JPH0376344B2 - - Google Patents
Info
- Publication number
- JPH0376344B2 JPH0376344B2 JP59049211A JP4921184A JPH0376344B2 JP H0376344 B2 JPH0376344 B2 JP H0376344B2 JP 59049211 A JP59049211 A JP 59049211A JP 4921184 A JP4921184 A JP 4921184A JP H0376344 B2 JPH0376344 B2 JP H0376344B2
- Authority
- JP
- Japan
- Prior art keywords
- aluminum nitride
- weight
- powder
- sheet
- organic polymer
- 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.)
- Expired - Lifetime
Links
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 41
- 239000000843 powder Substances 0.000 claims description 41
- 239000002245 particle Substances 0.000 claims description 26
- 150000001875 compounds Chemical class 0.000 claims description 25
- 229920000620 organic polymer Polymers 0.000 claims description 21
- 239000002131 composite material Substances 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 13
- 239000007822 coupling agent Substances 0.000 claims description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- 239000012535 impurity Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 10
- 229910052799 carbon Inorganic materials 0.000 description 9
- 229920005989 resin Polymers 0.000 description 9
- 239000011347 resin Substances 0.000 description 9
- 238000002156 mixing Methods 0.000 description 8
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 7
- 229920002379 silicone rubber Polymers 0.000 description 7
- 239000004945 silicone rubber Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 239000006087 Silane Coupling Agent Substances 0.000 description 5
- 230000017525 heat dissipation Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920005992 thermoplastic resin Polymers 0.000 description 4
- 229920001187 thermosetting polymer Polymers 0.000 description 4
- -1 uropyrene Chemical compound 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920001778 nylon Polymers 0.000 description 3
- 239000002002 slurry Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 239000011701 zinc Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 239000004698 Polyethylene Substances 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 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
- 239000012298 atmosphere Substances 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000002612 dispersion medium Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 238000007606 doctor blade method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 239000012776 electronic material Substances 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 229920001519 homopolymer Polymers 0.000 description 2
- 239000011256 inorganic filler Substances 0.000 description 2
- 229910003475 inorganic filler Inorganic materials 0.000 description 2
- 150000002736 metal compounds Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- 229920000573 polyethylene Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- UOCLXMDMGBRAIB-UHFFFAOYSA-N 1,1,1-trichloroethane Chemical compound CC(Cl)(Cl)Cl UOCLXMDMGBRAIB-UHFFFAOYSA-N 0.000 description 1
- VXNZUUAINFGPBY-UHFFFAOYSA-N 1-Butene Chemical compound CCC=C VXNZUUAINFGPBY-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 1
- BMTAFVWTTFSTOG-UHFFFAOYSA-N Butylate Chemical compound CCSC(=O)N(CC(C)C)CC(C)C BMTAFVWTTFSTOG-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- PYVHTIWHNXTVPF-UHFFFAOYSA-N F.F.F.F.C=C Chemical compound F.F.F.F.C=C PYVHTIWHNXTVPF-UHFFFAOYSA-N 0.000 description 1
- 244000043261 Hevea brasiliensis Species 0.000 description 1
- 244000178870 Lavandula angustifolia Species 0.000 description 1
- 235000010663 Lavandula angustifolia Nutrition 0.000 description 1
- 229920000877 Melamine resin Polymers 0.000 description 1
- 239000004952 Polyamide Substances 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 229960004217 benzyl alcohol Drugs 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000012936 correction and preventive action Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 description 1
- XXBDWLFCJWSEKW-UHFFFAOYSA-N dimethylbenzylamine Chemical compound CN(C)CC1=CC=CC=C1 XXBDWLFCJWSEKW-UHFFFAOYSA-N 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- HDERJYVLTPVNRI-UHFFFAOYSA-N ethene;ethenyl acetate Chemical group C=C.CC(=O)OC=C HDERJYVLTPVNRI-UHFFFAOYSA-N 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- HCDGVLDPFQMKDK-UHFFFAOYSA-N hexafluoropropylene Chemical compound FC(F)=C(F)C(F)(F)F HCDGVLDPFQMKDK-UHFFFAOYSA-N 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000011872 intimate mixture Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229920003052 natural elastomer Polymers 0.000 description 1
- 229920001194 natural rubber Polymers 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- 229920001084 poly(chloroprene) Polymers 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920005629 polypropylene homopolymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229940124530 sulfonamide Drugs 0.000 description 1
- 150000003456 sulfonamides Chemical class 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 229920005613 synthetic organic polymer Polymers 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Description
本発明は新規なシートを提供する。詳しくは
（）有機高分子化合物と（）カツプリング剤
で処理された平均粒子径が2μｍ以下で、3μｍ以
下の粒子のものを70容量％以上の割合で含有し、
且つ酸素含有量が3.0重量％以下及び純度が95％
以上の窒化アルミニウム粉末とよりなり、前記有
機高分子化合物100重量部に対して、窒化アルミ
ニウム粉末が、300〜1000重量部均一に分散した
組成物よりなる極めて熱伝導性の大きいという特
色を有する複合シートである。
従来、有機高分子化合物に無機粉末を配合した
素材を用いた複合シートは公知で、該有機高分子
化合物を無機粉末の種々の組合せが提案されてい
る。一般には得られる複合シートに要求される性
状に応じて特定の無機粉末が選択して使用され
る。即ち複合シートの用途に応じて要求させる性
状は混合される無機粉末の性状によつて影響させ
る場合が多く、如何なる性状を有する無機粉末を
選択するかが大きな技術開発の焦点となる。
また、熱伝導性の大きい放熱シートとして、特
定の無機充填剤を35〜70容量％含有させた加硫ゴ
ムシートも提案されている。このものは、或る程
度高い熱伝導性を有するため、パワートランジス
タや集積回路等の発熱性電子部品に対する放熱シ
ートとして有用である。しかし、電子機器の進歩
は著じるしく、益々集積度が高く、高密度化し、
発熱量も大きくなりつつあり、それに伴つて、よ
り高い熱伝導性の絶縁性材料が要求されつつあ
る。
そこで、本発明者は従来提案されている特定の
無機充填剤、例えば市販の窒化アルミニウム粉末
を用いて、シリコンゴムに配合し、熱伝導性の改
良を試みたが、窒化アルミニウムの配合量が少な
い場合は、勿論熱伝導性の改良効果が劣り、配合
量の増加と共に熱伝導性の改良は認められるが、
次第にゴムが硬質化する欠点が生ずる。更に50容
量％を超えると配合が困難で且つ最早ゴムの性質
を全く示さなくなり、例えば曲げに対する回復力
が乏しく、場合によると折れるようになるため、
期待される程高い熱伝導性を有する高分子材料を
得ることが困難であることを知つた。
本発明者は、種々のセラミツクを開発した経験
に基づいて、高熱伝導性セラミツクである窒化ア
ルミニウムを配合した高分子化合物による高熱伝
導性材料を鋭意研究した結果、上記の如く、特定
の窒化アルミニウム粉末をカツプリング剤で処理
したものは、極めて高充填が可能であり、しかも
高熱伝導性の性状を与えるだけでなく、ほとんど
制限なく種々のょ有機高分子化合物とよく混合さ
れることを見出したこの知見に基づき本発明を完
成し、ここに提案するに至つた。
即ち、（）有機高分子化合物と（）カツプ
リング剤で処理された平均粒子径が2μｍ以下で、
3μｍ以下の粒子のものを70容量％以上の割合で
含有し、且つ酸素含有量が3.0重量％以下及び純
度が95％以上の窒化アルミニウム粉末とよりな
り、前記有機高分子化合物100重量部に対して、
窒化アルミニウム粉末が、300〜1000重量部均一
に分散した組成物よりなる複合シートである。
本発明で用いる有機高分子化合物は特に限定さ
れる公知のものが使用出来る。一般には分子量
3000〜1000000好ましくは5000〜500000の有機高
分子化合物が好適である。また該有機高分子化合
物は天然のもの或いは合成のものになんら区別さ
れず使用出来る。例えば天然の有機高分子化合と
しては天然ゴムがその代表的なものである。また
合成の有機高分子化合物は熱可塑性樹脂又は熱硬
化性樹脂のいずれをも特に限定されず使用出来
る。該熱可塑樹脂の代表的なものを例示すれば、
スチレン−ブタジエン−ラバン、クロロプレンゴ
ム、シリコーンオゴム等のゴム状有機高分子化合
物；エチレン、ウロピレン、ブテン、スチレン等
のオレフインの単独重合体又は共重合体；塩化ビ
ニル、塩化ビニリデン、四弗化エチレン、６弗化
プロピレン等の含ハロゲンビニル化合物の単独重
合体又は共重合体；ポリエステル；ポリアミド；
ポリ酢酸ビニル；ポリアクリレート；ポリアクリ
ロニトリル；ポリカーボネート；酢酸ビニル−エ
チレン共重合体等が好適に使用される。また前記
熱硬化性樹脂の代表的なものを例示すると、フエ
ノール樹脂；ホルムアルデヒドおよびケトン樹
脂；メラミン樹脂；スルホンアミド樹脂；アルキ
ド樹脂；アポキシ樹脂；不飽和ポリエステル樹脂
等が好適に使用される。
本発明に於ける他の成分は下記特性を有する窒
化アルミニウム粉末である。
即ち、平均粒子径2μｍ以下で、3μｍ以下の粒
子のものを70容量％以上の割合で含有し且つ酸素
含有量3.0重量％以下及び窒化アルミニウムの純
度が95％以上の窒化アルミニウム粉末である。尚
上記窒化アルミニウムの純度は次ぎのような定義
にしたがう。即ち窒化アルミニウムはアルミニウ
ムと窒素の１：１の化合物であり、これ以外のも
のを原則としてすべて不純物として取扱う。但し
窒化アルミニウム粉末の表面は空気中で不可避的
に酸化されAl−Ｎ結合がAl−Ｏ結合に置代つて
いるので、このAl−Ｏ結合しているアルミニウ
ムは陽イオン不純物とはみなさない。また前記に
おける平均粒子径とは光透過式の粒度分布測定器
による体積基準の中間粒子径をいう。
即ち、本発明において、窒化アルミニウムの粒
子形が平均2μｍ以上である場合は、均一な分散
が行われ難いため大量の配合が難しく、得られる
複合シートの物理的性質も乏化する。特に3μｍ
以上の粒子の割合が増加するとその傾向が顕著と
なる。また不純物、特に酸素含有量が増大すると
熱伝導性の改良効果が減殺される傾向がある。そ
の他の不純物についても同様であり、本発明に用
いる窒化アルミニウムの純度は95％以上のものを
使用すべきである。
前記のような性状を有する窒化アルミニウム粉
末は新規なものである。本発明に於いては上記性
状を有する窒化アルミニウムの製法までも限定す
るものではないが一般に好適に使用される代表的
な方法を例示すると次の通りである。即ち、
(1) 平均粒子径が2μｍ以下のアルミナ微粒子と
灰分含量0.2重量％で平均粒子径が1μｍ以下の
カーボン微粉末とを水、アルコール類、炭化水
素等の液体分散媒体中で緊密に混合し、そのさ
い該アルミナ微粉末対該カーボン微粉末の重量
比は１：0.36〜１：１であり；
(2) 得られた緊密混合物を、適宜乾燥し、窒素又
はアンモニアの雰囲気下で1400〜1700℃の温度
で焼成し；
(3) 次いで得られた微粉末を酸素を含む雰囲気下
で600〜900℃の温度で加熱して未反応のカーボ
ンを加熱除去し、窒化アルミニウム含量が少く
とも95重量％であり、結合酸素の含量が最大
3.0重量％好ましくは1.5重量％であり、且つ不
純物としての金属化合物の含量が金属として最
大0.3重量％である平均粒子径が2μｍ以下の窒
化アルミニウム粉分末を生成せしめる、
ことによつて製造することができる。
また上記方法ではアルミナとカーボンは特定の
性状のものを用いる必要がある。一般にアルミナ
微分末としては平均粒子径が2μｍ以下の微粉末
を用いる必要があり、好のもしくは少なくとも
99.0重量％より好ましくは少なくとも99.9重量％
の純度のものが用いられる。またカーボン微粉末
は灰分の含有量最大0.2重量％好ましくは最大0.1
重量％のものとして用いる必要がある。また該カ
ーボンの平均粒子径は1μｍ以下の微粒子として
用いる必要がある。さらに該カーボンとしてはカ
ーボンブラツク、黒鉛化カーボン等が使用されう
るが一般にはカーボンブラツクが好ましい。そし
て窒化アルミニウム粉末中の不純物としての金属
化合物の含量を減するためには上記原料となるア
ルミナに該不純物となる金属成分例えば、珪素、
マンガン、鉄、クロム、ニツケル、コバルト、
銅、亜鉛、チタン等を陽イオン成分とする化合物
が金属として0.3重量％以下好ましくは0.2重量％
以下更に好ましくは0.1重量％以下のものを用い
るのが好ましい。勿論上記不純物成分は前記アル
ミナ及びカーボンの原料を湿式混合する場合も、
混合装置から混入することもあるので一般にはこ
れらの不純物成分が窒化アルミニウム粉末中に混
入するのを避けるために、窒化アルミニウム自身
あるいは99.9重量％以上の高純度アルミナとする
のが好ましい。また混合装置の原料と接する面を
すべてプラスチツク製とするかプラスチツクでコ
ーテイングすることもできる。該プラスチツクと
しては特に限定されず例えばポリエチレン、ポリ
プロピレン、ナイロン、ポリエステル、ポリウレ
タン等が使用できる。この場合、プラスチツク中
には安定剤として種々の金属成分を含む場合があ
るので、予めチエツクして使用するようにすべき
である。
本発明は、高い熱伝導製を有し、且つ必要な可
撓性等を維持した複合シートを得るものであり、
大量の窒化アルミニウムの配合を行なうにかかわ
らず、十分な均一性と物理的性質を保つために前
記性状の窒化アルミニウム粉末をカツプリング剤
で処理し、その表面を被覆して用いる。該カツプ
リング剤は特に限定されず有機高分子化合物に無
機化合物を混入するときにカツプリング剤とに使
用されうることが公知のものを特に剤限されず使
用出来る。一般には例えば、アミノミラン、ビニ
ルシラン、エポキシシラン、有機チタネート化合
物等のシアンカツプリング剤或いは表面処理剤等
が好適に使用される。
これらのカツプリング剤による処理方法は、公
知の方法が何ら制限なく使用される。
前記有機高分子化合物と前記窒化アルミニウム
粉末との混合割合は得られるシートに要求される
性状によつて異なり一概に限定出来ないが一般に
は有機高分子化合物10重量部に対しで窒化アルミ
ニウム粉末は300〜900重量部の範囲から選べばよ
い。かくして、極めて高い熱伝導性の複合シート
が得られる。例えば、第１図に本発明の実施例３
と同様な方法で窒化アルミニウムの配合量を変化
させた場合の熱伝導性の変化を図を示す。また、
本発明の如くカツプリング剤による処理を施さな
い市販の窒化アルミニウム（平均粒子径、約3μ
ｍ、不純物として、カーボンを含む純度約90％）
をそのまま用いた場合の例も比較のため併せ示
す。この場合は、配合量が85重量％以上になると
均一混合が困難となつた。
第１図から、本発明において特に高い窒化アル
ミニウムの配合域において、優れた熱伝導性が得
られることがわかる。
前記有機高分子化合物と窒化アルミニウム粉末
との混合物から本発明のシートを製造する方法は
特に限定されず公知のシートの製法が採用出来
る。例えば有機高分子化合物をして熱硬化性樹脂
を用いる場合は、前記混合物を加温下例れば50〜
80℃程度の温度下に混合し、該混合物は必要に応
じて粉砕した後、加圧下に或いは常圧下に硬化温
度まで加熱してシートに成形する方法が採用され
る。また有機高分子化合物が熱可塑性樹脂の場合
な熱可塑性樹脂と前記窒化アルミニムウとの混合
物をシート状に加熱成形する方法が一般的であ
る。また有機高分子化合物がシリコ−ンゴムなど
のゴム状物質の場合有機溶媒にシリコーンゴムを
溶解し、窒化アルミニウムを加え、得られるスラ
リーに必要に応じて触媒を加えた後、例えばドク
ターブレード法などの手段でシート状物を成形
し、該シート状物を加熱例えば160〜180℃でプレ
ス加硫して目的の複合シートを得ることも出来
る。
本発明の複合シートは熱伝導率が著しく改良さ
れたシートとなるので例えばパワートランジスタ
ー、サイリスターなどの電子材料で放熱を必要と
する箇所の絶縁シートとして有効に使用される。
また熱硬化性樹脂と前記窒化アルミニウム粉末と
より構成されてなる複合シートは高放熱樹脂基板
として例えばIC基板に使用される。
本発明の複合シートの開発によつて、特に高放
熱、絶縁を必要とする電子材料、電気機器として
の用途がより広く拡がるもので本発明の寄与は計
り知れないものである。
本発明を更に具体的に説明するための以下実施
例を挙げて説明するが本発明はこれらの実施例に
限定されるものではない。
実施例 １
純度99.99％（不純物分析値を表１に示す）で
平均粒子径が0.52μｍで3μｍ以下の粒子の割合が
95vol％のアルミナ100重量部と、灰分0.08wt％で
平均粒子径が0.45μｍのカーボンブラツク50重量
部とを、ナイロン製ポツトとナイロンコーテイン
グしたがボールを用いエタノールを分散媒体とし
て均一にボーリミル混合した。得られた混合物を
乾燥後、高純度黒鉛製平皿に入れ電気炉内に窒素
ガスを３／minで連続的に供給しながら1600℃
の温度で６時間加熱した。得られた反応混合物を
空気中で750℃の温度で４時間加熱し、未反応の
カーボンを酸化除去した。得られた白色の粉末は
Ｘ線回析分析（Xray diffraction analysis）の
結果、単相（single phase）のAlNであり、
Al2O3の回析ピークは無かつた。また該粉末の平
均粒子径を粒度分布測定器（堀場製作所製CAPA
−500）を用いて側てしたところ1.31μｍであり、
3μｍ以下が90容量％を占めた。走査型電子顕微
鏡による観察ではこの粉末は平均0.7μｍ程度の均
一な粒子であつた。また比表面積の測定値は4.0
m2／ｇであつた。この粉末の分析値を表２に示
す。
表 １
Al2O3粉末分析値
Al2O3含有量 99.99％
元 素 含有量（PPM）
Mg ＜５
Cr ＜10
Si 30
Zn ＜５
Fe 22
Cu ＜５
Ca ＜20
Ni 15
Ti ＜５
表 ２
AlN粉末分析値
AlN含有量 97.8％
元 素 含有量
Mg ＜５（PPM）
Cr 21（ 〃 ）
Si 125（ 〃 ）
Zn ９（ 〃 ）
Fe 20（ 〃 ）
Cu ＜５（ 〃 ）
Mn ５（ 〃 ）
Ni 27（ 〃 ）
Ti ＜５（ 〃 ）
Co ＜５（ 〃 ）
Al 64.8（wt％）
Ｎ 33.4（ 〃 ）
Ｏ 1.1（ 〃 ）
Ｃ 0.11（ 〃 ）
このようにして得られた窒化アルミニウム粉末
を２％のシランカツプリング剤（日本ユニカー社
製Ａ−172）水溶液と接触させた後過して、室
温で減圧乾燥した。次いでエポキシ樹脂（シエル
化学社製エピコート1001）に硬化剤としてジシア
ノジアミドおよびベンジルジメチルアミンを各々
４重量％、0.2重量％添加した後ロール式混練機
で80℃の温度で混練した。混練しながら前記シラ
ンカツプリング剤処理した窒化アルミニウム粉末
を樹脂100重量部に対して700重量部添加し均一に
混合した。得られた混合物は室温で粉砕し、この
粉末を100Kg／cm2の圧力、16℃の温度で30分間予
備硬化させた。次いで無加圧下で180℃の温度で
硬化処理をし、厚さ1.2mmのシートを得た。得ら
れたシートの熱伝導率を理学電機製のレーザーフ
ラツシユ法熱定数測定装置を用いて測定したとこ
ろ0.012cal／cm・sec・Ｋであつた。
実施例 ２
実施例１と同じ方法で、エポキシ樹脂と窒化ア
ルミニウム粉末の配合比を変えて実験した結果を
表３に示す。
The present invention provides a novel sheet. Specifically, it contains 70% or more by volume of particles with an average particle diameter of 2 μm or less and 3 μm or less treated with () an organic polymer compound and () a coupling agent,
And oxygen content is 3.0% by weight or less and purity is 95%
A composite material comprising the above aluminum nitride powder and having an extremely high thermal conductivity, comprising a composition in which 300 to 1000 parts by weight of the aluminum nitride powder is uniformly dispersed in 100 parts by weight of the organic polymer compound. It is a sheet. BACKGROUND OF THE INVENTION Conventionally, composite sheets using a material containing an organic polymer compound and an inorganic powder have been known, and various combinations of the organic polymer compound and inorganic powder have been proposed. Generally, a specific inorganic powder is selected and used depending on the properties required of the resulting composite sheet. That is, the properties required depending on the application of the composite sheet are often influenced by the properties of the inorganic powder to be mixed, and the selection of the inorganic powder having the properties is a major focus of technological development. Furthermore, a vulcanized rubber sheet containing 35 to 70% by volume of a specific inorganic filler has also been proposed as a heat dissipation sheet with high thermal conductivity. Since this material has a somewhat high thermal conductivity, it is useful as a heat dissipation sheet for heat-generating electronic components such as power transistors and integrated circuits. However, the progress of electronic devices has been remarkable, and they have become increasingly integrated and densely packed.
The amount of heat generated is also increasing, and as a result, insulating materials with higher thermal conductivity are being required. Therefore, the present inventor attempted to improve thermal conductivity by blending silicone rubber with specific inorganic fillers that have been proposed in the past, such as commercially available aluminum nitride powder, but the amount of aluminum nitride blended was small. In this case, the effect of improving thermal conductivity is of course inferior, and an improvement in thermal conductivity is observed as the amount added increases, but
The disadvantage is that the rubber gradually becomes harder. Furthermore, if it exceeds 50% by volume, it will be difficult to blend and will no longer exhibit rubber properties at all, for example, it will have poor resilience against bending and may even break.
We have learned that it is difficult to obtain polymeric materials with as high thermal conductivity as expected. Based on the experience of developing various ceramics, the present inventor has conducted extensive research into high thermal conductive materials made from polymer compounds containing aluminum nitride, which is a highly thermally conductive ceramic. This finding found that treated with a coupling agent not only allows for extremely high loading and provides high thermal conductivity, but also mixes well with various organic polymer compounds with almost no restrictions. Based on this, the present invention has been completed and proposed here. That is, the average particle diameter treated with () an organic polymer compound and () a coupling agent is 2 μm or less,
The aluminum nitride powder contains particles of 3 μm or less in a ratio of 70% by volume or more, has an oxygen content of 3.0% by weight or less, and has a purity of 95% or more, based on 100 parts by weight of the organic polymer compound. hand,
This is a composite sheet made of a composition in which 300 to 1000 parts by weight of aluminum nitride powder is uniformly dispersed. The organic polymer compound used in the present invention may be any known organic compound with particular limitations. Generally molecular weight
An organic polymer compound having a molecular weight of 3,000 to 1,000,000, preferably 5,000 to 500,000 is suitable. Further, the organic polymer compound can be used without any distinction whether it is natural or synthetic. For example, natural rubber is a typical natural organic polymer compound. Furthermore, the synthetic organic polymer compound may be either a thermoplastic resin or a thermosetting resin without any particular limitation. Typical examples of thermoplastic resins include:
Rubbery organic polymer compounds such as styrene-butadiene-laban, chloroprene rubber, and silicone rubber; homopolymers or copolymers of olefins such as ethylene, uropyrene, butene, and styrene; vinyl chloride, vinylidene chloride, and ethylene tetrafluoride , homopolymers or copolymers of halogen-containing vinyl compounds such as propylene hexafluoride; polyesters; polyamides;
Polyvinyl acetate; polyacrylate; polyacrylonitrile; polycarbonate; vinyl acetate-ethylene copolymer, etc. are preferably used. In addition, to illustrate typical thermosetting resins, phenol resins; formaldehyde and ketone resins; melamine resins; sulfonamide resins; alkyd resins; apoxy resins; unsaturated polyester resins and the like are preferably used. Another component in the present invention is aluminum nitride powder having the following properties. That is, the aluminum nitride powder has an average particle diameter of 2 μm or less, contains particles of 3 μm or less in a ratio of 70% by volume or more, has an oxygen content of 3.0% by weight or less, and has an aluminum nitride purity of 95% or more. The purity of the aluminum nitride is defined as follows. That is, aluminum nitride is a 1:1 compound of aluminum and nitrogen, and everything else is treated as an impurity in principle. However, since the surface of the aluminum nitride powder is inevitably oxidized in the air and Al--N bonds replace Al--O bonds, the aluminum bonded to Al--O is not considered as a cationic impurity. Moreover, the average particle diameter in the above refers to the volume-based median particle diameter measured by a light transmission type particle size distribution analyzer. That is, in the present invention, if the average particle size of aluminum nitride is 2 μm or more, uniform dispersion is difficult to achieve, making it difficult to blend in large quantities, and the resulting composite sheet also has poor physical properties. Especially 3μm
This tendency becomes more pronounced as the proportion of the above particles increases. Furthermore, when impurities, especially oxygen content, increases, the effect of improving thermal conductivity tends to be diminished. The same applies to other impurities, and the purity of aluminum nitride used in the present invention should be 95% or higher. The aluminum nitride powder having the properties described above is new. Although the present invention does not limit the method for producing aluminum nitride having the above-mentioned properties, typical methods that are generally suitably used are exemplified as follows. That is, (1) Fine alumina particles with an average particle size of 2 μm or less and fine carbon powder with an ash content of 0.2% by weight and an average particle size of 1 μm or less are intimately mixed in a liquid dispersion medium such as water, alcohol, or hydrocarbon. At that time, the weight ratio of the fine alumina powder to the fine carbon powder is 1:0.36 to 1:1; (2) The resulting intimate mixture is suitably dried and heated to 1400 to 1000 ml under an atmosphere of nitrogen or ammonia. (3) The resulting fine powder is then heated at a temperature of 600 to 900°C in an oxygen-containing atmosphere to remove unreacted carbon and reduce the aluminum nitride content to at least 95%. % by weight, and the content of combined oxygen is maximum
3.0% by weight, preferably 1.5% by weight, and the content of metal compounds as impurities is at most 0.3% by weight as metal, and the average particle size is 2 μm or less. be able to. Further, in the above method, it is necessary to use alumina and carbon having specific properties. Generally, it is necessary to use a fine powder with an average particle size of 2 μm or less as alumina differential powder, and it is preferable or at least
more preferably at least 99.9% by weight than 99.0% by weight
of purity is used. Furthermore, the carbon fine powder has an ash content of up to 0.2% by weight, preferably up to 0.1%.
It is necessary to use it as a percentage by weight. Further, the carbon needs to be used as fine particles with an average particle size of 1 μm or less. Furthermore, carbon black, graphitized carbon, etc. can be used as the carbon, but carbon black is generally preferred. In order to reduce the content of metal compounds as impurities in the aluminum nitride powder, metal components as impurities such as silicon,
manganese, iron, chromium, nickel, cobalt,
Compounds containing copper, zinc, titanium, etc. as cationic components: 0.3% by weight or less, preferably 0.2% by weight as metals
It is more preferable to use 0.1% by weight or less. Of course, the above impurity components are also contained in the case where the alumina and carbon raw materials are wet mixed.
Generally, in order to avoid these impurity components from being mixed into the aluminum nitride powder, it is preferable to use aluminum nitride itself or high-purity alumina of 99.9% by weight or more since these impurity components may be mixed in from the mixing device. Furthermore, all surfaces of the mixing device that come into contact with the raw materials can be made of plastic or coated with plastic. The plastic is not particularly limited, and for example, polyethylene, polypropylene, nylon, polyester, polyurethane, etc. can be used. In this case, since the plastic may contain various metal components as stabilizers, it should be checked before use. The present invention provides a composite sheet that has high thermal conductivity and maintains necessary flexibility, etc.
In order to maintain sufficient uniformity and physical properties even when a large amount of aluminum nitride is blended, the aluminum nitride powder having the above properties is treated with a coupling agent and its surface is coated before use. The coupling agent is not particularly limited, and any known coupling agent that can be used as a coupling agent when an inorganic compound is mixed into an organic polymer compound can be used without particular limitation. Generally, for example, cyan coupling agents or surface treatment agents such as aminomilane, vinylsilane, epoxysilane, and organic titanate compounds are preferably used. As the treatment method using these coupling agents, known methods can be used without any restrictions. The mixing ratio of the organic polymer compound and the aluminum nitride powder varies depending on the properties required of the sheet to be obtained and cannot be absolutely limited, but generally it is 10 parts by weight of the organic polymer compound and 300 parts by weight of the aluminum nitride powder. You may choose from a range of ~900 parts by weight. A composite sheet with extremely high thermal conductivity is thus obtained. For example, FIG. 1 shows Embodiment 3 of the present invention.
The figure shows the change in thermal conductivity when the amount of aluminum nitride is changed in the same manner as in the figure. Also,
Commercially available aluminum nitride (average particle size, approximately 3 μm) that is not treated with a coupling agent as in the present invention.
m, purity approximately 90% including carbon as an impurity)
For comparison, an example in which is used as is is also shown. In this case, uniform mixing became difficult when the blending amount exceeded 85% by weight. From FIG. 1, it can be seen that in the present invention, excellent thermal conductivity can be obtained particularly in the high aluminum nitride content range. The method for manufacturing the sheet of the present invention from the mixture of the organic polymer compound and aluminum nitride powder is not particularly limited, and any known sheet manufacturing method can be employed. For example, when using a thermosetting resin with an organic polymer compound, the mixture is heated to
A method is adopted in which the mixture is mixed at a temperature of about 80° C., and the mixture is pulverized if necessary, and then heated to a curing temperature under pressure or normal pressure to form a sheet. Further, when the organic polymer compound is a thermoplastic resin, a method of thermoforming a mixture of the thermoplastic resin and the aluminum nitride into a sheet shape is common. In addition, when the organic polymer compound is a rubbery substance such as silicone rubber, the silicone rubber is dissolved in an organic solvent, aluminum nitride is added, and a catalyst is added as necessary to the resulting slurry, followed by a method such as a doctor blade method. The desired composite sheet can also be obtained by forming a sheet-like material by means of a method and press-curing the sheet-like material by heating, for example, at 160 to 180°C. Since the composite sheet of the present invention has significantly improved thermal conductivity, it can be effectively used as an insulating sheet for parts of electronic materials such as power transistors and thyristors that require heat dissipation.
Further, a composite sheet composed of a thermosetting resin and the aluminum nitride powder is used as a high heat dissipation resin substrate, for example, for an IC substrate. The development of the composite sheet of the present invention will expand its use particularly as electronic materials and electrical equipment that require high heat dissipation and insulation, and the contribution of the present invention is immeasurable. EXAMPLES The present invention will be described below with reference to Examples to explain the present invention more specifically, but the present invention is not limited to these Examples. Example 1 The purity is 99.99% (impurity analysis values are shown in Table 1), the average particle diameter is 0.52 μm, and the proportion of particles of 3 μm or less is
100 parts by weight of alumina of 95 vol% and 50 parts by weight of carbon black having an ash content of 0.08 wt% and an average particle diameter of 0.45 μm were uniformly mixed by a Bore mill using a nylon pot and a nylon-coated ball with ethanol as a dispersion medium. . After drying the resulting mixture, it was placed in a flat plate made of high-purity graphite and heated at 1600°C while continuously supplying nitrogen gas at 3/min in an electric furnace.
The mixture was heated at a temperature of 6 hours. The resulting reaction mixture was heated in air at a temperature of 750° C. for 4 hours to oxidize and remove unreacted carbon. As a result of X-ray diffraction analysis, the obtained white powder was found to be single phase AlN.
There was no Al 2 O 3 diffraction peak. In addition, the average particle diameter of the powder was measured using a particle size distribution analyzer (CAPA manufactured by Horiba, Ltd.).
-500), it was 1.31μm,
3μm or less accounted for 90% of the capacity. When observed using a scanning electron microscope, this powder was found to be uniform particles with an average size of about 0.7 μm. Also, the measured value of specific surface area is 4.0
m 2 /g. The analytical values of this powder are shown in Table 2. Table 1 Al 2 O 3 powder analysis values Al 2 O 3 content 99.99% Element content (PPM) Mg <5 Cr <10 Si 30 Zn <5 Fe 22 Cu <5 Ca <20 Ni 15 Ti <5 Table 2 AlN powder analysis value AlN content 97.8% Element Content Mg <5 (PPM) Cr 21 ( ) Si 125 ( ) Zn 9 ( ) Fe 20 ( ) Cu <5 ( ) Mn 5 ( ) Ni 27 ( ) Ti <5 ( ) Co <5 ( ) Al 64.8 (wt%) N 33.4 ( ) O 1.1 ( ) C 0.11 ( ) The aluminum nitride powder thus obtained was % of an aqueous solution of a silane coupling agent (A-172, manufactured by Nippon Unicar Co., Ltd.), filtered, and dried under reduced pressure at room temperature. Next, 4% by weight and 0.2% by weight of dicyanodiamide and benzyldimethylamine were added as curing agents to an epoxy resin (Epicoat 1001 manufactured by Schiel Kagaku Co., Ltd.), and the mixture was kneaded at a temperature of 80° C. using a roll kneader. While kneading, 700 parts by weight of the aluminum nitride powder treated with the silane coupling agent was added to 100 parts by weight of the resin and mixed uniformly. The resulting mixture was ground at room temperature and the powder was precured at a pressure of 100 Kg/cm 2 and a temperature of 16° C. for 30 minutes. Then, a curing treatment was performed at a temperature of 180° C. without applying pressure to obtain a sheet with a thickness of 1.2 mm. The thermal conductivity of the obtained sheet was measured using a laser flash method thermal constant measuring device manufactured by Rigaku Denki and was found to be 0.012 cal/cm·sec·K. Example 2 Table 3 shows the results of an experiment conducted in the same manner as in Example 1, but with different blending ratios of epoxy resin and aluminum nitride powder.
【表】
実施例 ３
加熱加硫型のシリコーンゴム100ｇをトリクロ
ロエタン700ｇに溶解させた後実施例１で用いた
ものを同じシランカツプリング剤処理した窒化ア
ルミニウム粉末600ｇを加え均一に撹拌しながら
真空脱泡した。得られたスラリーをポリエチレン
シート上に塗布し乾燥後温度165℃で40分プレス
加硫した。得られた厚さ0.6mmのシートの熱伝導
率は0.010cal／cm・sec・Ｋであつた。
実施例 ４
実施例３で得られたのと同じ、窒化アルミニウ
ム粉末を含むシリコーンゴムスラリーをドクター
ブレード法で約0.3mmの厚さにシート成形し乾燥
した。このシート３枚の各々の間にシランカツプ
リング剤（前記と同じもの）処理をした厚さ0.05
mmのガラスクロス２枚をはさんで165℃で40分プ
レス加硫した。得られた複合シートを作成した。
このシートの熱伝導率は0.010cal／cm・sec・Ｋ
であつた。
実施例 ５
ポリプロピレンホモポリマー（メルトインデツ
クス＝４）100重量部に安定剤
（Butylatehydroxytoluene）0.3重量部および実
施例１で用いたものと同じシランカツプリング剤
処理した窒化アルミニウム粉末650重量部を加え
ブラベンダープラスチコーダーを用いロータ回転
数50rpmで200℃の温度で20分間混練した。これ
を２枚のフエロ板の間にはさみ220℃で10分予熱
後、100Kg／cm2、220℃の条件下で加圧成形して厚
さ1.8mmのシートを作成した。このシートの熱伝
導率は0.007cal／cm・sec・Ｋであつた。[Table] Example 3 After dissolving 100 g of heat-curable silicone rubber in 700 g of trichloroethane, 600 g of aluminum nitride powder treated with the same silane coupling agent used in Example 1 was added, and vacuum decomposition was performed while stirring uniformly. It bubbled. The obtained slurry was applied onto a polyethylene sheet, dried, and then press-vulcanized at a temperature of 165°C for 40 minutes. The thermal conductivity of the obtained sheet with a thickness of 0.6 mm was 0.010 cal/cm·sec·K. Example 4 The same silicone rubber slurry containing aluminum nitride powder as obtained in Example 3 was formed into a sheet with a thickness of about 0.3 mm using a doctor blade method and dried. A thickness of 0.05 silane coupling agent (same as above) was applied between each of these three sheets.
It was press-vulcanized at 165°C for 40 minutes with two pieces of glass cloth of mm size sandwiched in between. The resulting composite sheet was created.
The thermal conductivity of this sheet is 0.010cal/cm・sec・K
It was hot. Example 5 0.3 parts by weight of a stabilizer (butylate hydroxytoluene) and 650 parts by weight of aluminum nitride powder treated with the same silane coupling agent as used in Example 1 were added to 100 parts by weight of polypropylene homopolymer (melt index = 4). The mixture was kneaded using a lavender plasticorder at a rotor speed of 50 rpm and a temperature of 200°C for 20 minutes. This was sandwiched between two ferro plates, preheated at 220°C for 10 minutes, and then pressure-molded at 100 kg/cm 2 and 220°C to produce a sheet with a thickness of 1.8 mm. The thermal conductivity of this sheet was 0.007 cal/cm·sec·K.
第１図は、シリコンゴムに対する窒化アルミニ
ウムの配合割合を変化させた場合の熱伝導性の変
化の状態を示すものであり、図中１の曲線は、本
発明の例、２の曲線は、比較例である。
Figure 1 shows how the thermal conductivity changes when the blending ratio of aluminum nitride to silicone rubber is changed. In the figure, curve 1 is an example of the present invention, and curve 2 is a comparative example. This is an example.
Claims (1)
グ剤で処理された平均粒子径が2μｍ以下で、3μ
ｍ以下の粒子のものを70容量％以上の割合で含有
し、且つ酸素含有量が3.0重量％以下及び純度が
95％以上の窒化アルミニウム粉末とよりなり、前
記有機高分子化合物100重量部に対して、窒化ア
ルミニウム粉末が、300〜1000重量部均一に分散
した組成物よりなる複合シート。1 The average particle diameter treated with () organic polymer compound and () coupling agent is 2 μm or less, and 3 μm
Contains 70% by volume or more of particles with a size of 3.0 m or less, an oxygen content of 3.0% by weight or less, and a purity of
A composite sheet comprising a composition comprising 95% or more of aluminum nitride powder, in which 300 to 1000 parts by weight of the aluminum nitride powder is uniformly dispersed with respect to 100 parts by weight of the organic polymer compound.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59049211A JPS60195160A (en) | 1984-03-16 | 1984-03-16 | Composite sheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP59049211A JPS60195160A (en) | 1984-03-16 | 1984-03-16 | Composite sheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60195160A JPS60195160A (en) | 1985-10-03 |
| JPH0376344B2 true JPH0376344B2 (en) | 1991-12-05 |
Family
ID=12824642
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP59049211A Granted JPS60195160A (en) | 1984-03-16 | 1984-03-16 | Composite sheet |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60195160A (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0651561B2 (en) * | 1986-04-11 | 1994-07-06 | 住友電気工業株式会社 | Aluminum nitride powder |
| US4852646A (en) * | 1987-06-16 | 1989-08-01 | Raychem Corporation | Thermally conductive gel materials |
| JPH01182357A (en) * | 1988-01-14 | 1989-07-20 | Matsushita Electric Works Ltd | Epoxy resin molding material |
| JP2583261B2 (en) * | 1988-01-14 | 1997-02-19 | 電気化学工業株式会社 | filler |
| JPH0668062B2 (en) * | 1988-01-14 | 1994-08-31 | 松下電工株式会社 | Method for producing epoxy resin molding material |
| WO2014208352A1 (en) * | 2013-06-25 | 2014-12-31 | 味の素株式会社 | Resin composition |
| JP6694513B2 (en) * | 2016-08-22 | 2020-05-13 | 富士フイルム株式会社 | Light-shielding composition, light-shielding film, solid-state image sensor, color filter, and liquid crystal display device |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57100148A (en) * | 1980-12-13 | 1982-06-22 | Denki Kagaku Kogyo Kk | Heat dissipating sheet |
-
1984
- 1984-03-16 JP JP59049211A patent/JPS60195160A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57100148A (en) * | 1980-12-13 | 1982-06-22 | Denki Kagaku Kogyo Kk | Heat dissipating sheet |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60195160A (en) | 1985-10-03 |
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