JP5939983B2 - 接着剤組成物、及びこれらの接着剤組成物の使用方法と調製方法 - Google Patents
接着剤組成物、及びこれらの接着剤組成物の使用方法と調製方法 Download PDFInfo
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- 239000000853 adhesive Substances 0.000 title claims description 77
- 230000001070 adhesive effect Effects 0.000 title claims description 77
- 239000000203 mixture Substances 0.000 title claims description 66
- 238000000034 method Methods 0.000 title claims description 20
- 238000002360 preparation method Methods 0.000 title description 8
- 239000002245 particle Substances 0.000 claims description 69
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 60
- 238000000576 coating method Methods 0.000 claims description 54
- 229910052799 carbon Inorganic materials 0.000 claims description 53
- 239000011248 coating agent Substances 0.000 claims description 53
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 33
- 239000004917 carbon fiber Substances 0.000 claims description 33
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 18
- 239000011230 binding agent Substances 0.000 claims description 17
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- 239000002243 precursor Substances 0.000 claims description 7
- 238000000151 deposition Methods 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000004020 conductor Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 150000001247 metal acetylides Chemical class 0.000 claims description 3
- 229910044991 metal oxide Inorganic materials 0.000 claims description 3
- 150000004706 metal oxides Chemical class 0.000 claims description 3
- 150000004767 nitrides Chemical class 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 20
- 150000001875 compounds Chemical class 0.000 description 15
- 229910052582 BN Inorganic materials 0.000 description 13
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 13
- 239000000835 fiber Substances 0.000 description 12
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 12
- 229910052786 argon Inorganic materials 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 8
- BGECDVWSWDRFSP-UHFFFAOYSA-N borazine Chemical compound B1NBNBN1 BGECDVWSWDRFSP-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 8
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- 238000005229 chemical vapour deposition Methods 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
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- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 5
- 238000002149 energy-dispersive X-ray emission spectroscopy Methods 0.000 description 5
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- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000000654 additive Substances 0.000 description 3
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- 238000004518 low pressure chemical vapour deposition Methods 0.000 description 3
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- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000001505 atmospheric-pressure chemical vapour deposition Methods 0.000 description 2
- 238000000231 atomic layer deposition Methods 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000012790 confirmation Methods 0.000 description 2
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- 229920003023 plastic Polymers 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000000038 ultrahigh vacuum chemical vapour deposition Methods 0.000 description 2
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- 229910052580 B4C Inorganic materials 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- 229920006397 acrylic thermoplastic Polymers 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000002518 antifoaming agent Chemical class 0.000 description 1
- 239000003429 antifungal agent Substances 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- INAHAJYZKVIDIZ-UHFFFAOYSA-N boron carbide Chemical compound B12B3B4C32B41 INAHAJYZKVIDIZ-UHFFFAOYSA-N 0.000 description 1
- 150000001639 boron compounds Chemical class 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 239000011853 conductive carbon based material Substances 0.000 description 1
- ZOCHARZZJNPSEU-UHFFFAOYSA-N diboron Chemical compound B#B ZOCHARZZJNPSEU-UHFFFAOYSA-N 0.000 description 1
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- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 230000004224 protection Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 150000003377 silicon compounds Chemical class 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
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- 239000004094 surface-active agent Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 description 1
- 239000002470 thermal conductor Substances 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-UHFFFAOYSA-N 0.000 description 1
- ZDHXKXAHOVTTAH-UHFFFAOYSA-N trichlorosilane Chemical compound Cl[SiH](Cl)Cl ZDHXKXAHOVTTAH-UHFFFAOYSA-N 0.000 description 1
- 239000005052 trichlorosilane Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
- B29C65/4855—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by their physical properties, e.g. being electrically-conductive
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- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
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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
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/0097—Glues or adhesives, e.g. hot melts or thermofusible adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2105/00—Condition, form or state of moulded material or of the material to be shaped
- B29K2105/06—Condition, form or state of moulded material or of the material to be shaped containing reinforcements, fillers or inserts
- B29K2105/16—Fillers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2507/00—Use of elements other than metals as filler
- B29K2507/04—Carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29K2995/00—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds
- B29K2995/0012—Properties of moulding materials, reinforcements, fillers, preformed parts or moulds having particular thermal properties
- B29K2995/0013—Conductive
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- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
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- B29L2031/34—Electrical apparatus, e.g. sparking plugs or parts thereof
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- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/29—Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
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Description
石英チューブに炭素繊維(Cytec Industries Inc./コネティカット州スタンフォード)製のThermalGraph(登録商標)DKD)(0.50g)を詰め、石英チューブをアルミナボートに載せた。チューブ及びボートをチューブ炉に入れた。アルゴンガス管を石英チューブの一方の端部に接続した。アルゴン管をボラジンバブラー(及びバブラーバイパス)に接続して、ボラジンをガス流に、石英チューブに加える前に添加した。石英チューブの他方の端部から排気を、オイルバブラー及びヒュームフードに導いた。
実施例1のコーティング済み炭素繊維(20mg)にFTIRペレットプレスで圧力をかけて7mmのペレットとした。コーティング前の炭素繊維(20mg)にも圧力をかけて7mmのペレットとした。これらのペレットを透明プラスチックテープに取り付け、各ペレットの導電率を、4点プローブを使用して検査した。未処理の炭素ペレットは、285Ωの電気抵抗を有し、実施例1のコーティング済みペレットは、1.75x106Ωというずっと大きい電気抵抗を有していた。
実施例1を繰り返し、かつ炉を700℃ではなく1000℃に加熱した。図4から分かるように、結晶が繊維の表面に形成された。これらの結晶によって、不均一なコーティングがこれらの繊維の上に形成された。EDAX分析から、これらの結晶が、ホウ素及び窒素から成り、繊維の露出部分が炭素であったことが確認された。
実施例1の電気絶縁性炭素繊維を調製して、エポキシ樹脂系の熱伝導性接着剤とした。30分遅硬化型エポキシ(部品番号SY−SS;Super Glue Corporation(カリフォルニア州ランチョクーカモンガ)を樹脂系として使用した。エポキシは、樹脂及び硬化剤を含有する2成分調製剤である。実施例1の樹脂(0.982g)及びコーティング済み炭素繊維(0.103g)を手でへらを動かして一括混合した。流動性の良い黒色液体が得られるまで、硬化剤(0.984g)を、樹脂及び炭素繊維の懸濁液に、へらを動かして混入させた。この混合物から、5重量%の充填接着剤が調製されたが、この調製は通常、炭素充填熱伝導性接着剤に対して行なわれる。充填接着剤を、スライドガラスにフィルムとして、0.040インチ(1mm)のギャップドローダウンバーを使用して適用し、48時間に亘って硬化させることができた。硬化フィルムは黒色であり、均一に見え、0.034インチ(0.86mm)の高さであった。電気抵抗を、4点プローブステーションを用いて測定し、開回路と等価である(計測器で測定することができる最大抵抗は1GΩであるので、エポキシの電気抵抗は少なくとも109Ω*cmである)ことが判明したが、これは、接着剤が電気絶縁性を呈することを示している。
接着剤を調製し、実施例4の方法に従って検査したが、この場合、樹脂(0.271g)、コーティング済み炭素繊維(0.060g)及び硬化剤(0.276g)を異なる量とした。この混合物から10重量%の充填接着剤が調製されたが、この調製も通常、炭素充填熱伝導性接着剤に対して行なわれる。硬化フィルムは黒色であり、均一に見え、0.031インチ(0.79mm)の高さであった。この電気抵抗は、接着剤の電気抵抗が少なくとも109Ω*cmの開回路になっていることも判明した。
未処理の炭素繊維(Cytec Industries Inc./コネティカット州スタンフォード)製のThermalGraph(登録商標)DKD)を接着剤に混入し、実施例4の方法に従って検査した。接着剤に、樹脂(0.620g)、コーティング前の炭素繊維(0.137g)、及び硬化剤(0.616g)を含有させることにより、コーティング前の10重量%の炭素繊維を含有する接着剤を調製した。硬化フィルムは黒色であり、均一に見え、0.025インチ(0.64mm)の高さであった。電気抵抗を測定したところ、17x106Ω*cmであったが、この値は、コーティング済み炭素繊維を含有する接着剤よりも大幅に小さい。
石英チューブに炭素繊維(Cytec Industries Inc./コネティカット州スタンフォード)製のThermalGraph(登録商標)DKD)(0.50g)を詰め、石英チューブをアルミナボートに載せた。チューブ及びボートをチューブ炉に入れた。電気接続用継手内のアルゴンガス管を石英チューブの一方の端部に接続した。2本のスチールワイヤを電気バイパスから、セラミックジャケットの内部のチューブ炉内に延出させた。ワイヤの両先端部を、セラミックジャケットの端部で露出させ、これらの先端部を使用してプラズマを衝突させた。これらのワイヤを1500V,0.5Aの電源に接続した。アルゴン管をボラジンバブラー(及び、バブラーバイパス)に接続してボラジンをガス流に、石英チューブに加える前に添加した。石英チューブの他方の端部から排気を、オイルバブラー及びヒュームフードに導いた。
Claims (9)
- 電子部品の熱伝導体として使用されるのに適する接着剤組成物であって、セラミックス及びダイヤモンド状炭素から選択される電気絶縁コーティングを有する炭素系粒子を含み、前記電気絶縁コーティングが前記炭素系粒子の一部に渡って延在することにより前記炭素系粒子のコーティングされた部分と露出した部分が分かれており、前記コーティングされた炭素系粒子が少なくとも50Ω*cmの電気抵抗を有し、前記接着性組成物の少なくとも10重量%である接着剤組成物。
- 前記炭素系粒子が黒鉛炭素を含む、請求項1に記載の接着剤組成物。
- 前記黒鉛炭素が、炭素繊維、黒鉛、膨張黒鉛、グラフェン、及びこれらの組み合わせから選択される材料である、請求項2に記載の接着剤組成物。
- ペーストである、請求項1に記載の接着剤組成物。
- 前記電気絶縁コーティングが、金属酸化物、金属窒化物、金属炭化物、及びこれらの組み合わせから成るグループから選択されるセラミックである、請求項1に記載の接着剤組成物。
- 更にバインダを含む、請求項1に記載の接着剤組成物。
- 熱伝導性接着剤組成物を生成する方法であって、
電気絶縁コーティングを炭素系粒子の上に堆積させる工程と、
前記コーティング済み炭素系粒子をバインダに混合する工程と
を含み、
前記電気絶縁コーティングが前記炭素系粒子の一部に渡って延在することにより前記炭素系粒子のコーティングされた部分と露出した部分が分かれており、前記コーティングされた炭素系粒子が少なくとも50Ω*cmの電気抵抗を有し、前記接着性組成物の少なくとも10重量%であり、
前記電気絶縁コーティングが、金属酸化物、金属窒化物、金属炭化物、及びこれらの組み合わせから成るグループから選択されるセラミックである方法。 - 前駆体ガスを前記炭素系粒子の表面上に引き込んで、前記ガスを反応させ、前記コーティングを前記粒子の上に堆積させる工程を含む、請求項7に記載の方法。
- 前記炭素系粒子が炭素繊維を含む、請求項7に記載の方法。
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