JP5621592B2 - 熱伝導性感圧接着剤組成物及び熱伝導性感圧接着性シート - Google Patents
熱伝導性感圧接着剤組成物及び熱伝導性感圧接着性シート Download PDFInfo
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- JP5621592B2 JP5621592B2 JP2010517877A JP2010517877A JP5621592B2 JP 5621592 B2 JP5621592 B2 JP 5621592B2 JP 2010517877 A JP2010517877 A JP 2010517877A JP 2010517877 A JP2010517877 A JP 2010517877A JP 5621592 B2 JP5621592 B2 JP 5621592B2
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- 239000003999 initiator Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
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- 229920000592 inorganic polymer Polymers 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 239000012948 isocyanate Substances 0.000 description 1
- 150000002513 isocyanates Chemical class 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
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- 230000014759 maintenance of location Effects 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000005641 methacryl group Chemical group 0.000 description 1
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- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 150000002763 monocarboxylic acids Chemical class 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
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- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 description 1
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- 150000003016 phosphoric acids Chemical class 0.000 description 1
- PMJHHCWVYXUKFD-UHFFFAOYSA-N piperylene Natural products CC=CC=C PMJHHCWVYXUKFD-UHFFFAOYSA-N 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920001490 poly(butyl methacrylate) polymer Polymers 0.000 description 1
- 229920003055 poly(ester-imide) Polymers 0.000 description 1
- 229920001643 poly(ether ketone) Polymers 0.000 description 1
- 229920001483 poly(ethyl methacrylate) polymer Polymers 0.000 description 1
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920001481 poly(stearyl methacrylate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920002312 polyamide-imide Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920000647 polyepoxide Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920001601 polyetherimide Polymers 0.000 description 1
- 229920000120 polyethyl acrylate Polymers 0.000 description 1
- 239000011112 polyethylene naphthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920001195 polyisoprene Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 229920001955 polyphenylene ether Polymers 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 229920001291 polyvinyl halide Polymers 0.000 description 1
- 229920000131 polyvinylidene Polymers 0.000 description 1
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 description 1
- 229940114930 potassium stearate Drugs 0.000 description 1
- MQOCIYICOGDBSG-UHFFFAOYSA-M potassium;hexadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCC([O-])=O MQOCIYICOGDBSG-UHFFFAOYSA-M 0.000 description 1
- ANBFRLKBEIFNQU-UHFFFAOYSA-M potassium;octadecanoate Chemical compound [K+].CCCCCCCCCCCCCCCCCC([O-])=O ANBFRLKBEIFNQU-UHFFFAOYSA-M 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010526 radical polymerization reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- 229940045870 sodium palmitate Drugs 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- GGXKEBACDBNFAF-UHFFFAOYSA-M sodium;hexadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCC([O-])=O GGXKEBACDBNFAF-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 239000011115 styrene butadiene Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 125000000944 sulfenic acid group Chemical group 0.000 description 1
- 125000000626 sulfinic acid group Chemical group 0.000 description 1
- 150000003460 sulfonic acids Chemical class 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 239000003784 tall oil Substances 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 239000004408 titanium dioxide Substances 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
- LDHQCZJRKDOVOX-UHFFFAOYSA-N trans-crotonic acid Natural products CC=CC(O)=O LDHQCZJRKDOVOX-UHFFFAOYSA-N 0.000 description 1
- 150000003918 triazines Chemical class 0.000 description 1
- 125000003866 trichloromethyl group Chemical group ClC(Cl)(Cl)* 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- KOWVWXQNQNCRRS-UHFFFAOYSA-N tris(2,4-dimethylphenyl) phosphate Chemical compound CC1=CC(C)=CC=C1OP(=O)(OC=1C(=CC(C)=CC=1)C)OC1=CC=C(C)C=C1C KOWVWXQNQNCRRS-UHFFFAOYSA-N 0.000 description 1
- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 238000009849 vacuum degassing Methods 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229940098697 zinc laurate Drugs 0.000 description 1
- 229940012185 zinc palmitate Drugs 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
- GPYYEEJOMCKTPR-UHFFFAOYSA-L zinc;dodecanoate Chemical compound [Zn+2].CCCCCCCCCCCC([O-])=O.CCCCCCCCCCCC([O-])=O GPYYEEJOMCKTPR-UHFFFAOYSA-L 0.000 description 1
- GJAPSKMAVXDBIU-UHFFFAOYSA-L zinc;hexadecanoate Chemical compound [Zn+2].CCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCC([O-])=O GJAPSKMAVXDBIU-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
- 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
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Adhesive Tapes (AREA)
- Adhesives Or Adhesive Processes (AREA)
Description
熱伝導性感圧接着剤組成物(E)に燃焼抑制剤(B)、膨張化黒鉛粉(C)及び熱伝導性繊維(D)を含有させることによって、熱伝導性感圧接着剤組成物(E)からなる熱伝導性感圧接着性シート(F)が燃焼する際、膨張化黒鉛粉(C)が膨らんで熱伝導性繊維(D)と絡み合うことで断熱層を形成すると考えられる。さらに燃焼抑制剤(B)によって熱伝導性感圧接着性シート(F)の燃焼速度が抑制されるために断熱層が形成される前に燃焼が広がる事なく、断熱層にて燃焼を防止できる。したがって、熱伝導性感圧接着剤組成物(E)に燃焼抑制剤(B)、膨張化黒鉛粉(C)及び熱伝導性繊維(D)を含有させることで、熱伝導性感圧接着性シート(F)の難燃性を向上させることができる。
重合体(S)を構成するものとしては、ゴム、エラストマー及び樹脂の中から任意に選んだ少なくとも一種を挙げることができる。重合体(S)に、接着性及び/又は粘着性を備えさせるためには、ゴム、エラストマー及び樹脂は、接着性及び/又は粘着性を有するものの中から選ぶことが好ましい。しかしながら、接着性及び/又は粘着性を有しないゴム、エラストマー及び樹脂に、粘接着性付与剤を組み合わせて用いることもできる。
重合体(S)を構成するものとしては、(メタ)アクリル酸エステル重合体(A1)が好ましい。
本発明の熱伝導性感圧接着剤組成物(E)は、(メタ)アクリル酸エステル重合体(A1)に加えて、さらに、(メタ)アクリル酸エステル単量体(A2m)を含有することがより好ましい。本発明の熱伝導性感圧接着剤組成物(E)を成形して、熱伝導性感圧接着性シート(F)とする際に、熱伝導性感圧接着剤組成物(E)中の(メタ)アクリル酸エステル単量体(A2m)は、重合して(メタ)アクリル酸エステル重合体に変換する。
本発明の熱伝導性感圧接着剤組成物(E)には、燃焼抑制剤(B)が含有される。本発明に用いることができる燃焼抑制剤(B)は特に限定されることはなく、有機難燃剤も無機難燃剤も用いることができる。ただし、環境負荷の低減や安全性を考慮したものを用いることが好ましく、そのような観点からは、ハロゲン化物や危険物を除外して、水酸化アルミニウム、水酸化マグネシウム、水酸化カルシウム、2水和石膏、ホウ酸亜鉛、カオリンクレー、アルミン酸カルシウム、炭酸カルシウム、炭酸アルミニウム、ドーソナイト、リン酸エステル、ハイドロタルサイト類、酸化アンチモンなどを挙げることができる。これらの燃焼抑制剤(B)は、一種を単独で使用してもよく、二種以上を併用してもよい。
。
本発明の熱伝導性感圧接着剤組成物(E)には、膨張化黒鉛粉(C)が含有される。本発明に用いることができる膨張化黒鉛粉の例としては、酸処理した黒鉛を500℃〜1200℃にて熱処理して100ml/g〜300ml/gに膨張させ、次いで、粉砕することを含む工程を経て得られたものを挙げることができる。より好ましくは、黒鉛を強酸で処理した後アルカリ中で焼結し、その後再度強酸で処理したものを500℃〜1200℃にて熱処理して、酸を除去すると共に100ml/g〜300ml/gに膨張させ、次いで、粉砕することを含む工程を経て得られたものを挙げることができる。上記熱処理の温度は、特に好ましくは800℃〜1000℃である。
本発明の熱伝導性感圧接着剤組成物(E)には、熱伝導性繊維(D)が含有される。本発明に用いることができる熱伝導性繊維(D)は熱伝導性が高い繊維であれば良く、具体例としては、炭素繊維や金属繊維などを挙げることができる。ただし、熱伝導性感圧接着剤組成物(E)を熱伝導性感圧接着性シート(F)にする際の成形性の観点からは、炭素繊維を用いることが好ましい。
熱伝導性感圧接着性シート(F)を成形する際に、熱伝導性感圧接着剤組成物(E)中の(メタ)アクリル酸エステル単量体(A2m)は重合する。その重合を促進するため、熱伝導性感圧接着剤組成物(E)は、(メタ)アクリル酸エステル重合体(A1)及び(メタ)アクリル酸エステル単量体(A2m)に加えて、さらに、重合開始剤(H)を含有することが好ましい。
本発明の熱伝導性感圧接着剤組成物(E)には、それから得られる熱伝導性感圧接着性シート(F)を発泡させるために、発泡剤を添加することもできる。発泡剤としては、熱分解性有機発泡剤(J)が好ましい。さらに、熱分解性有機発泡剤(J)としては、80℃以上かつ200℃以下の分解開始温度を有するものが好ましい。
本発明の熱伝導性感圧接着剤組成物(E)には、感圧接着剤としての凝集力を高め、耐熱性などを向上させるために、外部架橋剤を添加して、(メタ)アクリル酸エステル重合体(A1)の存在下に(メタ)アクリル酸エステル単量体(A2m)を重合してなる重合体に架橋構造を導入することができる。
本発明の熱伝導性感圧接着剤組成物(E)には、さらに、必要により、顔料、その他の充填材、老化防止剤、増粘剤、などの公知の各種添加剤を、本発明の効果を損なわない範囲で含有することができる。
本発明の熱伝導性感圧接着性シート(F)は、熱伝導性感圧接着剤組成物(E)をシート状に成形してなる。
幅30mm×長さ50mm×厚さ1mmの熱伝導性感圧接着性シート(F)の試料を複数枚用意し、それらにタルクを使用して粉打ちし、厚さが6mm程度になるように積層した。その後、積層された試料を硬度計(商品名「CL−150」、高分子計器株式会社製)の試料台上に乗せ、ダンパーを落として硬度の測定を開始した。ダンパーが試料に当たった時点から20秒後の値を測定値として読み取った。
厚さ1mmの熱伝導性感圧接着性シート(F)をはさみで幅50mm×長さ110mmの大きさに裁断した試料を用意した。この試料の離形PETを剥がし、離形PETを剥がした面に、空気が入らないようにラップフィルムを貼った。このラップフィルムの大きさは、試料の粘着面より大きいものであれば良い。そして、このラップフィルムを貼った試料を用いて熱伝導率を測定した。熱伝導率(単位:W/m・K)測定には、迅速熱伝導率計(商品名「QTM―500」、京都電子工業株式会社製)を用いて、非定常熱線比較法により行った。なお、リファレンスプレートには、石英(電流値:4A)、ジルコニア(電流値:6A)、及び、ムライト(電流値:9A)をこの順で使用した。
厚さ1mmの熱伝導性感圧接着性シートを幅10mm×長さ150mmの大きさに裁断した試験片を5本用意した。ブンゼンバーナーの空気およびガスの流量を調整して高さ20mm程度の青色炎をつくり、試験片を垂直に支持した試験片の下端にバーナーの炎をあてて(炎と約10mm交わるように)10秒間保ち、その後、試験片とバーナー炎を離した。その後、試験片の炎が消えれば直ちにバーナー炎を試験片にあて、10秒間保持した後、試験片とバーナー炎を離した。この試験によって、UL−94(難燃性規格)の判定を行った。すなわち、1回目と2回目の接炎終了後の有炎燃焼持続時間、2回目の接炎終了後の有炎燃焼持続時間及び無炎燃焼持続時間の合計、5本の試験片の有炎燃焼時間の合計、並びに燃焼滴下物(ドリップ)の有無で、V−0に該当するかどうかを判定した。1回目、2回目ともに10秒以内に有炎燃焼を終え、2回目の有炎燃焼持続時間と無炎燃焼時間の合計が30秒以内であって、更に5本の試験片の有炎燃焼時間の合計が50秒以内であり、燃焼落下物がないものをV−0とした。なお、表2における「燃焼試験〔燃焼〕(秒)」は、5本の試験片の有炎燃焼時間の合計の秒数を表す。
反応器に、アクリル酸2−エチルヘキシル94%とアクリル酸6%とからなる単量体混合物100部、2,2'−アゾビスイソブチロニトリル0.03部及び酢酸エチル700部を入れて均一に溶解し、窒素置換後、80℃で6時間重合反応を行った。重合転化率は97%であった。得られた重合体を減圧乾燥して酢酸エチルを蒸発させ、粘性のある固体状の(メタ)アクリル酸エステル重合体(A1)を得た。(メタ)アクリル酸エステル重合体(A1)の重量平均分子量(Mw)は270,000、重量平均分子量(Mw)/数平均分子量(Mn)は3.1であった。重量平均分子量(Mw)及び数平均分子量(Mn)は、テトラヒドロフランを溶離液とするゲルパーミエーションクロマトグラフィーにより、標準ポリスチレン換算で求めた。
混合条件:
恒温槽(商品名「ビスコメイト 150III」、東機産業株式会社製)を用いて、ホバート容器の温調を40℃に設定。
1.回転数メモリ3×10分で混合
2.回転数メモリ5×20分で混合
3.回転数メモリ3×10分、−0.1MPaで真空脱泡しながら混合
これを金型から取り出し、155℃の熱風炉で30分間、重合を行わせ、両面を離型剤付きポリエステルフィルムで覆われた、熱伝導性感圧接着性シート(F1)を得た。結果を表2に示す。
熱伝導性感圧接着性シート(F1)中の残存単量体量から(メタ)アクリル酸エステル単量体混合物(A2m)の重合転化率を計算したところ、99.9%であった。
表1に示すように、炭素繊維(D)の含有量を5部から1部に変更した以外は実施例1と同様にして、熱伝導性感圧接着剤組成物(E2)及び熱伝導性感圧接着性シート(F2)を得た。結果を表2に示す。
表1に示すように、炭素繊維(D)の含有量を5部から30部に変更した以外は実施例1と同様にして、熱伝導性感圧接着剤組成物(E3)及び熱伝導性感圧接着性シート(F3)を得た。結果を表2に示す。
表1に示すように、リン酸エステルを含有させず、水酸化アルミニウムの含有量を300部から350部に変更した以外は実施例1と同様にして、熱伝導性感圧接着剤組成物(E4)及び熱伝導性感圧接着性シート(F4)を得た。結果を表2に示す。
表1に示すように、炭素繊維(D)を含有させないこと以外は実施例1と同様にして、熱伝導性感圧接着剤組成物(EC1)及び熱伝導性感圧接着性シート(FC1)を得た。
結果を表2に示す。
表1に示すように、膨張化黒鉛粉(C)を含有させないこと以外は実施例1と同様にし
て、熱伝導性感圧接着剤組成物(EC2)及び熱伝導性感圧接着性シート(FC2)を得
た。結果を表2に示す。
表1に示すように、水酸化アルミニウムの含有量を300部から500部に変更した以外は比較例2と同様にして、熱伝導性感圧接着剤組成物(EC3)及び熱伝導性感圧接着性シート(FC3)を得た。結果を表2に示す。
上記で作製した熱伝導性感圧接着性シートを評価した。その結果を表2に示す。
(付記)
(付記1)
ゴム、エラストマー及び樹脂よりなる群から選ばれる少なくとも一種の重合体(S)と、燃焼抑制剤(B)と、膨張化黒鉛粉(C)と、熱伝導性繊維(D)と、を含有してなる、熱伝導性感圧接着剤組成物(E)。
(付記2)
前記重合体(S)が(メタ)アクリル酸エステル重合体(A1)である、付記1に記載の熱伝導性感圧接着剤組成物(E)。
(付記3)
前記燃焼抑制剤(B)が水酸化アルミニウムからなるものである、付記1又は2に記載の熱伝導性感圧接着剤組成物(E)。
(付記4)
前記燃焼抑制剤(B)が水酸化アルミニウム及びリン酸エステルからなるものである、付記1又は2に記載の熱伝導性感圧接着剤組成物(E)。
(付記5)
前記膨張化黒鉛粉(C)の平均粒径が30μm〜500μmである、付記1〜4のいずれか1に記載の熱伝導性感圧接着剤組成物(E)。
(付記6)
前記熱伝導性繊維(D)が炭素繊維である、付記1〜5のいずれか1に記載の熱伝導性感圧接着剤組成物(E)。
(付記7)
前記炭素繊維の繊維長が0.5mm〜25mmであり、かつ、前記炭素繊維の繊維径が1μm〜30μmである、付記6に記載の熱伝導性感圧接着剤組成物(E)。
(付記8)
前記重合体(S)が(メタ)アクリル酸エステル重合体(A1)であり、さらに、(メタ)アクリル酸エステル単量体(A2m)を含有する、付記2〜7のいずれか1に記載の熱伝導性感圧接着剤組成物(E)。
(付記9)
前記(メタ)アクリル酸エステル重合体(A1)及び(メタ)アクリル酸エステル単量体(A2m)の合計量100質量部と、前記水酸化アルミニウム50質量部〜400質量部と、前記リン酸エステル10質量部〜100質量部と、前記膨張化黒鉛粉(C)10質量部〜150質量部と、前記熱伝導性繊維(D)0.5質量部〜50質量部と、を含有してなる、付記8に記載の熱伝導性感圧接着剤組成物(E)。
(付記10)
付記1〜9のいずれか1に記載の熱伝導性感圧接着剤組成物(E)を加熱およびシート状に形成してなる、熱伝導性感圧接着性シート(F)。
(付記11)
付記8又は9に記載の熱伝導性感圧接着剤組成物(E)をシート状に成形しながら、又はシート状に成形した後、該熱伝導性感圧接着剤組成物(E)中の(メタ)アクリル酸エステル重合体(A1)の存在下に該熱伝導性感圧接着剤組成物(E)中の(メタ)アクリル酸エステル単量体(A2m)を重合することにより得られる、該熱伝導性感圧接着剤組成物(E)の固化物(E')のシート状成形体である、熱伝導性感圧接着性シート(F)。
Claims (10)
- ゴム、エラストマー及び樹脂よりなる群から選ばれる少なくとも一種の重合体(S)と、燃焼抑制剤(B)と、膨張化黒鉛粉(C)と、熱伝導性繊維(D)と、を含有し、
前記熱伝導性繊維(D)が炭素繊維であり、
前記炭素繊維の繊維長が1mm〜25mmである、熱伝導性感圧接着剤組成物(E)。 - 前記重合体(S)が(メタ)アクリル酸エステル重合体(A1)である、請求項1に記載の熱伝導性感圧接着剤組成物(E)。
- 前記燃焼抑制剤(B)が水酸化アルミニウムからなるものである、請求項1又は2に記載の熱伝導性感圧接着剤組成物(E)。
- 前記燃焼抑制剤(B)が水酸化アルミニウム及びリン酸エステルからなるものである、請求項1又は2に記載の熱伝導性感圧接着剤組成物(E)。
- 前記膨張化黒鉛粉(C)の平均粒径が30μm〜500μmである、請求項1〜4のいずれか1項に記載の熱伝導性感圧接着剤組成物(E)。
- 前記炭素繊維の繊維径が1μm〜30μmである、請求項1〜5のいずれか1項に記載の熱伝導性感圧接着剤組成物(E)。
- 前記重合体(S)が(メタ)アクリル酸エステル重合体(A1)であり、さらに、(メタ)アクリル酸エステル単量体(A2m)を含有する、請求項1〜6のいずれか1項に記載の熱伝導性感圧接着剤組成物(E)。
- 前記(メタ)アクリル酸エステル重合体(A1)及び前記(メタ)アクリル酸エステル単量体(A2m)の合計量100質量部と、前記水酸化アルミニウム50質量部〜400質量部と、前記リン酸エステル10質量部〜100質量部と、前記膨張化黒鉛粉(C)10質量部〜150質量部と、前記熱伝導性繊維(D)0.5質量部〜50質量部と、を含有してなる、請求項7に記載の熱伝導性感圧接着剤組成物(E)。
- 請求項1〜8のいずれか1項に記載の熱伝導性感圧接着剤組成物(E)を加熱およびシート状に形成してなる、熱伝導性感圧接着性シート(F)。
- 請求項7又は8に記載の熱伝導性感圧接着剤組成物(E)をシート状に成形しながら、又はシート状に成形した後、該熱伝導性感圧接着剤組成物(E)中の前記(メタ)アクリル酸エステル重合体(A1)の存在下に該熱伝導性感圧接着剤組成物(E)中の前記(メタ)アクリル酸エステル単量体(A2m)を重合することにより得られる、該熱伝導性感圧接着剤組成物(E)の固化物(E’)のシート状成形体である、熱伝導性感圧接着性シート(F)。
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