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JP3891969B2 - Thermally conductive grease - Google Patents
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JP3891969B2 - Thermally conductive grease - Google Patents

Thermally conductive grease Download PDF

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JP3891969B2
JP3891969B2 JP2003287620A JP2003287620A JP3891969B2 JP 3891969 B2 JP3891969 B2 JP 3891969B2 JP 2003287620 A JP2003287620 A JP 2003287620A JP 2003287620 A JP2003287620 A JP 2003287620A JP 3891969 B2 JP3891969 B2 JP 3891969B2
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grease
powder
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JP2005054099A (en
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正人 川野
博昭 澤
敏勝 光永
政秀 金子
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Denka Co Ltd
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Denki Kagaku Kogyo KK
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Description

本発明は、発熱性電子部品の放熱材料に適した熱伝導性グリースに関する。   The present invention relates to a thermally conductive grease suitable as a heat dissipation material for a heat-generating electronic component.

近年、発熱性電子部品の高密度化や、携帯用パソコンをはじめとする電子機器の小型、薄型、軽量化に伴い、それらに用いられる放熱部材の低熱抵抗化の要求が益々高まっている。放熱部材としては、シリコーンゴムに熱伝導性無機粉末の充填された硬化物からなる放熱シート、シリコーンゲルに熱伝導性無機粉末が充填され、柔軟性を有する硬化物からなる放熱スペーサー、液状シリコーンに熱伝導性無機粉末の充填された流動性のある放熱グリース、樹脂の相変化を利用したフェーズチェンジ型放熱部材等が例示される。これらのうち、低熱抵抗化が容易なものは、放熱グリース及びフェーズチェンジ型放熱部材であり、低価格の放熱グリースが好んで使用されている。 In recent years, with the increase in the density of heat-generating electronic components and the reduction in size, thickness, and weight of electronic devices such as portable personal computers, there has been an increasing demand for low heat resistance of heat radiating members used therein. The heat radiating member includes a heat radiating sheet made of a cured product in which a silicone rubber is filled with a heat conductive inorganic powder, a heat radiating spacer made of a hardened material having a flexibility and a silicone gel filled with a heat conductive inorganic powder, and a liquid silicone. Examples thereof include fluid heat-dissipating grease filled with a heat conductive inorganic powder, a phase change heat dissipating member utilizing a phase change of a resin, and the like. Among these, those that can be easily reduced in thermal resistance are heat radiation grease and phase change type heat radiation members, and low-cost heat radiation grease is preferably used.

放熱グリースは、シリコーンオイルと熱伝導性無機粉末よりなるが、近年の更なる高熱伝導性向上の要求を受け、熱伝導性無機粉末として窒化アルミニウム粉末を用いたものが提案されている(特許文献1〜3)。しかしながら、窒化アルミニウム粉末は、充填量を多くすると耐湿性が悪くなる問題がある。   The heat dissipating grease is composed of silicone oil and heat conductive inorganic powder. In response to the recent demand for further improvement in heat conductivity, a material using aluminum nitride powder as a heat conductive inorganic powder has been proposed (Patent Literature). 1-3). However, the aluminum nitride powder has a problem that the moisture resistance deteriorates when the filling amount is increased.

一方、放熱グリースを発熱部品と放熱部品との間に挟んで使用する場合においては、ヒートサイクルが長期間繰り返されると、シリコーンオイル成分が分離するいわゆる「離油」が生じ、熱抵抗が上昇してしまう。これを解決するため、特殊なシリコーンを用いたものが提案されているが(特許文献4〜6)、いずれも熱伝導率の小さいものであった。また、放熱グリースを発熱部材と放熱部品との間に使用した場合、密着力が大きく、しかも経時変化により更に大きくなり、一度装着すれば剥離することが困難であったが、この解決法はなかった。
特開2000−109373号公報 特開2000−169873号公報 特許第3142800号公報 特開昭61−157587号公報 特公平6−19027号公報 特開2002−194379号公報
On the other hand, when using heat-dissipating grease sandwiched between a heat-generating component and a heat-dissipating component, if the heat cycle is repeated for a long period of time, so-called "oil separation" occurs in which the silicone oil component separates, increasing the thermal resistance. End up. In order to solve this, those using special silicone have been proposed (Patent Documents 4 to 6), but all of them have low thermal conductivity. In addition, when heat dissipation grease is used between the heat generating member and the heat dissipation component, the adhesive force is large, and it becomes even larger due to changes over time. It was.
JP 2000-109373 A JP 2000-169873 A Japanese Patent No. 3142800 JP-A 61-157487 Japanese Patent Publication No. 6-19027 JP 2002-194379 A

本発明の目的は、上記に鑑み、高熱伝導性、高信頼性かつ使用後の剥離が容易なグリース、特に発熱性電子部品の放熱材料に適した熱伝導性グリースを提供することである。本発明の目的は、低動粘度のシリコーンオイル及び球状アルミナ粉末の微粉と超微粉、窒化アルミニウムの微粉の所定量を充填することによって達成することができる。   In view of the above, an object of the present invention is to provide a grease having high thermal conductivity, high reliability, and easy peeling after use, in particular, a thermal conductive grease suitable for a heat dissipation material for heat-generating electronic components. The object of the present invention can be achieved by filling predetermined amounts of low kinematic viscosity silicone oil, fine and fine powders of spherical alumina powder and fine powder of aluminum nitride.

すなわち、本発明は、室温に於ける動粘度が10〜500mm/sのシリコーンオイル10〜30質量%、平均粒径1μm以上3μm未満の球状アルミナ微粉40〜60質量%、平均粒径1μm以上3μm未満の窒化アルミニウム微粉4〜10質量%、平均粒径0.1μm以上1μm未満の球状アルミナ超微粉10〜30質量%を含有してなることを特徴とする熱伝導性グリースである。この場合において、熱伝導率が2W/mK以上、室温に於けるちょう度が300〜600、アルミニウム材との初期及び120℃×100Hr処理後の剥離強度がいずれも55kPa以下であることが好ましい。 That is, the present invention has a kinematic viscosity at room temperature of 10 to 500 mm 2 / s of silicone oil 10 to 30% by mass, spherical alumina fine powder 40 to 60% by mass with an average particle size of 1 μm to less than 3 μm, and an average particle size of 1 μm or more. A thermal conductive grease comprising 4 to 10% by mass of aluminum nitride fine powder of less than 3 μm and 10 to 30% by mass of spherical alumina ultrafine powder having an average particle size of 0.1 μm or more and less than 1 μm. In this case, it is preferable that the thermal conductivity is 2 W / mK or more, the consistency at room temperature is 300 to 600, and the initial peel strength after treatment with aluminum material and 120 ° C. × 100 Hr is 55 kPa or less.

本発明によれば、高熱伝導性、高信頼性かつ使用後の剥離が容易な熱伝導性グリースが提供される。   ADVANTAGE OF THE INVENTION According to this invention, the heat conductive grease with high heat conductivity, high reliability, and easy peeling after use is provided.

本発明で使用される熱伝導性無機粉末(充填材)は、球状アルミナ粉末及び窒化アルミニウム粉末を必須成分とするが、最大粒径10μm以下の炭化ホウ素粉末、炭化ケイ素粉末、酸化亜鉛、窒化ケイ素、窒化ホウ素、アルミニウム粉末、銅粉末等から選ばれた一種又は二種以上の粉末を、充填材の合計中、10質量%まで含有していてもよい。重要なことは、球状アルミナ粉末の微粉と超微粉及び窒化アルミニウム粉末の微粉を併用することであり、それによって高熱伝導性と高流動性を両立させることができる。   The thermally conductive inorganic powder (filler) used in the present invention contains spherical alumina powder and aluminum nitride powder as essential components, but boron carbide powder, silicon carbide powder, zinc oxide, silicon nitride having a maximum particle size of 10 μm or less. , Boron nitride, aluminum powder, copper powder or the like may be contained in one or more powders up to 10% by mass in the total of the filler. What is important is to use a fine powder of spherical alumina powder, a super fine powder, and a fine powder of aluminum nitride powder in combination, thereby achieving both high thermal conductivity and high fluidity.

本発明において充填材は、熱伝導性グリースの動きをスムーズ化し、使用後の剥離性を容易とするため、平均粒径の異なる3種類又はそれ以上の粉末が使用される。すなわち、平均粒径0.2μm以上1μm未満、好ましくは0.4〜0.6μmの球状アルミナ超微粉と、平均粒径1〜3μm、最大粒径2〜10μm、好ましくは平均粒径1〜2μm、最大粒径2〜5μmの球状アルミナ微粉と、平均粒径1〜3μm、最大粒径2〜10μm、好ましくは平均粒径1〜2μm、最大粒径2〜5μmの窒化アルミニウム微粉が必須の充填材となる。   In the present invention, three or more kinds of powders having different average particle diameters are used as the filler in order to smooth the movement of the heat conductive grease and facilitate the peelability after use. That is, a spherical alumina ultrafine powder having an average particle size of 0.2 μm or more and less than 1 μm, preferably 0.4 to 0.6 μm, an average particle size of 1 to 3 μm, a maximum particle size of 2 to 10 μm, preferably an average particle size of 1 to 2 μm Filling with spherical alumina fine powder having a maximum particle size of 2 to 5 μm and an average particle size of 1 to 3 μm and a maximum particle size of 2 to 10 μm, preferably an aluminum nitride fine powder having an average particle size of 1 to 2 μm and a maximum particle size of 2 to 5 μm Become a material.

球状アルミナ超微粉の平均粒径が0.2μm未満ではグリースの粘度が高くなりすぎて薄化し難くなり、1μm以上では充填性が悪く、グリースにした時の粘度が高くなり、剥離性も悪化する。一方、球状アルミナ微粉及び窒化アルミニウム微粉の平均粒径が1μm未満であるか、又は最大粒径が2μm未満であると、熱伝導性無機粉末粒子間の接触点数が多くなりすぎて更なる高熱伝導性を発現しない。また、球状アルミナ微粉及び窒化アルミニウム微粉の平均粒径が3μmをこえるか、又は最大粒径が10μmをこえると、グリースが薄肉し過ぎ、低熱抵抗化が困難となる。更には、充填材として窒化アルミニウム粉を併用しないと、シリコーンオイルが流れ出し、低熱抵抗化が困難となる。   If the average particle size of the spherical alumina ultrafine powder is less than 0.2 μm, the viscosity of the grease will be too high and it will be difficult to thin, and if it is 1 μm or more, the filling property will be poor, the viscosity when made into grease will be high, and the peelability will also deteriorate. . On the other hand, when the average particle size of the spherical alumina fine powder and the aluminum nitride fine powder is less than 1 μm, or the maximum particle size is less than 2 μm, the number of contact points between the heat conductive inorganic powder particles becomes too large, and further high heat conduction is achieved. Does not express sex. On the other hand, if the average particle size of the spherical alumina fine powder and the aluminum nitride fine powder exceeds 3 μm, or the maximum particle diameter exceeds 10 μm, the grease becomes too thin and it is difficult to reduce the thermal resistance. Furthermore, if aluminum nitride powder is not used as a filler, silicone oil will flow out, making it difficult to reduce the thermal resistance.

本発明の熱伝導性グリースは、上記充填材の含有率が70〜90質量%、シリコーンオイルの含有率が10〜30質量%であることが好ましい。充填材の含有率が70質量%未満であると、熱伝導率が低く、いくら薄化しても低熱抵抗化は困難となる。また、充填材の含有率が90質量%をこえると、グリースの粘度が高くなり、使用後の剥離性が悪化する。特に好適な充填材の構成割合は、球状アルミナ微粉40〜60質量%、窒化アルミニウム微粉4〜10質量%、球状アルミナ超微粉10〜30質量%である。   In the heat conductive grease of the present invention, the content of the filler is preferably 70 to 90% by mass, and the content of silicone oil is preferably 10 to 30% by mass. When the content of the filler is less than 70% by mass, the thermal conductivity is low, and it is difficult to reduce the thermal resistance no matter how thin the filler is. Moreover, when the content rate of a filler exceeds 90 mass%, the viscosity of grease will become high and the peelability after use will deteriorate. The composition ratio of a particularly preferable filler is 40 to 60% by mass of spherical alumina fine powder, 4 to 10% by mass of aluminum nitride fine powder, and 10 to 30% by mass of spherical alumina ultrafine powder.

球状アルミナ微粉は、グリースの流動性を得るための必須成分であり、40質量%未満ではグリースの流動性が低下し、薄化が困難となる。60質量%をこえると、グリースの粘度が高くなりすぎて薄化が困難となる。窒化アルミニウム微粉は、熱伝導性を向上させるための必須成分であり、4質量%未満では熱伝導率の向上が認められず、10質量%をこえるとグリースの粘度が高くなりすぎて薄化が困難となり、いずれの場合とも低熱抵抗化が困難となる。球状アルミナ超微粉は、球状アルミナ微粉及び窒化アルミニウム微粉の粒子と粒子の隙間を埋め、熱伝導性を一段と向上させるための成分であり、10質量%未満ではその効果が認められず、30質量%をこえるとグリースの粘度が高くなりすぎて薄化が困難となる。 The spherical alumina fine powder is an essential component for obtaining the fluidity of the grease, and if it is less than 40% by mass, the fluidity of the grease is lowered and it is difficult to make it thin. When it exceeds 60% by mass, the viscosity of the grease becomes too high and thinning becomes difficult. Aluminum nitride fine powder is an essential component for improving the thermal conductivity, and if it is less than 4% by mass, no improvement in thermal conductivity is observed. If it exceeds 10% by mass, the viscosity of the grease becomes too high and thinning occurs. In either case, it is difficult to reduce the thermal resistance. Spherical alumina ultrafine powder is a component for filling the gap between the particles of spherical alumina fine powder and aluminum nitride fine powder to further improve the thermal conductivity, and the effect is not recognized at less than 10% by mass, and 30% by mass. Beyond that, the viscosity of the grease becomes too high, making it difficult to thin it.

充填材の主材質が、球状アルミナ粉と窒化アルミニウム粉の混合粉ではなく、例えば窒化ケイ素、窒化ホウ素、酸化亜鉛、酸化珪素粉末であると、球形度と熱伝導性のバランスが悪くなることによって、熱伝導性と流動性を両立させることができない。充填材の形状は、角状でもよいが、球形度が高いほど流動性は高く、剥離性も向上するので、本発明では平均球形度が0.8以上、特に0.85以上が好ましい。   If the main material of the filler is not a mixed powder of spherical alumina powder and aluminum nitride powder, but, for example, silicon nitride, boron nitride, zinc oxide, or silicon oxide powder, the balance between sphericity and thermal conductivity will deteriorate. , Heat conductivity and fluidity cannot be achieved at the same time. The shape of the filler may be square, but the higher the sphericity, the higher the fluidity and the better the peelability. Therefore, in the present invention, the average sphericity is preferably 0.8 or more, particularly preferably 0.85 or more.

平均球形度は、実体顕微鏡、例えば「モデルSMZ−10型」(ニコン社製)、走査型電子顕微鏡等にて撮影した粒子像を画像解析装置、例えば(日本アビオニクス社製など)に取り込み、次のようにして測定することができる。すなわち、写真から粒子の投影面積(A)と周囲長(PM)を測定する。周囲長(PM)に対応する真円の面積を(B)とすると、その粒子の真円度はA/Bとして表示できる。そこで、試料粒子の周囲長(PM)と同一の周囲長を持つ真円を想定すると、PM=2πr、B=πrであるから、B=π×(PM/2π)となり、個々の粒子の球形度は、球形度=A/B=A×4π/(PM)として算出することができる。このようにして得られた任意の粒子200個の球形度を求めその平均値を平均球形度とした。 The average sphericity is obtained by taking a particle image taken with a stereomicroscope such as “Model SMZ-10” (Nikon Corporation), a scanning electron microscope or the like into an image analyzer such as Nihon Avionics Co., Ltd. It can measure as follows. That is, the projected area (A) and the perimeter (PM) of particles are measured from a photograph. When the area of a perfect circle corresponding to the perimeter (PM) is (B), the roundness of the particle can be displayed as A / B. Therefore, assuming a perfect circle having the same circumference as the sample particle (PM), PM = 2πr and B = πr 2 , so that B = π × (PM / 2π) 2 , and each particle Can be calculated as sphericity = A / B = A × 4π / (PM) 2 . The sphericity of 200 arbitrary particles thus obtained was determined, and the average value was defined as the average sphericity.

本発明で用いられるシリコーンオイルは、低動粘度であることが要求され、室温に於ける動粘度が10〜500mm/s、好ましくは30〜100mm/sである。これをマトリックスとすることによって流動性の高い熱伝導性グリースが得られる。シリコーンオイルの割合は、熱伝導性グリース中、10〜30質量%であることが好ましい。10質量%未満では、グリースの流動性が乏しく薄化できない。30質量%をこえると、グリースの熱伝導性が低く、低熱抵抗が得られない。シリコーンオイルは、一般にジメチルシリコーンオイル、メチルフェニルシリコーンオイル、変性シリコーンオイルと呼ばれるものが使用でき、市販品がある。 The silicone oil used in the present invention is required to have a low kinematic viscosity, and has a kinematic viscosity at room temperature of 10 to 500 mm 2 / s, preferably 30 to 100 mm 2 / s. By using this as a matrix, a highly fluid thermal conductive grease can be obtained. The proportion of silicone oil is preferably 10 to 30% by mass in the heat conductive grease. If it is less than 10 mass%, the fluidity of the grease is poor and cannot be thinned. If it exceeds 30% by mass, the thermal conductivity of the grease is low and low thermal resistance cannot be obtained. As the silicone oil, those generally called dimethyl silicone oil, methylphenyl silicone oil, and modified silicone oil can be used, and there are commercially available products.

本発明の熱伝導性グリースは、熱伝導率が高いことが望ましく、2W/mK以上、特に3W/mK以上であることが好ましい。このような高熱伝導化は、上記必須充填材の粒度と配合比率を適正化することによって達成することができる。  The heat conductive grease of the present invention desirably has a high heat conductivity, and preferably 2 W / mK or more, particularly 3 W / mK or more. Such high thermal conductivity can be achieved by optimizing the particle size and blending ratio of the essential filler.

本発明の熱伝導性グリースのちょう度は高いことが望ましく、300〜600、特に350〜500であることが好ましい。300未満では、グリースが均一に塗布できずに熱抵抗が大きくなり、600をこえると、電子機器を使用中にグリースがCPUと放熱フィンの間から流れ出し、使用中に熱抵抗が大きくなる。このような、熱伝導性グリースは、低動粘度のシリコーンオイルを用いることによって製造することができる。  The consistency of the heat conductive grease of the present invention is desirably high, and is preferably 300 to 600, particularly 350 to 500. If it is less than 300, grease cannot be applied uniformly and the thermal resistance increases, and if it exceeds 600, the grease flows out from between the CPU and the heat radiating fin during use of the electronic device, and the thermal resistance increases during use. Such a heat conductive grease can be manufactured by using a silicone oil having a low kinematic viscosity.

更には、本発明の熱伝導性グリースは、アルミニウム材との剥離強度が小さいことが好ましく、初期及び120℃×100Hr処理後の剥離強度がいずれも55kPa以下、特に30kPa以下であることが好ましい。剥離強度がいずれも55kPaをこえると、放熱フィンを取りはずす時に、グリースとCPUとの接着力が強すぎて、CPUが基板から外れてしまう。このような、熱伝導性グリースは、上記充填材と低動粘度シリコーンオイルの配合比率を適正化することによって製造することができる。  Furthermore, the thermal conductive grease of the present invention preferably has a small peel strength from the aluminum material, and the peel strength after the initial treatment and 120 ° C. × 100 Hr treatment is preferably 55 kPa or less, particularly preferably 30 kPa or less. If the peel strength exceeds 55 kPa, the adhesive force between the grease and the CPU is too strong when the heat dissipating fin is removed, and the CPU comes off the substrate. Such a heat conductive grease can be manufactured by optimizing the blending ratio of the filler and the low kinematic viscosity silicone oil.

本発明の熱伝導性グリースは、上記材料を万能混合攪拌機、ニーダー等で混練りすることによって製造することができる。   The heat conductive grease of the present invention can be produced by kneading the above materials with a universal mixer and kneader.

実施例1〜6
表1に示される充填材{窒化アルミニウム微粉(トクヤマ社製商品名「Hグレード」)、球状アルミナ微紛(住友化学工業社製商品名「AA−2」)、及び球状アルミナ超微紛(住友化学工業社製商品名「AA−05」)}と、表2に示される室温動粘度が10〜500mm/sの範囲にある各種シリコーンオイル(東芝シリコーン社製商品名「TSF451−10」、「TSF451−50」、「TSF451−100」、「TSF451−350」、「TSF451−500」、「TSF4445」)を準備した。これらを表3の割合で配合し、30分間混合しながら真空脱泡して熱伝導性グリースを製造した。
Examples 1-6
Fillers shown in Table 1 {Aluminum nitride fine powder (trade name “H grade” manufactured by Tokuyama Co., Ltd.), spherical alumina fine powder (trade name “AA-2” manufactured by Sumitomo Chemical Co., Ltd.), and spherical alumina super fine powder (Sumitomo) Chemical industry trade name “AA-05”)} and various silicone oils having a room temperature kinematic viscosity in the range of 10 to 500 mm 2 / s shown in Table 2 (trade names “TSF451-10” made by Toshiba Silicone, “TSF451-50”, “TSF451-100”, “TSF451-350”, “TSF451-500”, “TSF4445”) were prepared. These were blended in the proportions shown in Table 3 and vacuum degassed while mixing for 30 minutes to produce a thermally conductive grease.

比較例1
球状アルミナ微紛のかわりに、角取り状アルミナ紛(住友化学社製商品名「AA−7」)を用いたこと以外は、実施例1と同様にしてグリースを製造した。
Comparative Example 1
Grease was produced in the same manner as in Example 1 except that a chamfered alumina powder (trade name “AA-7” manufactured by Sumitomo Chemical Co., Ltd.) was used instead of the spherical alumina fine powder.

比較例2
窒化アルミニウム微紛のかわりに、平均粒径10μmの市販窒化アルミニウム粉(東洋アルミニウム社製商品名「TOYALNITE FL」)を用いたこと以外は、実施例1と同様にしてグリースを製造した。
Comparative Example 2
Grease was produced in the same manner as in Example 1 except that a commercial aluminum nitride powder (trade name “TOYALNITE FL” manufactured by Toyo Aluminum Co., Ltd.) having an average particle diameter of 10 μm was used instead of the aluminum nitride fine powder.

比較例3
球状アルミナ超微紛のかわりに、非球状の住友化学社製商品名「AKP−G008」を用いたこと以外は、実施例1と同様にしてグリースを製造した。
Comparative Example 3
Grease was produced in the same manner as in Example 1 except that non-spherical Sumitomo Chemical trade name “AKP-G008” was used instead of spherical alumina superfine powder.

比較例4〜6
充填材を表3に示す割合で配合したこと以外は、実施例1に準じてグリースを製造した。
Comparative Examples 4-6
A grease was produced in accordance with Example 1 except that the filler was blended in the ratio shown in Table 3.

比較例7、8
シリコーンオイルとして、表2に示されるGE東芝シリコーン社製商品名「TSF451−10」(室温動粘度7mm/s)、「TSF4445」(室温動粘度800mm/s)を用いたこと以外は、実施例1と同様にしてグリースを製造した。
Comparative Examples 7 and 8
Except for using GE Toshiba Silicone product names “TSF451-10” (room temperature kinematic viscosity 7 mm 2 / s) and “TSF4445” (room temperature kinematic viscosity 800 mm 2 / s) shown in Table 2 as the silicone oil, A grease was produced in the same manner as in Example 1.

得られたグリースの熱伝導率、ちょう度、剥離強度と、充填材の平均粒径及び最大粒径を以下に従って測定した。それらの結果を表4に示す。
(1)熱伝導率:先端が□10mmのヒーターの埋め込まれた銅製治具と、□10mmの銅製冷却治具との間に試料(グリース)約0.5cmを挟み、4.2kgの荷重を掛けてセットする。なお、試料量は、セット面全体を埋めるのに十分な量であり、セット部分からはみ出した状態となる。ヒーターに電力20Wをかけて30分間保持し、銅製ヒーターケースと銅板との温度差(℃)を測定し、式、熱抵抗(℃/W)=温度差(℃)/電力(W)、により算出した。
The thermal conductivity, consistency, peel strength, average particle size and maximum particle size of the filler were measured according to the following. The results are shown in Table 4.
(1) Thermal conductivity: A sample (grease) of about 0.5 cm 3 is sandwiched between a copper jig embedded with a heater with a 10 mm tip and a 10 mm copper cooling jig, and a load of 4.2 kg Multiply and set. Note that the sample amount is sufficient to fill the entire set surface, and is in a state of protruding from the set portion. Hold the heater with electric power of 20W and hold it for 30 minutes, measure the temperature difference (° C) between the copper heater case and the copper plate, and use the formula: Calculated.

(2)ちょう度:JIS K 2220に準拠した方法で測定した。   (2) Consistency: Measured by a method based on JIS K 2220.

(3)剥離強度:30×30mmサイズのアルミニウム板2枚の間に、試料約0.2mlを均一に塗布して挟み、120℃×100時間加熱後冷却し、剥離強度を測定した。また、初期の剥離強度は、加熱処理を行わずに測定した。   (3) Peel strength: About 0.2 ml of the sample was uniformly coated between two 30 × 30 mm size aluminum plates, cooled after heating at 120 ° C. for 100 hours, and the peel strength was measured. Further, the initial peel strength was measured without performing heat treatment.

(4)充填材の平均粒径と最大粒径:L&N社製粒度分布計「マイクロトラックSP−A」を用いて測定した。   (4) Average particle size and maximum particle size of filler: measured using a particle size distribution meter “Microtrac SP-A” manufactured by L & N.

Figure 0003891969
Figure 0003891969

Figure 0003891969
Figure 0003891969

Figure 0003891969
Figure 0003891969

Figure 0003891969
Figure 0003891969

表に示すとおり、特定動粘度のシリコーンオイルに、特定粒径の窒化アルミニウム微粉、球状アルミナ微紛、球状アルミナ超微粉を充填材として充填された本発明の熱伝導性グリースは、比較例のグリースに比べて著大な熱伝導率が達成され、しかも剥離強度が低くなった。   As shown in the table, the heat conductive grease of the present invention filled with a specific kinematic viscosity silicone oil as a filler with a specific particle size of aluminum nitride fine powder, spherical alumina fine powder, and spherical alumina ultrafine powder is a grease of a comparative example. Compared to the above, a remarkable thermal conductivity was achieved, and the peel strength was low.

本発明の熱伝導性グリースの用途としては、電子部品の放熱部材、熱伝導性充填剤、温度測定用等の絶縁性充填剤等がある。たとえば、本発明の熱伝導性グリースは、MPUやパワートランジスタ、トランス等の発熱性電子部品からの熱を放熱フィンや放熱ファン等の放熱部品に伝熱させるために使用され、発熱性電子部品と放熱部品の間に挟み込まれて使用される。これによって、発熱性電子部品と放熱部品間の伝熱が良好となり、長期的に発熱性電子部品の誤作動を軽減させることができる。 Applications of the heat conductive grease of the present invention include heat dissipating members for electronic parts, heat conductive fillers, insulating fillers for temperature measurement, and the like. For example, the thermally conductive grease of the present invention is used to transfer heat from heat-generating electronic components such as MPUs, power transistors, and transformers to heat-dissipating components such as heat-dissipating fins and heat-dissipating fans. Used by being sandwiched between heat dissipation components. As a result, heat transfer between the heat-generating electronic component and the heat-dissipating component is improved, and malfunction of the heat-generating electronic component can be reduced in the long term.

Claims (2)

室温に於ける動粘度が10〜500mm/sのシリコーンオイル10〜30質量%、平均粒径1μm以上3μm未満の球状アルミナ微粉40〜60質量%、平均粒径1μm以上3μm未満の窒化アルミニウム微粉4〜10質量%、平均粒径0.1μm以上1μm未満の球状アルミナ超微粉10〜30質量%を含有してなることを特徴とする熱伝導性グリース。 10-30 mass% of silicone oil having a kinematic viscosity at room temperature of 10-500 mm 2 / s, 40-60 mass% of spherical alumina fine powder having an average particle diameter of 1 μm or more and less than 3 μm, and aluminum nitride fine powder having an average particle diameter of 1 μm or more and less than 3 μm A thermal conductive grease comprising 10 to 30% by mass of spherical alumina ultrafine powder having an average particle diameter of 4 to 10% by mass and an average particle size of 0.1 to 1 μm. 熱伝導率が2W/mK以上、室温に於けるちょう度が300〜600であり、アルミニウム材との初期及び120℃×100Hr処理後の剥離強度がいずれも55kPa以下であることを特徴とする請求項1記載の熱伝導性グリース。 The thermal conductivity is 2 W / mK or more, the consistency at room temperature is 300 to 600, and the initial peel strength after treatment with an aluminum material and after 120 ° C. × 100 Hr treatment is 55 kPa or less. Item 2. The thermally conductive grease according to Item 1.
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