JP2010163477A - 粘着シート - Google Patents
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- Publication number
- JP2010163477A JP2010163477A JP2009004464A JP2009004464A JP2010163477A JP 2010163477 A JP2010163477 A JP 2010163477A JP 2009004464 A JP2009004464 A JP 2009004464A JP 2009004464 A JP2009004464 A JP 2009004464A JP 2010163477 A JP2010163477 A JP 2010163477A
- Authority
- JP
- Japan
- Prior art keywords
- pressure
- sensitive adhesive
- adhesive sheet
- sulfur
- mercaptan
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 195
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 87
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 87
- 239000011593 sulfur Substances 0.000 claims abstract description 87
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 56
- 239000010410 layer Substances 0.000 claims abstract description 55
- 239000000203 mixture Substances 0.000 claims abstract description 48
- 239000012986 chain transfer agent Substances 0.000 claims abstract description 46
- 238000012360 testing method Methods 0.000 claims abstract description 19
- 239000007789 gas Substances 0.000 claims description 65
- -1 aromatic mercaptans Chemical group 0.000 claims description 57
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 38
- 125000004432 carbon atom Chemical group C* 0.000 claims description 25
- 125000003396 thiol group Chemical group [H]S* 0.000 claims description 14
- 229910052799 carbon Inorganic materials 0.000 claims description 13
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical group S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 claims description 12
- 239000000470 constituent Substances 0.000 claims description 10
- 125000004429 atom Chemical group 0.000 claims description 9
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 7
- 238000009792 diffusion process Methods 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 abstract description 39
- 239000002184 metal Substances 0.000 abstract description 39
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 abstract description 12
- 230000002829 reductive effect Effects 0.000 abstract description 3
- 239000000853 adhesive Substances 0.000 description 63
- 230000001070 adhesive effect Effects 0.000 description 62
- 239000000178 monomer Substances 0.000 description 58
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 57
- 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 42
- 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 42
- 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 42
- 229920005989 resin Polymers 0.000 description 34
- 239000011347 resin Substances 0.000 description 34
- 230000007797 corrosion Effects 0.000 description 30
- 238000005260 corrosion Methods 0.000 description 30
- 239000003431 cross linking reagent Substances 0.000 description 26
- 239000003995 emulsifying agent Substances 0.000 description 25
- 238000000034 method Methods 0.000 description 23
- 125000000217 alkyl group Chemical group 0.000 description 21
- 239000000758 substrate Substances 0.000 description 20
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- 125000003118 aryl group Chemical group 0.000 description 14
- 238000011282 treatment Methods 0.000 description 14
- 238000004132 cross linking Methods 0.000 description 13
- 125000000524 functional group Chemical group 0.000 description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 12
- 238000005516 engineering process Methods 0.000 description 12
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- 230000015572 biosynthetic process Effects 0.000 description 10
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- 150000003505 terpenes Chemical class 0.000 description 10
- 235000007586 terpenes Nutrition 0.000 description 10
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 9
- 239000003505 polymerization initiator Substances 0.000 description 9
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 8
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 description 8
- 230000002401 inhibitory effect Effects 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- 238000003786 synthesis reaction Methods 0.000 description 8
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- 239000012874 anionic emulsifier Substances 0.000 description 7
- 125000000129 anionic group Chemical group 0.000 description 7
- 229910052709 silver Inorganic materials 0.000 description 7
- 238000012546 transfer Methods 0.000 description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 6
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000000123 paper Substances 0.000 description 6
- RMVRSNDYEFQCLF-UHFFFAOYSA-N thiophenol Chemical compound SC1=CC=CC=C1 RMVRSNDYEFQCLF-UHFFFAOYSA-N 0.000 description 6
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 description 5
- 239000013032 Hydrocarbon resin Substances 0.000 description 5
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 5
- 239000000654 additive Substances 0.000 description 5
- 239000012790 adhesive layer Substances 0.000 description 5
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
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- 150000002148 esters Chemical class 0.000 description 5
- 239000000835 fiber Substances 0.000 description 5
- 229920006270 hydrocarbon resin Polymers 0.000 description 5
- 150000002739 metals Chemical class 0.000 description 5
- 239000012875 nonionic emulsifier Substances 0.000 description 5
- 150000002978 peroxides Chemical class 0.000 description 5
- 239000003208 petroleum Substances 0.000 description 5
- 239000005011 phenolic resin Substances 0.000 description 5
- WMXCDAVJEZZYLT-UHFFFAOYSA-N tert-butylthiol Chemical compound CC(C)(C)S WMXCDAVJEZZYLT-UHFFFAOYSA-N 0.000 description 5
- GRWFGVWFFZKLTI-IUCAKERBSA-N (-)-α-pinene Chemical compound CC1=CC[C@@H]2C(C)(C)[C@H]1C2 GRWFGVWFFZKLTI-IUCAKERBSA-N 0.000 description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 4
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 4
- 150000001298 alcohols Chemical class 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000005536 corrosion prevention Methods 0.000 description 4
- 229920001971 elastomer Polymers 0.000 description 4
- 238000005227 gel permeation chromatography Methods 0.000 description 4
- 125000001072 heteroaryl group Chemical group 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000004745 nonwoven fabric Substances 0.000 description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Natural products OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000001252 acrylic acid derivatives Chemical class 0.000 description 3
- 239000003522 acrylic cement Substances 0.000 description 3
- 125000001931 aliphatic group Chemical group 0.000 description 3
- 229920006272 aromatic hydrocarbon resin Polymers 0.000 description 3
- 235000010323 ascorbic acid Nutrition 0.000 description 3
- 229960005070 ascorbic acid Drugs 0.000 description 3
- 239000011668 ascorbic acid Substances 0.000 description 3
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000003480 eluent Substances 0.000 description 3
- 238000010556 emulsion polymerization method Methods 0.000 description 3
- 239000011737 fluorine Substances 0.000 description 3
- 229910052731 fluorine Inorganic materials 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 239000011888 foil Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229930195733 hydrocarbon Natural products 0.000 description 3
- 150000002430 hydrocarbons Chemical class 0.000 description 3
- TYQCGQRIZGCHNB-JLAZNSOCSA-N l-ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(O)=C(O)C1=O TYQCGQRIZGCHNB-JLAZNSOCSA-N 0.000 description 3
- 239000007769 metal material Substances 0.000 description 3
- 239000002985 plastic film Substances 0.000 description 3
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- 239000000243 solution Substances 0.000 description 3
- 150000004670 unsaturated fatty acids Chemical group 0.000 description 3
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 3
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 2
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical compound C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 2
- JLIDVCMBCGBIEY-UHFFFAOYSA-N 1-penten-3-one Chemical compound CCC(=O)C=C JLIDVCMBCGBIEY-UHFFFAOYSA-N 0.000 description 2
- YBYIRNPNPLQARY-UHFFFAOYSA-N 1H-indene Chemical compound C1=CC=C2CC=CC2=C1 YBYIRNPNPLQARY-UHFFFAOYSA-N 0.000 description 2
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 2
- BVYRHLPUAHNHKR-UHFFFAOYSA-N 3-[[1-amino-2-[[1-amino-1-(2-carboxyethylimino)-2-methylpropan-2-yl]diazenyl]-2-methylpropylidene]amino]propanoic acid;hydrate Chemical compound O.OC(=O)CCNC(=N)C(C)(C)N=NC(C)(C)C(=N)NCCC(O)=O BVYRHLPUAHNHKR-UHFFFAOYSA-N 0.000 description 2
- XDQWJFXZTAWJST-UHFFFAOYSA-N 3-triethoxysilylpropyl prop-2-enoate Chemical compound CCO[Si](OCC)(OCC)CCCOC(=O)C=C XDQWJFXZTAWJST-UHFFFAOYSA-N 0.000 description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 description 2
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- OJOWICOBYCXEKR-KRXBUXKQSA-N (5e)-5-ethylidenebicyclo[2.2.1]hept-2-ene Chemical compound C1C2C(=C/C)/CC1C=C2 OJOWICOBYCXEKR-KRXBUXKQSA-N 0.000 description 1
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- NALFRYPTRXKZPN-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane Chemical compound CC1CC(C)(C)CC(OOC(C)(C)C)(OOC(C)(C)C)C1 NALFRYPTRXKZPN-UHFFFAOYSA-N 0.000 description 1
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Images
Classifications
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- H01L24/01—Means for bonding being attached to, or being formed on, the surface to be connected, e.g. chip-to-package, die-attach, "first-level" interconnects; Manufacturing methods related thereto
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- H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
- H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J133/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
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- C09J133/08—Homopolymers or copolymers of acrylic acid esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
- C08F230/04—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal
- C08F230/08—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon
- C08F230/085—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal containing a metal containing silicon the monomer being a polymerisable silane, e.g. (meth)acryloyloxy trialkoxy silanes or vinyl trialkoxysilanes
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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Abstract
【解決手段】本発明により提供される粘着シートは、水分散型粘着剤組成物から形成された粘着剤層を備える。上記粘着剤組成物は、硫黄含有連鎖移動剤を用いて合成された水分散型アクリル系重合体を含む。そして、該粘着シートを85℃で1時間加熱するガス発生試験において、硫黄含有ガスの放散量が、前記シートの面積1cm2当たり、SO4 2−換算で0.043μg以下である。
【選択図】なし
Description
(1)水分散型粘着剤組成物から形成された粘着剤層を備える粘着シートであって、
該粘着剤組成物は、3級メルカプタンおよび芳香族メルカプタンからなる群から選択される少なくとも一種のメルカプタンを用いて合成されたアクリル系重合体を含み、
当該粘着シートを85℃で1時間加熱するガス発生試験において、硫黄含有ガスの放散量が0.043μgSO4 2−/cm2以下である、粘着シート。
(2)硫黄含有連鎖移動剤を用いて合成されたアクリル系重合体を含む水分散型粘着剤組成物であって、
当該組成物を乾燥または硬化させて得られる粘着剤を85℃で1時間加熱するガス発生試験において、該粘着剤1g当たりの硫黄含有ガスの放散量が、SO4 2−換算で2.7μg以下(以下、「2.7μgSO4 2−/g以下」と表すことがある。)である、水分散型粘着剤組成物。
CH2=C(R1)COOR2
(1)
ここで、上記式(1)中のR1は水素原子またはメチル基である。また、R2は炭素原子数1〜20のアルキル基である。R2の具体例としては、メチル基、エチル基、プロピル基、イソプロピル基、ブチル基、イソブチル基、s−ブチル基、t−ブチル基、ペンチル基、イソアミル基、ネオペンチル基、ヘキシル基、ヘプチル基、オクチル基、イソオクチル基、2−エチルヘキシル基、ノニル基、イソノニル基、デシル基、イソデシル基、ウンデシル基、ドデシル基、トリデシル基、テトラデシル基、ペンタデシル基、ヘキサデシル基、ヘプタデシル基、オクタデシル基、ノナデシル基、エイコシル基等のアルキル基が挙げられる。粘着剤の貯蔵弾性率等の観点から、これらのうちR2が炭素原子数2〜14(以下、このような炭素原子数の範囲を「C2−14」と表すことがある。)のアルキル基であるアルキル(メタ)アクリレートが好ましく、R2がC2−10のアルキル基であるアルキル(メタ)アクリレートがより好ましい。特に好ましいR2として、ブチル基および2−エチルヘキシル基が例示される。
水酸基含有モノマー:例えば、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)アクリレート等の、ヒドロキシアルキル(メタ)アクリレート類;ビニルアルコール、アリルアルコール等の、不飽和アルコール類。
アミノ基含有モノマー:例えば、アミノエチル(メタ)アクリレート、N,N−ジメチルアミノエチル(メタ)アクリレート、t−ブチルアミノエチル(メタ)アクリレート。
シアノ基含有モノマー:例えば、アクリロニトリル、メタクリロニトリル。
ケト基含有モノマー:例えば、ジアセトン(メタ)アクリルアミド、ジアセトン(メタ)アクリレート、ビニルメチルケトン、ビニルエチルケトン、アリルアセトアセテート、ビニルアセトアセテート。
硫黄含有連鎖移動剤の実質的に全部が腐食防止型メルカプタンであってもよい。ここに開示される技術において使用する硫黄含有連鎖移動剤に含まれる腐食防止型メルカプタンの種類は、一種類であってもよく、二種類以上であってもよい。例えば、実質的にターシャリーラウリルメルカプタン(複数の構造異性体の混合物であり得る。)からなる連鎖移動剤を好ましく用いることができる。
冷却管、窒素導入管、温度計および攪拌機を備えた反応容器にイオン交換水40部を入れ、窒素ガスを導入しながら60℃で1時間以上攪拌して窒素置換を行った。この反応容器に、2,2’−アゾビス[N−(2−カルボキシエチル)−2−メチルプロピオンアミジン]ハイドレート(重合開始剤)0.1部を加えた。系を60℃に保ちつつ、ここにモノマーエマルションを3時間かけて徐々に滴下して乳化重合反応を進行させた。モノマーエマルションとしては、ブチルアクリレート90部、2−エチルヘキシルアクリレート10部、アクリル酸4部、ターシャリーブチルメルカプタン0.02部、3−メタクリロキシプロピルトリメトキシシラン(信越化学工業株式会社製品、商品名「KBM−503」)0.07部およびポリオキシエチレンラウリル硫酸ナトリウム(乳化剤)2部を、イオン交換水30部に加えて乳化したものを使用した。モノマーエマルションの滴下終了後、さらに3時間60℃に保持し、次いで過酸化水素水0.075部およびアスコルビン酸0.15部を添加した。このようにして水分散型アクリル系重合体を合成した。上記で得られた重合反応液を室温まで冷却した後、10%アンモニア水の添加によりpHを7に調整して、本例に係る水分散型アクリル系粘着剤組成物を得た。
本例では、例1で用いたターシャリーブチルメルカプタンに代えて、ターシャリーラウリルメルカプタン(東京化成工業株式会社製)0.05部を使用した。その他の点については例1と同様にして水分散型アクリル系粘着剤組成物を得、この組成物を用いて例1と同様に両面粘着シートを作製した。
本例では、例1で用いたターシャリーブチルメルカプタンに代えて、フェニルメルカプタン0.03部を使用した。その他の点については例1と同様にして水分散型アクリル系粘着剤組成物を得、この組成物を用いて例1と同様に両面粘着シートを作製した。
本例では、例1で用いたターシャリーブチルメルカプタンに代えて、n−ラウリルメルカプタン0.05部を使用した。その他の点については例1と同様にして水分散型アクリル系粘着剤組成物を得、この組成物を用いて例1と同様に両面粘着シートを作製した。
両面粘着シートの一方の粘着面を覆う剥離ライナーを剥がし、厚さ25μmのポリエチレンテレフタレート(PET)フィルムを貼り付けて裏打ちした。この裏打ちされた粘着シートを幅20mm、長さ100mmのサイズにカットしたものを測定用サンプルとした。上記サンプルの他方の粘着面から剥離ライナーを剥がし、2kgのローラを1往復させてステンレス(SUS:BA304)板に圧着した。これを23℃に30分間保持した後、引張試験機を用い、JIS Z 0237に準拠して、温度23℃、RH50%の測定環境にて引張速度300mm/分の条件で180°引き剥がし粘着力を測定した。
両面粘着シートの一方の面を覆う剥離ライナーを剥がし、厚さ25μmのPETフィルムを貼り付けて裏打ちした。この裏打ちされた粘着シートを幅10mmにカットして試料片を作製した。上記試料片の他方の面から剥離ライナーを剥がし、被着体としてのフェノール樹脂板に幅10mm、長さ20mmの接着面積にて上記試料片を貼り付けた。これを40℃の環境下に30分間放置した後、フェノール樹脂板を垂下し、試料片の自由端に500gの荷重を付与した。JIS Z 0237に準じて、該荷重が付与された状態で40℃の環境下に1時間放置した後における試料片のズレ距離(mm)を測定した。
両粘着面から剥離ライナーを剥がした各粘着シート約0.1gを燃焼装置用試料ボートに載せ、燃焼装置(ダイアインスツルメンツ社製の自動試料燃焼装置、型式「AQF−100」)を用いて85℃で1時間加熱した。このとき粘着シートから発生したガスを10mLの吸収液に通過させた。この吸収液は、純水に30ppmの過酸化水素を含ませたものであって、上記発生ガスに含まれ得る硫黄含有ガス(H2S、SO2等)をSO4 2−に変換して捕集することができる。上記発生ガスを通過させた後の吸収液に純水を加えて20mLの容量に調整し、イオンクロマトグラフ(ダイオネクス社製、商品名「DX−320」)を用いてSO4 2−の定量分析を行うことにより、粘着シート1g当たりSO4 2−発生量を求めた。なお、上記試料ボートが空の状態で同様の操作を行ったものをブランクとした。得られた結果を、各粘着シートの面積当たりのSO4 2−発生量、および、粘着剤1g当たりのSO4 2−発生量に換算した。これらの結果を表1に示す。なお、上記換算には、各例に係る粘着シートの1cm2当たりの質量が0.017gであること、および、各粘着シート1cm2に含まれる粘着剤の質量が0.0156gであることを利用した。
温度:Inlet 85℃、Outlet 85℃
ガス流量:O2 400mL/分、Ar(送水ユニット:目盛0)150mL/分
分離カラム:IonPac AS18(4mm×250mm)
ガードカラム:IonPac AG18(4mm×50mm)
除去システム:ASRS-ULTRA(エクスターナルモード、75mA)
検出器:電気伝導度検出器
溶離液:13mM KOH(0〜20分)
30mM KOH(20〜30分)
(溶離液ジェネレーターEG40を使用)
溶離液流量:1.0mL/分
試料注入量:250μL
両粘着面から剥離ライナーを剥がした各粘着シート(不織布基材およびその両面に設けられた粘着剤層からなる。)約1.0gと、研磨した銀板(銀純度>99.95%、サイズ1mm×10mm×10mm)とを用意した。これらを直接接触しないように容積50mLのスクリュー管に入れ、密閉して85℃に1週間保持した。試験後の銀板を未使用(試験前)の銀板と比較して、腐食発生(金属光沢の消失、着色等の外観変化により判断した。)の有無を目視で確認することにより金属腐食性を評価した。その結果を、腐食が認められた場合には金属腐食性「有」、腐食が認められなかった場合には金属腐食性「無」として表1に示した。
10:基材
21,22:粘着剤層
31,32:剥離ライナー
Claims (6)
- 水分散型粘着剤組成物から形成された粘着剤層を備える粘着シートであって、
該粘着剤組成物は、硫黄を構成原子として含む連鎖移動剤を用いて合成された水分散型アクリル系重合体を含み、
当該粘着シートを85℃で1時間加熱するガス発生試験において、硫黄を構成原子として含むガスの放散量が、前記シートの面積1cm2当たり、SO4 2−換算で0.043μg以下である、粘着シート。 - 前記連鎖移動剤は、前記ガス発生試験において、前記ガスを実質的に発生しない連鎖移動剤である、請求項1に記載の粘着シート。
- 前記連鎖移動剤は、メルカプト基の結合している炭素原子上に水素原子を有しない構造のメルカプタンを主成分とする、請求項1または2に記載の粘着シート。
- 前記メルカプタンは、3級メルカプタンおよび芳香族メルカプタンからなる群から選択される一種または二種以上である、請求項3に記載の粘着シート。
- 基材の両面に前記粘着剤層を備える両面粘着シートとして構成された、請求項1から4のいずれか一項に記載の粘着シート。
- 電子機器の内部で用いられる、請求項1から5のいずれか一項に記載の粘着シート。
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JP2009004464A JP5190384B2 (ja) | 2009-01-13 | 2009-01-13 | 粘着シート |
US12/683,891 US20100178500A1 (en) | 2009-01-13 | 2010-01-07 | Pressure-sensitive adhesive sheet |
EP10150397A EP2206758B1 (en) | 2009-01-13 | 2010-01-11 | Pressure-sensitive adhesive sheet with low emission of sulfur-containing volatile components |
CN201010002196A CN101775258A (zh) | 2009-01-13 | 2010-01-13 | 粘合片 |
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JP2017132993A (ja) * | 2016-01-29 | 2017-08-03 | 日東電工株式会社 | 水性粘着剤組成物およびその利用 |
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TWI510581B (zh) * | 2011-05-27 | 2015-12-01 | Cheil Ind Inc | 黏著劑組成物及使用其之表面保護膜 |
TWI510582B (zh) * | 2011-05-27 | 2015-12-01 | Cheil Ind Inc | 黏著劑組成物及使用其之光學構件 |
US9163167B2 (en) | 2011-06-08 | 2015-10-20 | Cheil Industries, Inc. | Adhesive composition and optical member using the same |
CN102816545B (zh) * | 2011-06-09 | 2015-10-21 | 第一毛织株式会社 | 粘合剂组合物和使用该粘合剂组合物的光学元件 |
MX2017003634A (es) * | 2014-09-22 | 2017-07-13 | Dow Global Technologies Llc | Envoltura de lamina con propiedades adhesivas. |
WO2016179010A1 (en) | 2015-05-01 | 2016-11-10 | Lord Corporation | Adhesive for rubber bonding |
WO2018047919A1 (ja) * | 2016-09-07 | 2018-03-15 | リンテック株式会社 | 接着剤組成物、封止シート、及び封止体 |
CN110527453B (zh) * | 2019-09-10 | 2021-11-19 | 江苏皇冠新材料科技有限公司 | 用于5g天线制程的基于丙烯酸系共聚物的粘合片 |
KR102426905B1 (ko) * | 2020-12-08 | 2022-08-01 | (주)트러스 | 광경화형 점착제와 열발포제를 포함하는 재박리 가능한 점착제 및 이를 포함하는 재박리 가능한 점착테이프 |
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JP5190384B2 (ja) | 2013-04-24 |
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