminodiphenylmethane.
有機多価イミン化合物としては、N,N’−ジフェニルメタン−4,4’−ビス(1−アジリジンカルボキシアミド)、トリメチロールプロパン−トリ−β−アジリジニルプロピオナート、テトラメチロールメタン−トリ−β−アジリジニルプロピオナート、N,N’−トルエン−2,4−ビス(1−アジリジンカルボキシアミド)トリエチレンメラミン等が挙げられる。 Examples of organic polyvalent imine compounds include N, N′-diphenylmethane-4,4′-bis (1-aziridinecarboxamide), trimethylolpropane-tri-β-aziridinylpropionate, tetramethylolmethane-tri- β-aziridinylpropionate, N, N′-toluene-2,4-bis (1-aziridinecarboxyamide) triethylenemelamine and the like can be mentioned.
架橋剤の添加量としては、粘着力を高める観点から、アクリル系共重合体の固形分100質量部に対して0.01〜10質量部とするのが好ましく、0.03〜7質量部とするのがより好ましく、0.05〜5質量部とするのが特に好ましい。 As an addition amount of a crosslinking agent, it is preferable to set it as 0.01-10 mass parts with respect to solid content of 100 mass parts of an acrylic copolymer from a viewpoint of raising adhesive force, 0.03-7 mass parts and More preferably, it is particularly preferably 0.05 to 5 parts by mass.
また、本発明の導電膜貼付用粘着剤の材質としては、ポリイソブチレン系樹脂と水素化石油樹脂からなることが好ましい。 In addition, the material for the adhesive for attaching a conductive film of the present invention is preferably composed of a polyisobutylene resin and a hydrogenated petroleum resin.
前記ポリイソブチレン系樹脂の質量平均分子量としては2万以上が好ましく、5万〜600万がより好ましく、15万〜50万が特に好ましい。
また、前記ポリイソブチレン系樹脂の含有量は、粘着剤中、30〜95質量%が好ましく、40〜90質量%がより好ましく、50〜85質量%が特に好ましい。
The mass average molecular weight of the polyisobutylene resin is preferably 20,000 or more, more preferably 50,000 to 6,000,000, particularly preferably 150,000 to 500,000.
Moreover, 30-95 mass% is preferable in an adhesive, and, as for content of the said polyisobutylene-type resin, 40-90 mass% is more preferable, and 50-85 mass% is especially preferable.
本発明において、水素化石油樹脂とは、水素化触媒を使用して、脂肪族系石油樹脂、芳香族系石油樹脂、シクロペンタジエン系石油樹脂等の石油樹脂を水素化したものである。
前記水素化石油樹脂の含有量は、粘着剤中、5〜50質量%が好ましく10〜40質量%がより好ましく、15〜30質量%が特に好ましい。
In the present invention, the hydrogenated petroleum resin is obtained by hydrogenating a petroleum resin such as an aliphatic petroleum resin, an aromatic petroleum resin, or a cyclopentadiene petroleum resin using a hydrogenation catalyst.
The content of the hydrogenated petroleum resin is preferably 5 to 50% by mass, more preferably 10 to 40% by mass, and particularly preferably 15 to 30% by mass in the pressure-sensitive adhesive.
本発明の粘着剤はシート状に加工された様々な粘着シートの形態をとりうる。例えば前記本発明の粘着剤からなる粘着剤層の両面に剥離シートが積層された基材フィルム無し両面粘着シートの形態としても良い。この形態とした場合、ITOやAgナノワイヤーなどの導電膜と、LCDなどの表示装置の固定に用いられる。 The pressure-sensitive adhesive of the present invention can take various forms of pressure-sensitive adhesive sheets processed into a sheet shape. For example, it is good also as a form of the double-sided adhesive sheet without a base film by which the peeling sheet was laminated | stacked on both surfaces of the adhesive layer which consists of an adhesive of the said invention. In this case, it is used for fixing a conductive film such as ITO or Ag nanowire and a display device such as an LCD.
本発明の粘着シートに用いられる剥離シートとしては、種々の剥離シートを使用できるが、代表的に剥離性を表面に有するシート材から構成される。シート材としては、ポリエチレンテレフタレート、ポリエチレン、ポリプロピレン、ポリブデン、ポリブタジエン、ポリメチルペンテン、ポリ塩化ビニル、塩化ビニル共重合体、ポリブチレンテレフタレート、ポリウレタン、エチレン−酢酸ビニル共重合体、アイオノマー樹脂、エチレン(メタ)アクリル酸共重合体、ポリスチレン、ポリカーボネート、フッ素樹脂、低密度ポリエチレン、直鎖低密度ポリエチレン、トリアセチルセルロース等の樹脂フィルムや、上質紙、コート紙、グラシン紙、ラミネート紙などが挙げられる。 Although various release sheets can be used as the release sheet used in the pressure-sensitive adhesive sheet of the present invention, it is typically composed of a sheet material having peelability on the surface. Sheet materials include polyethylene terephthalate, polyethylene, polypropylene, polybutene, polybutadiene, polymethylpentene, polyvinyl chloride, vinyl chloride copolymer, polybutylene terephthalate, polyurethane, ethylene-vinyl acetate copolymer, ionomer resin, ethylene (meta ) Acrylic acid copolymer, polystyrene, polycarbonate, fluororesin, low density polyethylene, linear low density polyethylene, triacetyl cellulose resin film, fine paper, coated paper, glassine paper, laminated paper, and the like.
剥離シート用のシート材の表面に剥離性を持たせるには、シート材の表面にフッ素系樹脂、シリコーン系樹脂、長鎖アルキル基含有カルバメート等の剥離剤を塗布により付着させる。
剥離シート用基材フィルムの厚さは、5μm〜300μmが好ましく、10μm〜200μmがより好ましい。剥離シート用基材フィルムとしてポリエチレンテレフタレート系フィルムを用いる場合は、10μm〜100μmが特に好ましい。
In order to make the surface of the sheet material for the release sheet have releasability, a release agent such as a fluororesin, a silicone resin, or a long chain alkyl group-containing carbamate is attached to the surface of the sheet material by coating.
The thickness of the base film for release sheet is preferably 5 μm to 300 μm, and more preferably 10 μm to 200 μm. When a polyethylene terephthalate film is used as the base film for the release sheet, 10 μm to 100 μm is particularly preferable.
本発明の粘着剤を剥離シートに塗工する方法としては、グラビアコート法、バーコート法、スプレーコート法、スピンコート法、ロールコート法、ダイコート法、ナイフコート法、エアナイフコート法、カーテンコート法などの従来公知の方法を用いて、粘着剤含有組成物を塗布する方法が挙げられる。粘着剤含有組成物を塗布した後、溶剤や低沸点成分の残留を防ぐために、80℃〜150℃程度の温度で30秒〜5分間程度加熱することにより、粘着性が発現する。 As a method for applying the adhesive of the present invention to a release sheet, gravure coating method, bar coating method, spray coating method, spin coating method, roll coating method, die coating method, knife coating method, air knife coating method, curtain coating method The method of apply | coating an adhesive containing composition using conventionally well-known methods, such as these, is mentioned. After applying the pressure-sensitive adhesive-containing composition, in order to prevent the solvent and low boiling point components from remaining, heating is performed at a temperature of about 80 ° C. to 150 ° C. for about 30 seconds to 5 minutes.
塗布装置としては、特に制限無く、公知のものを使用できる。乾燥後の塗布量は、1〜100g/m2の範囲が好ましく、5〜50g/m2の範囲がより好ましく、10〜30g/m2の範囲が特に好ましい。1g/m2以上とすることにより十分な粘着性能が得られ、100g/m2以下とすることにより粘着剤層がはみ出すのを防止する。 As a coating apparatus, a well-known thing can be used without a restriction | limiting in particular. Coating amount after drying is preferably in the range of 1 to 100 g / m 2, more preferably in the range of 5 to 50 g / m 2, the range of 10 to 30 g / m 2 is particularly preferred. Adhesive performance sufficient by setting it as 1 g / m < 2 > or more is obtained, and it prevents that an adhesive layer protrudes by setting it as 100 g / m < 2 > or less.
基材フィルム無し両面粘着シートの形態とする場合には、2枚の剥離シートが必要となる。剥離シートに塗工された粘着剤層にもう一枚の剥離シートを貼り合わせて積層体とする。その際には、それぞれの剥離シートの剥離力に差をつけておくことが好ましい。剥離力に差をつけておけば、軽剥離シート側のみを剥がす際に、粘着剤層が重剥離シート側から浮くおそれや、双方の剥離シートに追従しようとして粘着剤層が引き伸ばされて変形するおそれを防ぐことができる。
もしくは、両面に剥離剤を塗布した剥離シートの一方の面に粘着剤層を塗工した後、それをロール状に巻いてもよい。
In the case of a double-sided pressure-sensitive adhesive sheet without a base film, two release sheets are required. Another release sheet is bonded to the adhesive layer coated on the release sheet to form a laminate. In that case, it is preferable to make a difference in the peeling force of each release sheet. If there is a difference in the peel force, when peeling only the light release sheet side, the adhesive layer may float from the heavy release sheet side, or the adhesive layer will stretch and deform to follow both release sheets Fear can be prevented.
Alternatively, after the pressure-sensitive adhesive layer is applied to one surface of a release sheet having a release agent applied on both sides, it may be wound into a roll.
本発明は、基材フィルムと上記粘着剤からなる基材フィルム付きの粘着シートの形態としてもよい。粘着シートの形態としては粘着剤層が基材フィルムの両面に塗工された基材フィルム付き両面粘着シートの形態としてもよいし、一方の面に塗工された基材フィルム付き片面粘着シートの形態としてもよい。 This invention is good also as a form of an adhesive sheet with a base film which consists of a base film and the said adhesive. As a form of the pressure-sensitive adhesive sheet, a pressure-sensitive adhesive layer may be in the form of a double-sided pressure-sensitive adhesive sheet with a base film coated on both sides of the base film, or a single-sided pressure-sensitive adhesive sheet with a base film coated on one side It is good also as a form.
本発明の基材フィルム付き両面粘着シートまたは基材フィルム付き片面粘着シートに用いられる基材としては、ポリエチレンテレフタレート、ポリエチレンナフタレート、ポリイミド、ポリエーテルイミド、ポリアラミド、ポリエーテルケトン、ポリエーテルエーテルケトン、ポリフェニレンサルフィド、ポリ(4−メチルペンテン−1)ポリエチレン、ポリプロピレン、ポリブテン、ポリブタジエン、ポリメチルペンテン、ポリ塩化ビニル、塩化ビニル共重合体、ポリエチレンテレフタレート、ポリウレタン、エチレン−酢酸ビニル共重合体、アイオノマー樹脂、エチレン(メタ)アクリル酸共重合体、ポリスチレン、ポリカーボネート、フッ素樹脂、低密度ポリエチレン、直鎖低密度ポリエチレン、トリアセチルセルロース、ポリメチルメタクリレート等の樹脂フィルムやそれらの樹脂フィルムの表面に易接着層を積層したフィルム、それらの樹脂フィルムで発泡構造を有するフィルム、上質紙、コート紙、グラシン紙、ラミネート紙等の紙基材が挙げられる。 As a base material used for a double-sided pressure-sensitive adhesive sheet with a base film or a single-sided pressure-sensitive adhesive sheet with a base film of the present invention, polyethylene terephthalate, polyethylene naphthalate, polyimide, polyetherimide, polyaramid, polyetherketone, polyetheretherketone, Polyphenylene sulfide, poly (4-methylpentene-1) polyethylene, polypropylene, polybutene, polybutadiene, polymethylpentene, polyvinyl chloride, vinyl chloride copolymer, polyethylene terephthalate, polyurethane, ethylene-vinyl acetate copolymer, ionomer resin , Ethylene (meth) acrylic acid copolymer, polystyrene, polycarbonate, fluororesin, low density polyethylene, linear low density polyethylene, triacetyl cellulose, polymethyl Resin films such as tacrylate, films with an easy-adhesion layer laminated on the surface of those resin films, films having a foamed structure with those resin films, paper substrates such as fine paper, coated paper, glassine paper, and laminated paper It is done.
本発明の基材フィルム付き両面粘着シートまたは基材フィルム付き片面粘着シートに用いられる基材フィルムの厚さは、使用する材料によって多少異なるが、5μm〜300μmが好ましく、10μm〜100μmがより好ましい。 Although the thickness of the base film used for the double-sided pressure-sensitive adhesive sheet with a base film or the single-sided pressure-sensitive adhesive sheet with a base film of the present invention varies somewhat depending on the material used, it is preferably 5 μm to 300 μm, more preferably 10 μm to 100 μm.
基材フィルム付き両面粘着シートの形態とする場合には、剥離シートに塗工された粘着剤層に、基材フィルムを貼り合わせて積層体とし、別の剥離シートに塗工された粘着剤層と前記積層体の基材フィルムとを貼り合わせて積層体とする。または、一方の剥離シートを剥離した基材フィルム無し両面粘着シートを、基材フィルムの両面に貼り合わせて積層体とする。または、基材フィルムの両面に粘着剤含有組成物を直接塗布し、剥離シートを貼り合わせて積層体とする。もしくは基材フィルムの一方の面に基材フィルム無し両面粘着シートを貼り合わせ、他方の面に粘着剤含有組成物を直接塗布して積層体とする。 In the case of the form of a double-sided pressure-sensitive adhesive sheet with a base film, a pressure-sensitive adhesive layer applied to another release sheet by laminating a base film on the pressure-sensitive adhesive layer applied to the release sheet And a substrate film of the laminate are laminated to form a laminate. Or the double-sided adhesive sheet without a base film which peeled one peeling sheet is bonded together on both surfaces of a base film, and it is set as a laminated body. Alternatively, the pressure-sensitive adhesive-containing composition is directly applied to both surfaces of the base film, and a release sheet is bonded to form a laminate. Alternatively, a double-sided pressure-sensitive adhesive sheet without a base film is bonded to one surface of the base film, and the pressure-sensitive adhesive-containing composition is directly applied to the other surface to obtain a laminate.
基材フィルム付き片面粘着シートの形態とする場合には、剥離シートに塗工された粘着剤層に、基材フィルムを貼り合わせて積層体とする。または、基材フィルムの一方の面に、一方の剥離シートのみ除去した基材無し両面粘着シートを貼り合わせて積層体とする。もしくは、基材フィルムの一方の面に粘着剤含有組成物を直接塗布し、剥離シートを貼り合わせて積層体とする。
基材フィルムの両面もしくは一方の面に粘着剤含有組成物を直接塗布する方法としては、粘着剤を剥離シートに塗工する方法と同様、従来公知の方法が挙げられる。
When setting it as the form of the single-sided adhesive sheet with a base film, it laminates | stacks a base film on the adhesive layer coated on the peeling sheet. Alternatively, a substrate-less double-sided pressure-sensitive adhesive sheet from which only one release sheet is removed is bonded to one surface of the substrate film to obtain a laminate. Alternatively, the pressure-sensitive adhesive-containing composition is directly applied to one surface of the base film, and a release sheet is bonded to form a laminate.
As a method of directly applying the pressure-sensitive adhesive-containing composition to both surfaces or one surface of the base film, a conventionally known method can be used as in the method of applying the pressure-sensitive adhesive to the release sheet.
本発明の導電膜貼付用粘着シートにおいて、貼付対象の導電膜の素材としては特に限定されないが、銀、銅、金、白金、酸化インジウム、酸化亜鉛、酸化スズ、酸化チタン、スズ添加酸化インジウム(ITO)、酸化インジウム・酸化亜鉛(IZO)、ガリウム添加酸化亜鉛(GZO)、アンチモンドープ酸化スズ(ATO)などが挙げられ、特にITOが好ましい。ITOとは、酸化インジウム(III)の結晶構造において一部のインジウム原子がスズ原子に置換した金属酸化物を指す。
ポリエチレンテレフタレートフィルムの表面にITOがドライコーティングされた透明導電性フィルムは、コストダウンや搭載機器の軽薄化という面で優位である。これらの要素が求められる携帯電話・スマートフォン用タッチパネル、特に投影型静電容量式タッチパネルについては、本発明の導電膜貼付用粘着シートを表面にITOを有するポリエチレンテレフタレートフィルムに貼付したものを部材として用いることが好ましい。
In the pressure-sensitive adhesive sheet for attaching a conductive film of the present invention, the material of the conductive film to be attached is not particularly limited, but silver, copper, gold, platinum, indium oxide, zinc oxide, tin oxide, titanium oxide, tin-added indium oxide ( ITO), indium oxide / zinc oxide (IZO), gallium-doped zinc oxide (GZO), antimony-doped tin oxide (ATO), and the like, and ITO is particularly preferable. ITO refers to a metal oxide in which some indium atoms are substituted with tin atoms in the crystal structure of indium (III) oxide.
A transparent conductive film obtained by dry-coating ITO on the surface of a polyethylene terephthalate film is advantageous in terms of reducing costs and reducing the thickness of mounted equipment. For touch panels for mobile phones and smartphones where these elements are required, especially projection-type capacitive touch panels, the adhesive sheet for applying a conductive film of the present invention attached to a polyethylene terephthalate film having ITO on the surface is used as a member. It is preferable.
本発明の導電膜貼付用粘着シートにおいて、貼付対象の導電膜としては特に限定されないが、高精度な位置検出が可能なことから透明タッチパネルに多用されるため、貼付対象の導電膜が高い可視光透過性を有していることが好ましい。 In the pressure-sensitive adhesive sheet for attaching a conductive film of the present invention, the conductive film to be applied is not particularly limited. However, since the position detection with high accuracy is possible, the conductive film to be applied is highly visible light. It preferably has transparency.
本発明の導電膜貼付用粘着シートは、含水率が低い粘着剤から構成されており、高温高湿の環境下においても貼付対象の導電膜の電気抵抗率を増加させないことから、タッチパネルの部材として使用されることが好ましい。
またタッチパネルには、抵抗膜方式、表面弾性波方式、赤外線方式、電磁誘導方式、静電容量方式等があるが、静電容量方式は画面などにタッチした際の電気容量の変化を検知することによってデバイスを作動させる方式であり、透明導電膜の四隅に流れる微弱な電流変化を表示装置が計算処理し、接触位置の検出を行う。このような原理から、静電容量方式タッチパネルは、透明導電膜のわずかな電気抵抗率の変化が精度の低下につながり、結果として故障の原因となる。本発明の導電膜貼付用粘着シートは、高温高湿の環境下においても貼付対象の導電膜の電気抵抗率を増加させないことから、特に静電容量方式のタッチパネルの部材として使用されることが好ましい。
静電容量式のタッチパネルは表面型と投影型があるが、本発明の導電膜貼付用粘着シートはどちらに用いてもよい。
The pressure-sensitive adhesive sheet for attaching a conductive film of the present invention is composed of a pressure-sensitive adhesive having a low water content, and does not increase the electrical resistivity of the conductive film to be attached even in a high-temperature and high-humidity environment. It is preferably used.
In addition, the touch panel includes a resistive film method, surface acoustic wave method, infrared method, electromagnetic induction method, capacitance method, etc. The capacitance method detects changes in capacitance when touching the screen. The display device calculates the weak current flowing in the four corners of the transparent conductive film, and detects the contact position. From such a principle, in the capacitive touch panel, a slight change in electrical resistivity of the transparent conductive film leads to a decrease in accuracy, resulting in a failure. The pressure-sensitive adhesive sheet for attaching a conductive film of the present invention does not increase the electrical resistivity of the conductive film to be attached even in a high-temperature and high-humidity environment, so that it is particularly preferably used as a member for a capacitive touch panel. .
Capacitive touch panels include a surface type and a projection type, but the adhesive sheet for attaching a conductive film of the present invention may be used for either.
以下、実施例により本発明をさらに具体的に説明するが、本発明は以下の実施例に限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention further more concretely, this invention is not limited to a following example.
(実施例1)
アクリル酸エステル共重合体(2−エチルヘキシルアクリレート:シクロヘキシルアクリレート:2−ヒドロキシエチルアクリレート(質量部)=59.7:40:0.3、質量平均分子量80万、濃度40%)溶液の100質量部に、イソシアネート系架橋剤(東洋インキ社製、製品名「BHS−8515」、濃度37.5%)0.5質量部(アクリル系共重合体固形分100質量部に対して架橋剤固形分0.47質量部)を混合して調製したアクリル系粘着剤溶液を、乾燥後の膜厚が25μmになるように重剥離シート(リンテック社製、製品名「SP−PET3811」)に塗布し、120℃で2分間加熱後、軽剥離シート(リンテック社製、製品名「SP−PET3801」)を粘着剤面に貼り合せて、基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
Example 1
100 parts by mass of acrylic acid ester copolymer (2-ethylhexyl acrylate: cyclohexyl acrylate: 2-hydroxyethyl acrylate (mass part) = 59.7: 40: 0.3, mass average molecular weight 800,000, concentration 40%) 0.5 parts by mass of an isocyanate-based crosslinking agent (product name “BHS-8515”, concentration 37.5%, manufactured by Toyo Ink Co., Ltd.) (crosslinker solid content 0 with respect to 100 parts by mass of acrylic copolymer solid content) .47 parts by mass) was applied to a heavy release sheet (product name “SP-PET3811” manufactured by Lintec Corporation) so that the film thickness after drying was 25 μm, and 120 After heating at ℃ for 2 minutes, a light release sheet (product name “SP-PET3801” manufactured by Lintec Co., Ltd.) is bonded to the adhesive surface to obtain a double-sided adhesive sheet without a substrate. And a conductive film stuck adhesive sheet for this.
(実施例2)
実施例1記載のアクリル系粘着剤溶液に代えて、アクリル酸エステル共重合体(ブチルアクリレート:2,2,2−トリフルオロエチルメタクリレート、:2−ヒドロキシエチルアクリレート(質量部)=87:10:3、質量平均分子量70万、濃度26.7%)溶液の100質量部に、イソシアネート系架橋剤(東洋インキ社製、製品名「BHS−8515」、濃度37.5%)2質量部(アクリル系共重合体固形分100質量部に対して架橋剤固形分2.81質量部)を混合して調製したフッ素含有アクリル系粘着剤溶液を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
(Example 2)
Instead of the acrylic pressure-sensitive adhesive solution described in Example 1, an acrylic ester copolymer (butyl acrylate: 2,2,2-trifluoroethyl methacrylate,: 2-hydroxyethyl acrylate (parts by mass) = 87: 10: 3. To 100 parts by mass of a solution having a mass average molecular weight of 700,000 and a concentration of 26.7%), 2 parts by mass of an isocyanate-based crosslinking agent (product name “BHS-8515”, concentration: 37.5%, manufactured by Toyo Ink Co., Ltd.) In the same manner as in Example 1, except that a fluorine-containing acrylic pressure-sensitive adhesive solution prepared by mixing 100 parts by mass of the solid content of the copolymer and 2.81 parts by mass of the solid content of the crosslinking agent was used. A material-free double-sided PSA sheet was obtained and used as a PSA sheet for attaching a conductive film.
(実施例3)
実施例1記載のアクリル系粘着剤溶液に代えて、ポリイソブチレン系樹脂(BASF社製、製品名Oppanol B50、質量平均分子量34万)100質量部に対して、ポリイソブチレン系樹脂(BASF社製、製品名Oppanol B30、質量平均分子量20万)75質量部と水素化石油樹脂(荒川化学工業社製、製品名アルコンP−100)52.5質量部を混合して調製したゴム系粘着剤溶液を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
(Example 3)
Instead of the acrylic pressure-sensitive adhesive solution described in Example 1, polyisobutylene-based resin (manufactured by BASF, product name Oppanol B50, mass average molecular weight 340,000) per 100 parts by mass, polyisobutylene-based resin (manufactured by BASF, A rubber-based pressure-sensitive adhesive solution prepared by mixing 75 parts by mass of product name Opanol B30, mass average molecular weight 200,000) and 52.5 parts by mass of hydrogenated petroleum resin (product name Alcon P-100, manufactured by Arakawa Chemical Industries, Ltd.) Except having used, the base-material-free double-sided adhesive sheet was obtained by the method similar to Example 1, and this was used as the adhesive sheet for electrically conductive film sticking.
(実施例4)
実施例1記載のアクリル系粘着剤溶液に代えて、ポリイソブチレン系樹脂(BASF社製、製品名Oppanol B50、質量平均分子量34万)100質量部に対して、ポリイソブチレン系樹脂(BASF社製、製品名Oppanol B30、質量平均分子量20万)25質量部と水素化石油樹脂(荒川化学工業社製、製品名アルコンP−100)25質量部を混合して調製したゴム系粘着剤溶液を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
Example 4
Instead of the acrylic pressure-sensitive adhesive solution described in Example 1, polyisobutylene-based resin (manufactured by BASF, product name Oppanol B50, mass average molecular weight 340,000) per 100 parts by mass, polyisobutylene-based resin (manufactured by BASF, A rubber-based pressure-sensitive adhesive solution prepared by mixing 25 parts by mass of product name Oppanol B30, mass average molecular weight 200,000) and 25 parts by mass of hydrogenated petroleum resin (manufactured by Arakawa Chemical Industries, Ltd., product name Alcon P-100) was used. Except for this, a double-sided adhesive sheet without a substrate was obtained in the same manner as in Example 1, and this was used as an adhesive sheet for attaching a conductive film.
(比較例1)
実施例1記載のアクリル系粘着剤溶液に代えて、アクリル酸エステル共重合体(ブチルアクリレート:メチルアクリレート:アクリル酸(質量部)=77:20:3、質量平均分子量80万、濃度28%)溶液の100質量部に、イソシアネート系架橋剤(東洋インキ社製、製品名「BHS−8515」、濃度37.5%)1.75質量部(アクリル系共重合体固形分100質量部に対して架橋剤固形分2.34質量部)とアルミキレート系架橋剤(綜研化学社製、製品名「M−5A」、濃度4.95%)1.75質量部(アクリル系共重合体固形分100質量部に対して架橋剤固形分0.31質量部)を混合して調製したアクリル系粘着剤溶液を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
(Comparative Example 1)
Instead of the acrylic pressure-sensitive adhesive solution described in Example 1, an acrylic ester copolymer (butyl acrylate: methyl acrylate: acrylic acid (parts by mass) = 77: 20: 3, mass average molecular weight 800,000, concentration 28%) To 100 parts by mass of the solution, 1.75 parts by mass of an isocyanate-based crosslinking agent (product name “BHS-8515”, concentration 37.5%, manufactured by Toyo Ink Co., Ltd.) (based on 100 parts by mass of the acrylic copolymer solid content) Crosslinker solid content 2.34 parts by mass) and aluminum chelate crosslinker (manufactured by Soken Chemical Co., Ltd., product name “M-5A”, concentration 4.95%) 1.75 parts by mass (acrylic copolymer solid content 100) A double-sided pressure-sensitive adhesive sheet without a substrate was obtained in the same manner as in Example 1 except that an acrylic pressure-sensitive adhesive solution prepared by mixing 0.31 parts by mass of a crosslinking agent with respect to mass parts was used, This is attached to the conductive film It was a pressure-sensitive adhesive sheet.
(比較例2)
実施例1記載のアクリル系粘着剤溶液に代えて、アクリル酸エステル共重合体(ブチルアクリレート:エチルアクリレート:アクリル酸(質量部)=77:20:3、質量平均分子量90万、濃度30%)溶液の100質量部に、アルミキレート系架橋剤(綜研化学社製、製品名「M−5A」、濃度4.95%)4質量部(アクリル系共重合体固形分100質量部に対して架橋剤固形分0.66質量部)を混合して調製したアクリル系粘着剤溶液を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
(Comparative Example 2)
Instead of the acrylic pressure-sensitive adhesive solution described in Example 1, an acrylic ester copolymer (butyl acrylate: ethyl acrylate: acrylic acid (parts by mass) = 77: 20: 3, mass average molecular weight 900,000, concentration 30%) To 100 parts by mass of the solution, 4 parts by mass of an aluminum chelate-based crosslinking agent (manufactured by Soken Chemical Co., Ltd., product name “M-5A”, concentration 4.95%) (solid content of acrylic copolymer 100 parts by mass) Except that an acrylic pressure-sensitive adhesive solution prepared by mixing an agent solid content (0.66 parts by mass) was used to obtain a double-sided pressure-sensitive adhesive sheet without a base material in the same manner as in Example 1, and this was used for attaching a conductive film. An adhesive sheet was obtained.
(比較例3)
実施例1記載のアクリル系粘着剤溶液に代えて、アクリル酸エステル共重合体(ブチルアクリレート:メチルアクリレート:4−ヒドロキシブチルアクリレート(質量部)=79:20:1、質量平均分子量90万、濃度30%)溶液の100質量部に、イソシアネート系架橋剤(綜研化学社製、製品名「TD−75」、濃度75%)0.05質量部(アクリル系共重合体固形分100質量部に対して架橋剤固形分0.13質量部)を混合して調製したアクリル系粘着剤溶液を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
(Comparative Example 3)
Instead of the acrylic pressure-sensitive adhesive solution described in Example 1, an acrylic ester copolymer (butyl acrylate: methyl acrylate: 4-hydroxybutyl acrylate (part by mass) = 79: 20: 1, mass average molecular weight 900,000, concentration 30%) To 100 parts by mass of the solution, 0.05 mass parts (based on 100 mass parts of acrylic copolymer solid content), an isocyanate-based crosslinking agent (manufactured by Soken Chemical Co., Ltd., product name "TD-75", concentration 75%) In the same manner as in Example 1 except that an acrylic pressure-sensitive adhesive solution prepared by mixing 0.13 parts by mass of a crosslinking agent solid content was used, a baseless double-sided pressure-sensitive adhesive sheet was obtained in the same manner as in Example 1, and this was electrically conductive film. It was set as the adhesive sheet for sticking.
(比較例4)
実施例1記載のアクリル系粘着剤溶液に代えて、アクリル酸エステル共重合体(ブチルアクリレート:メチルアクリレート:アクリルアミド:2−ヒドロキシエチルアクリレート(質量部)=68.5:30:1:0.5、質量平均分子量90万、濃度29%)溶液の100質量部に、イソシアネート系架橋剤(綜研化学社製、製品名「TD−75」、濃度75%)0.05質量部(アクリル系共重合体固形分100質量部に対して架橋剤固形分0.13質量部)を混合して調製したアクリル系粘着剤溶液を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
(Comparative Example 4)
Instead of the acrylic pressure-sensitive adhesive solution described in Example 1, an acrylic ester copolymer (butyl acrylate: methyl acrylate: acrylamide: 2-hydroxyethyl acrylate (parts by mass) = 68.5: 30: 1: 0.5 , Mass average molecular weight 900,000, concentration 29%) to 100 parts by mass of an isocyanate crosslinking agent (manufactured by Soken Chemical Co., Ltd., product name “TD-75”, concentration 75%) 0.05 part by mass (acrylic copolymer) Double-sided pressure-sensitive adhesive sheet without a substrate in the same manner as in Example 1 except that an acrylic pressure-sensitive adhesive solution prepared by mixing 0.13 parts by mass of a crosslinking agent solid content with 100 parts by mass of the combined solid content was used. This was made into the adhesive sheet for electrically conductive film sticking.
(比較例5)
実施例1記載のアクリル系粘着剤溶液に代えて、アクリル酸エステル共重合体(ブチルアクリレート:イソブチルアクリレート:アクリル酸(質量部)=49.125:49.125:1.75、質量平均分子量50万、濃度32%)溶液の100質量部に、イソシアネート系架橋剤(東洋インキ社製、製品名「BHS−8515」、濃度37.5%)3質量部(アクリル系共重合体固形分100質量部に対して架橋剤固形分3.52質量部)を混合して調製したアクリル系粘着剤溶液を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
(Comparative Example 5)
Instead of the acrylic pressure-sensitive adhesive solution described in Example 1, an acrylic ester copolymer (butyl acrylate: isobutyl acrylate: acrylic acid (parts by mass) = 49.125: 49.125: 1.75, mass average molecular weight 50 Ten parts by weight of an isocyanate-based crosslinking agent (manufactured by Toyo Ink Co., Ltd., product name “BHS-8515”, concentration: 37.5%) 3 parts by weight (100% by weight of acrylic copolymer solids) A baseless double-sided pressure-sensitive adhesive sheet was obtained in the same manner as in Example 1 except that an acrylic pressure-sensitive adhesive solution prepared by mixing 3.52 parts by mass of a crosslinking agent with respect to the part was used. Was used as an adhesive sheet for attaching a conductive film.
(比較例6)
実施例1記載のアクリル系粘着剤溶液に代えて、シリコーン系粘着剤(東レダウコーニング社製、製品名「SD−4580」)の100質量部に、白金触媒(東レダウコーニング社製、製品名「SRX−212」)0.9質量部を混合して調製した粘着剤溶液を使用した。また実施例1記載の重剥離シートに代えてフッ素系重剥離シート(リンテック社製、製品名「PET50FD」)、軽剥離シートに代えて、フッ素系軽剥離シート(藤森工業社製、製品名「フィルムバイナ50YS−E」)を使用したこと以外は実施例1と同様の方法で基材無し両面粘着シートを得て、これを導電膜貼付用粘着シートとした。
(Comparative Example 6)
Instead of the acrylic adhesive solution described in Example 1, 100 parts by mass of a silicone adhesive (product name “SD-4580” manufactured by Toray Dow Corning Co., Ltd.) was added to a platinum catalyst (product name manufactured by Toray Dow Corning Co., Ltd.). “SRX-212”) A pressure-sensitive adhesive solution prepared by mixing 0.9 parts by mass was used. Further, instead of the heavy release sheet described in Example 1, a fluorine-based heavy release sheet (product name “PET50FD” manufactured by Lintec Corporation) and a light release sheet instead of a fluorine-based light release sheet (manufactured by Fujimori Kogyo Co., Ltd., product name “ Except for using the film binder 50YS-E "), a double-sided adhesive sheet without a substrate was obtained in the same manner as in Example 1, and this was used as an adhesive sheet for attaching a conductive film.
実施例1〜4及び比較例1〜6で得られた基材無し両面粘着シートを、以下の試験方法で測定し、結果を表1に示した。
(1) 電気抵抗値
図4を用いて、電気抵抗値測定試験に用いられる抵抗値測定サンプルを説明する。スパッタによりITO膜12を表面上に設けたポリエチレンテレフタレートフィルム13を用意し、ポリエチレンテレフタレートフィルム13のITO膜12が設けられていない側とガラス板15を接合テープ14(リンテック社製、製品名「タックライナーTL−70」)を介して接合した。次にITO膜12面上に銀を含有した導電性樹脂材料(藤倉化成社製、製品名「FA−301CA」ドータイトタッチパネル回路タイプ)を塗布し、80℃で20分間加熱乾燥させて、抵抗値の測定点となる電極11を2点作製した。その際2点間の距離は2cmとなるようにその位置を調整した。そこで実施例および比較例で得られた基材無し両面粘着シートの軽剥離シートを剥離し、基材10としてポリエチレンテレフタレートフィルム(東洋紡績社製、「PET50−A4100」、厚み50μm)を貼付し、本発明における基材フィルム付き片面粘着シートの形態とした導電膜貼付用粘着シートを作製した。得られた導電膜貼付用粘着シートを20mm×250mmの大きさに裁断し、導電膜貼付用粘着シートの重剥離シートを剥離し、粘着剤層7が電極11の2点の際に沿うように(ギリギリ接しないように)ITO12膜スパッタ面に貼付し、図4の抵抗値測定用サンプルを作製した。次に、図5に示されるように、デジタルハイテスタ(日置電機社製、「3802−50」)を用いて、電極11間の初期抵抗値R0を測定した。抵抗値測定サンプルを温度60℃、湿度90%の環境下に240時間放置した後、湿熱促進後抵抗値Rを測定した。抵抗値増加率は以下のように算出した。
抵抗値増加率(%)=(R−R0)/R0x100
(2) 含水率
実施例および比較例で得られた基材無し両面粘着シートの形態とした導電膜貼付用粘着シートの軽剥離シートと重剥離シートをそれぞれ剥離して得られた粘着剤100mgを23℃、50%相対湿度で24時間調湿し、カールフィッシャー水分計(京都電子工業社製、装置名「MKC−510N」)を用いて測定した。設定加熱温度を200℃、試薬は発生液としてリーデル・デ・ハーン社製、製品名「クーロマットAG−Oven」、対極液としてリーデル・デ・ハーン社製、製品名「クーロマットCG」をそれぞれ使用した。
The baseless double-sided PSA sheets obtained in Examples 1 to 4 and Comparative Examples 1 to 6 were measured by the following test methods, and the results are shown in Table 1.
(1) Electrical Resistance Value A resistance value measurement sample used in an electrical resistance value measurement test will be described with reference to FIG. A
Resistance value increase rate (%) = (R−R 0 ) / R 0 x100
(2) Moisture content Adhesive 100 mg obtained by peeling off the light release sheet and the heavy release sheet of the adhesive sheet for attaching a conductive film in the form of a baseless double-sided adhesive sheet obtained in Examples and Comparative Examples, respectively. The humidity was adjusted at 23 ° C. and 50% relative humidity for 24 hours, and the measurement was performed using a Karl Fischer moisture meter (manufactured by Kyoto Electronics Industry Co., Ltd., apparatus name “MKC-510N”). The set heating temperature was 200 ° C., the reagent used was Riedel de Haan, product name “Curomat AG-Oven” as the generation solution, and Riedel de Haan, product name “Curomat CG” was used as the counter electrode solution. .
表1に示すとおり、カールフィッシャー法による含水率が0〜0.2%である本発明の導電膜貼付用粘着剤を用いた実施例1〜4は、比較例1〜6に比べて抵抗値増加率が低かった。 As shown in Table 1, Examples 1-4 using the adhesive for electrically conductive film sticking of the present invention whose moisture content by Karl Fischer method is 0-0.2% are resistance values compared with comparative examples 1-6. The rate of increase was low.
1 ハードコート層
2 樹脂フィルム層
3 化粧印刷層
4 埋め込み用粘着剤層
5 ガラス層
6 透明導電膜
7 粘着剤層
8 表示装置
9 剥離シート
10 基材
11 電極
12 ITO膜
13 ポリエチレンテレフタレートフィルム
14 接合テープ
15 ガラス板
DESCRIPTION OF SYMBOLS 1
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WO2012018142A1 (en) * | 2010-08-04 | 2012-02-09 | リンテック株式会社 | Adhesive for crystalline metal oxide conducting film and adhesive sheet for crystalline metal oxide conducting film using the same |
KR20140060265A (en) * | 2011-06-28 | 2014-05-19 | 린텍 가부시키가이샤 | Adhesive composition and adhesive sheet |
KR101271470B1 (en) * | 2011-08-08 | 2013-06-05 | 도레이첨단소재 주식회사 | Dielectric adhesive film for flexible display device with electronic paper |
KR101385040B1 (en) | 2011-10-11 | 2014-04-14 | 제일모직주식회사 | Adhesive Composition, Adhesive Film Comprising the Same, Method for Preparing the Adhesive Film and Display Member Using the Same |
KR101385038B1 (en) | 2011-10-11 | 2014-04-14 | 제일모직주식회사 | Adhesive Composition, Adhesive Film Comprising the Same, Method for Preparing the Adhesive Film and Display Member Using the Same |
WO2013055015A1 (en) * | 2011-10-11 | 2013-04-18 | 제일모직 주식회사 | Adhesive composition, adhesive film, production method for same and display member using same |
KR101385042B1 (en) | 2011-12-30 | 2014-04-15 | 제일모직주식회사 | Adhesive Composition, Adhesive Film Comprising the Same, Method for Preparing the Adhesive Film and Display Member Using the Same |
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