JP2014105297A - Sheet-like molded body - Google Patents
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- JP2014105297A JP2014105297A JP2012260219A JP2012260219A JP2014105297A JP 2014105297 A JP2014105297 A JP 2014105297A JP 2012260219 A JP2012260219 A JP 2012260219A JP 2012260219 A JP2012260219 A JP 2012260219A JP 2014105297 A JP2014105297 A JP 2014105297A
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本発明は電子機器・部品の放熱材料として好適に使用することができるシート状成形体に関する。詳しくは、電気絶縁性を有し、かつ熱伝導性に優れ、しかも、柔軟性にも優れたシート状成形体を提供するものである。 The present invention relates to a sheet-like molded body that can be suitably used as a heat dissipation material for electronic devices and parts. Specifically, the present invention provides a sheet-like molded article having electrical insulation, excellent thermal conductivity, and excellent flexibility.
近年、半導体デバイスのパワー密度上昇に伴い、デバイスに使用される材料には、より高度な放熱特性が求められている。このような材料として、サーマルインターフェースマテリアルと呼ばれる一連の材料があり、その使用量は急速に拡大している。サーマルインターフェースマテリアルとは、半導体素子から発生する熱をヒートシンクまたは筐体等に逃がす経路の熱抵抗を緩和するための材料であり、シート、ゲル、グリースなど多様な形態が用いられる。一般に、サーマルインターフェースマテリアルは、熱伝導性フィラーをエポキシやシリコーンの様な樹脂に分散した複合材料であり、フィラーとしては金属酸化物が多く用いられている。しかし、上記金属酸化物を用いた複合材料により成形されるシート状成形体は、厚み方向の熱伝導率が１〜３Ｗ／ｍ・Ｋ程度に留まるものであり、より高い熱伝導率を有するシート状成形体が要求されている。 In recent years, with the increase in power density of semiconductor devices, materials used for devices are required to have higher heat dissipation characteristics. As such a material, there is a series of materials called thermal interface materials, and the amount of use is rapidly expanding. The thermal interface material is a material for relaxing the thermal resistance of the path through which heat generated from the semiconductor element is released to the heat sink or the housing, and various forms such as a sheet, gel, and grease are used. Generally, the thermal interface material is a composite material in which a thermally conductive filler is dispersed in a resin such as epoxy or silicone, and a metal oxide is often used as the filler. However, the sheet-like molded body molded from the composite material using the metal oxide has a thermal conductivity in the thickness direction of about 1 to 3 W / m · K, and has a higher thermal conductivity. A shaped molded body is required.
このため、上記成形体の製造に使用する複合材料として、熱伝導率の大きな鱗片状窒化硼素粉末と粒形状の金属酸化物で構成させる熱伝導性フィラーを樹脂に充填したものが提案されている（特許文献１参照）。 For this reason, as a composite material used for manufacturing the molded body, a material in which a resin is filled with a heat conductive filler composed of a scaly boron nitride powder having a high heat conductivity and a metal oxide in a grain shape has been proposed. (See Patent Document 1).
しかし、鱗片状窒化硼素粉末と粒形状の金属酸化物で構成させる熱伝導性フィラーを樹脂に分散した複合材料では、鱗片状窒化硼素粉末を多量に必要とし、そのため、樹脂との混合時の粘度上昇が起こり、これをシート状に成形する際の作業性が著しく低下するという問題が発生する。 However, a composite material in which a thermally conductive filler composed of scaly boron nitride powder and a particle-shaped metal oxide is dispersed in a resin requires a large amount of scaly boron nitride powder, and therefore the viscosity when mixed with the resin A rise occurs, and the problem that workability when forming the sheet into a sheet shape is significantly reduced.
また、鱗片状窒化硼素粉末の平均長径は、前記粒形状の金属酸化物の平均粒径より大きい場合が多く、該鱗片状窒化硼素粉末粒子がシートに成形した後に横方向に配向し易く、結果として、得られるシート状成形体の熱伝導率を十分向上することができなかったり、また、平面方向における熱伝導率のバラツキが大きくなるという問題が起こる。また、金属酸化物は、それ自体の熱伝導率が低いため、鱗片状窒化硼素粉末と混合して複合材料を構成しても、高い熱伝導性を有するシート状成形体を得ることが困難となる。 In addition, the average major axis of the scaly boron nitride powder is often larger than the average particle diameter of the grain-shaped metal oxide, and the scaly boron nitride powder particles are easily oriented in the lateral direction after being formed into a sheet. As a result, there arises a problem that the thermal conductivity of the obtained sheet-like molded product cannot be sufficiently improved, and the variation of the thermal conductivity in the planar direction becomes large. Further, since the metal oxide itself has a low thermal conductivity, it is difficult to obtain a sheet-like molded body having high thermal conductivity even if it is mixed with flaky boron nitride powder to constitute a composite material. Become.
従って、本発明の目的は、高い熱伝導性と柔軟性とを有し、縁放熱材料に好適に使用できるシート状成形体を提供することにある。 Accordingly, an object of the present invention is to provide a sheet-like molded body that has high thermal conductivity and flexibility and can be suitably used as an edge heat dissipation material.
本発明者らは上記問題点を解決すべく鋭意研究を重ねた結果、シート状成形体の原料となる前記複合材料の熱伝導性フィラーとして、それ自体が熱伝導性の高い窒化アルミニウム粉末と、鱗片状窒化硼素粉末とを使用し、且つ、上記鱗片状窒化硼素粉末を特定割合で含有せしめると共に、該鱗片状窒化硼素粉末の粒子の一定の割合以上が、特定の方向に配向した状態でシート状成形体中に存在するようにシート状成形体を構成することにより、前記目的を達成できることを見出し、本発明を完成するに至った。 As a result of intensive studies to solve the above problems, the inventors of the present invention, as a heat conductive filler of the composite material that is a raw material of the sheet-like molded body, itself an aluminum nitride powder having high heat conductivity, A sheet in which a scaly boron nitride powder is used and the scaly boron nitride powder is contained in a specific ratio, and a certain ratio or more of the scaly boron nitride powder particles are oriented in a specific direction. The present inventors have found that the object can be achieved by configuring the sheet-like molded body so as to exist in the shaped-molded body, and have completed the present invention.
すなわち、本発明は、鱗片状窒化硼素粉末と窒化アルミニウム粉末とを含む熱伝導性フィラーを、基材樹脂１００重量部に対して１００〜１０００重量部の割合で含有する樹脂組成物より成形されたシート状成形体であって、前記熱伝導性フィラー中に鱗片状窒化硼素粉末が１０〜３０質量部％の割合で含有され、且つ、前記シート状成形体中の鱗片状窒化硼素粉末は、個数割合で７０％以上の粒子が、該シート状成形体のシート面に対して、その結晶面が３０〜９０度の角度を成した状態で存在することを特徴とするシート状成形体である。 That is, this invention was shape | molded from the resin composition which contains the heat conductive filler containing scaly boron nitride powder and aluminum nitride powder in the ratio of 100-1000 weight part with respect to 100 weight part of base resin. It is a sheet-like molded article, and the flaky boron nitride powder is contained in the thermally conductive filler in a ratio of 10 to 30 parts by mass, and the flaky boron nitride powder in the sheet-like molded article is It is a sheet-like molded body characterized in that 70% or more of the particles are present in a state where the crystal plane forms an angle of 30 to 90 degrees with respect to the sheet surface of the sheet-like molded body.
上記シート状成形体において、窒化アルミニウム粉末は、平均粒子径が１〜１００μｍのものが、また、鱗片状窒化硼素粉末は、その平均長径が、上記窒化アルミニウム粉末の平均粒子径に対して０．０２〜１の大きさを有するものであることが好ましい。 In the sheet-like molded body, the aluminum nitride powder has an average particle diameter of 1 to 100 μm, and the scaly boron nitride powder has an average major axis of 0. 0 relative to the average particle diameter of the aluminum nitride powder. It is preferable that it has a size of 02-1.
本発明によれば、窒化アルミニウム粉末の優れた熱伝導性と、成形体中における鱗片状窒化硼素粉末の配向の制御による熱伝導性の向上効果とにより、熱伝導性フィラーの少ない添加量で、良好な熱伝導性と柔軟性とを有し、電子部品放熱用として好適に使用することができるシート状成形体を提供することができる。 According to the present invention, due to the excellent thermal conductivity of the aluminum nitride powder and the effect of improving the thermal conductivity by controlling the orientation of the flaky boron nitride powder in the molded body, with a small addition amount of the thermal conductive filler, It is possible to provide a sheet-like molded body that has good thermal conductivity and flexibility and can be suitably used for heat dissipation of electronic components.
一般に、前記鱗片状窒化硼素粉末の厚み方向の熱伝導率は１〜２Ｗ／ｍ・Ｋ程度、面方向の熱伝導率は１００〜２００Ｗ／ｍ・Ｋ程度であり、上記本発明の効果は、鱗片状窒化硼素粉末が特定の方向に配向することによって、窒化アルミニウムと鱗片状窒化硼素粉末との熱の伝達が良好となることにより発現するものと思われる。 In general, the scaly boron nitride powder has a thermal conductivity in the thickness direction of about 1 to 2 W / m · K, and a thermal conductivity in the plane direction of about 100 to 200 W / m · K. It appears that the scale-like boron nitride powder is oriented in a specific direction to improve heat transfer between aluminum nitride and the scale-like boron nitride powder.
また、上記本発明のシート状成形体は、熱伝導性フィラー、特に、鱗片状窒化硼素粉末の添加量の低減により、その成形時における樹脂の粘度上昇を低く抑えることができ、製造時の作業性を改善することができるというメリットをも有する。 In addition, the sheet-like molded product of the present invention can suppress an increase in the viscosity of the resin during molding by reducing the amount of heat conductive filler, in particular, flaky boron nitride powder, and the work during production It has the merit that it can improve the property.
本発明において、シート状成形体を成形するための複合材料中に充填される熱伝導性フィラーは、窒化アルミニウム粉末と鱗片状窒化硼素とを含む。 In this invention, the heat conductive filler with which the composite material for shape | molding a sheet-like molded object is filled contains aluminum nitride powder and scaly boron nitride.
上記窒化アルミニウム粉末は、公知のものが特に制限無く、還元窒化法、直接窒化法など公知の方法によって得られるものを使用することができる。上記窒化アルミニウム粉末の平均粒子径が１〜１００μｍ、好ましくは、５〜８０μｍのものが好適に使用される。また、その熱伝導率は、本発明の目的より、高いほど好ましく、１００Ｗ／ｍ・Ｋ以上、好ましくは、１２０〜２８０Ｗ／ｍ・Ｋのものが好適に使用される。 The aluminum nitride powder is not particularly limited, and those obtained by a known method such as a reduction nitriding method or a direct nitriding method can be used. The average particle diameter of the said aluminum nitride powder is 1-100 micrometers, Preferably, the thing of 5-80 micrometers is used suitably. Further, the higher the thermal conductivity, the more preferable it is for the purpose of the present invention, and a thermal conductivity of 100 W / m · K or more, preferably 120 to 280 W / m · K is preferably used.
また、前記鱗片状窒化硼素粉末は、公知のものが特に制限無く使用されるが、前記窒化アルミニウム粉末の平均粒子径に対して、平均長径が０．０２〜１、特に、０．０２５〜０．５の大きさを有するものであることが好ましい。即ち、上記鱗片状窒化硼素粉末の平均長径が、上記窒化アルミニウム粉末の平均粒子径に対して０．０２未満の場合には混合時の粘度が上昇し、作業性が低下する。鱗片状窒化硼素粉末の平均長径が、上記窒化アルミニウム粉末の平均粒子径に対して１．０を超える場合には、鱗片状窒化硼素粉末粒子の結晶面が横方向に配向し易くなり、結果として、シート状成形体の熱伝導率が低下したり、熱伝導率のバラツキが大きい等の問題が起こる場合がある。従って、窒化アルミニウム粉末の平均粒径に対して前記範囲の平均長径を有する鱗片状窒化硼素粉末を使用することにより、後述の成形において、後述する鱗片状窒化硼素粉末の個々の粒子の結晶面を特定の方向に配向し易くなる。 As the flaky boron nitride powder, known ones are used without particular limitation, but the average major axis is 0.02-1, particularly 0.025-0, relative to the average particle diameter of the aluminum nitride powder. Preferably it has a size of .5. That is, when the average long diameter of the flaky boron nitride powder is less than 0.02 with respect to the average particle diameter of the aluminum nitride powder, the viscosity at the time of mixing increases and the workability decreases. When the average major axis of the flaky boron nitride powder exceeds 1.0 with respect to the average particle diameter of the aluminum nitride powder, the crystal plane of the flaky boron nitride powder particles is easily oriented in the lateral direction, and as a result In some cases, the thermal conductivity of the sheet-like molded product may decrease, or the thermal conductivity may vary greatly. Therefore, by using the flaky boron nitride powder having an average major axis in the above range relative to the average particle diameter of the aluminum nitride powder, the crystal planes of the individual particles of the flaky boron nitride powder described later can be obtained in the molding described later. It becomes easy to orient in a specific direction.
前記熱伝導性フィラーは、前記成分の他に、本発明に著しく影響を与えない範囲で、前記金属酸化物などのフィラーを含有しても良い。 In addition to the above components, the thermally conductive filler may contain a filler such as the metal oxide as long as it does not significantly affect the present invention.
本発明において、熱伝導性フィラーは、鱗片状窒化硼素粉末を１０質量部％以上、特に、１５質量％以上の割合で含有することが、後述する熱伝導性フィラーの添加量において、得られるシート状成形体の熱伝導性の向上効果を十分発揮するために好ましい。但し、上記割合が多くなり過ぎると、他の熱伝導性フィラーの粒子との関係で、後述する鱗片状窒化硼素粉末の個々の粒子の結晶面を特定の方向に配向し難くなり、成形して得られるシート状成形体の厚み方向の熱伝導性を十分向上することが困難となる傾向があるため、３０質量％以下、特に、２５質量％以下の含有割合となるように調整することが好ましい。 In the present invention, the thermally conductive filler contains scaly boron nitride powder in an amount of 10 parts by mass or more, particularly 15% by mass or more, in the amount of the thermally conductive filler described later, the sheet obtained This is preferable in order to sufficiently exhibit the effect of improving the thermal conductivity of the shaped molded body. However, if the ratio is too large, it becomes difficult to orient the crystal planes of the individual particles of the scaly boron nitride powder to be described later in a specific direction because of the relationship with the other thermally conductive filler particles. Since it tends to be difficult to sufficiently improve the thermal conductivity in the thickness direction of the obtained sheet-like molded body, it is preferable to adjust the content ratio to 30% by mass or less, particularly 25% by mass or less. .
本発明で使用される基材樹脂は特に限定されないが、具体的には、ポリエチレン、ポリプロピレン、エチレン−プロピレン共重合体、ポリメチルペンテン、ポリ塩化ビニル、ポリ塩化ビニリデン、ポリ酢酸ビニル、エチレン−酢酸ビニル共重合体、ポリビニルアルコール、ポリアセタール、フッ素樹脂（ポリフッ化ビニリデン、ポリテトラフルオロエチレン等）、ポリエチレンテレフタレート、ポリブチレンテレフタレート、ポリエチレン２，６ナフタレート、ポリスチレン、ポリアクリロニトリル、スチレン−アクリロニトリル共重合体、ＡＢＳ樹脂、ポリフェニレンエーテル（ＰＰＥ）樹脂、変性ＰＰＥ樹脂、脂肪族ポリアミド類、芳香族ポリアミド類、ポリイミド、ポリアミドイミド、ポリメタクリル酸類（ポリメタクリル酸メチル等のポリメタクリル酸エステル）、ポリアクリル酸類、ポリカーボネート、ポリフェニレンスルフィド、ポリサルホン、ポリエーテルサルホン、ポリエーテルニトリル、ポリエーテルケトン、ポリエーテルエーテルケトン、ポリケトン、液晶ポリマー、アイオノマーなどの熱可塑性樹脂、更にエポキシ類、アクリル類、ウレタン類、シリコーン類、フェノール類、イミド類、熱硬化型変性ＰＰＥ類、および熱硬化型ＰＰＥ類などの熱硬化性樹脂を挙げることが出来る。特に、エポキシ類、アクリル類、ウレタン類、シリコーン類、を使用することが好ましい。 Although the base resin used in the present invention is not particularly limited, specifically, polyethylene, polypropylene, ethylene-propylene copolymer, polymethylpentene, polyvinyl chloride, polyvinylidene chloride, polyvinyl acetate, ethylene-acetic acid Vinyl copolymer, polyvinyl alcohol, polyacetal, fluororesin (polyvinylidene fluoride, polytetrafluoroethylene, etc.), polyethylene terephthalate, polybutylene terephthalate, polyethylene 2,6 naphthalate, polystyrene, polyacrylonitrile, styrene-acrylonitrile copolymer, ABS Resins, polyphenylene ether (PPE) resins, modified PPE resins, aliphatic polyamides, aromatic polyamides, polyimides, polyamideimides, polymethacrylic acids (polymethyl methacrylate, etc. Polymethacrylates), polyacrylic acids, polycarbonate, polyphenylene sulfide, polysulfone, polyethersulfone, polyethernitrile, polyetherketone, polyetheretherketone, polyketone, liquid crystal polymer, ionomer, and other thermoplastic resins, and epoxies And thermosetting resins such as acrylics, urethanes, silicones, phenols, imides, thermosetting modified PPEs, and thermosetting PPEs. In particular, it is preferable to use epoxies, acrylics, urethanes, and silicones.
また、熱伝導性フィラーと基材樹脂よりなる複合材料は、必要に応じて硬化剤、カップリング剤などの添加剤を含んでもよい。 Moreover, the composite material which consists of a heat conductive filler and base-material resin may also contain additives, such as a hardening | curing agent and a coupling agent, as needed.
本発明のシート状成形体を構成する複合材料は、基材樹脂１００重量部に対して、熱伝導性フィラーを１００〜１０００重量部、好ましくは３００〜６００重量部の範囲内で含有するものが使用される。即ち、熱伝導性フィラーが１００重量部未満の場合は複合材料での熱伝導率が低くなり、放熱シートとして十分な特性を得ることができない。また、１０００重量部を超える場合には、混合時の粘度が著しく上昇し、作業性が極めて悪くなり、更には、混合不良が発生し、熱伝導性低下を招く等の問題が起こる。 The composite material constituting the sheet-like molded body of the present invention contains 100 to 1000 parts by weight, preferably 300 to 600 parts by weight of the heat conductive filler with respect to 100 parts by weight of the base resin. used. That is, when the heat conductive filler is less than 100 parts by weight, the thermal conductivity of the composite material is low, and sufficient characteristics as a heat dissipation sheet cannot be obtained. On the other hand, when it exceeds 1000 parts by weight, the viscosity at the time of mixing is remarkably increased, the workability is extremely deteriorated, and further, mixing failure occurs, causing problems such as a decrease in thermal conductivity.
本発明のシート状成形体の最大の特徴は、前記シート状成形体中の鱗片状窒化硼素粉末は、個数割合で７０％以上、好ましくは、７５％以上の粒子が、該シート状成形体のシート面に対して、その結晶面が３０〜９０度の角度を成した状態で存在することにある。 The greatest feature of the sheet-like molded article of the present invention is that the scaly boron nitride powder in the sheet-like molded article has a particle ratio of 70% or more, preferably 75% or more of the particles of the sheet-like molded article. The crystal plane is present at an angle of 30 to 90 degrees with respect to the sheet surface.
尚、上記鱗片状窒化硼素の結晶面がシート面に対して成す角度は、９０度の角度を最大値として個々の粒子のシート面に対する角度を測定したものである。 The angle formed by the scaly boron nitride crystal plane with respect to the sheet surface is a value obtained by measuring the angle of each particle with respect to the sheet surface with an angle of 90 degrees as a maximum value.
前記個数割合で、鱗片状窒化硼素の粒子がかかる配向を成して存在することにより、前記熱伝導性フィラーの添加量において、厚み方向において良好な熱伝導性を有するシート状成形体を構成することができる。 By the presence of the flaky boron nitride particles in such an orientation at the number ratio, a sheet-like molded body having good thermal conductivity in the thickness direction is constituted with the addition amount of the thermal conductive filler. be able to.
また、本発明のシート状成形体は、前記したように、熱伝導性フィラーの添加量を抑制することが可能であり、同等の熱伝導性を示す従来のシート状成形体に比べて、柔軟性があるという特徴を有する。 Further, as described above, the sheet-like molded body of the present invention can suppress the amount of the thermally conductive filler added, and is more flexible than the conventional sheet-like molded body exhibiting the same thermal conductivity. It has the characteristic of having sex.
本発明のシート状成形体の製造方法は、特に制限されるものではないが、好適な方法を例示すれば、前記の窒化アルミニウム粉末と鱗片状窒化硼素粉末とを前記所定の割合で混合して得られる熱伝導性フィラーを、基材樹脂と前記所定の割合で混合して複合材料を得、これを公知の方法により成形する方法が挙げられる。 The production method of the sheet-like molded body of the present invention is not particularly limited, but if a suitable method is exemplified, the aluminum nitride powder and the scaly boron nitride powder are mixed at the predetermined ratio. The heat conductive filler obtained is mixed with a base resin at the predetermined ratio to obtain a composite material, and a method of molding this by a known method can be mentioned.
上記各成分の混合には、ロール、ニーダ、バンバリーミキサー、自転・公転ミキサー等の通常の混練機が使用される。また、成形は、加圧成形、押出成形、カレンダー成形等の通常の成形法を用いて加工することができる。場合によっては、溶剤等を用いてキャスティングによる成形法を採用することも可能である。 For mixing the above components, a normal kneader such as a roll, a kneader, a Banbury mixer, and a rotation / revolution mixer is used. Moreover, shaping | molding can be processed using normal shaping | molding methods, such as pressure molding, extrusion molding, and calendar molding. In some cases, it is possible to adopt a molding method by casting using a solvent or the like.
上記成形方法のうち、得られるシート状成形体鱗片状窒化硼素粉末の結晶面が前記配向を示す個数割合を増加させるためには、窒化アルミニウム粉末と鱗片状窒化硼素粉末が均一に分散し、鱗片状窒化硼素粉末の結晶面が３０〜９０°の角度となるような成形方法が好適である。押出し成形やカレンダー成形などの成形方法だとその成形原理から粒子の配向性が出やすいため、本発明の構成を実現するためには比較的等方的な力を加えることにより成形する方法が好ましく、具体的には、加圧成形が好適である。 Among the above molding methods, in order to increase the number ratio in which the crystal plane of the obtained sheet-like compact scaly boron nitride powder exhibits the orientation, the aluminum nitride powder and the scaly boron nitride powder are uniformly dispersed, and the scaly A forming method is preferable in which the crystal plane of the boron nitride powder is at an angle of 30 to 90 °. In the case of a molding method such as extrusion molding or calender molding, the orientation of the particles tends to be easily obtained from the molding principle, so that a method of molding by applying a relatively isotropic force is preferable in order to realize the configuration of the present invention. Specifically, pressure molding is preferred.
以下、実施例によって本発明を具体的に説明するが、本発明はこれらの例に限定されるものではない。 EXAMPLES Hereinafter, although an Example demonstrates this invention concretely, this invention is not limited to these examples.
尚、表１中の各成分としては、下記のものを用いた。 In addition, as each component in Table 1, the following were used.
基材樹脂：エポキシ樹脂（三菱化学株式会社製ＪＥＲ８０７）１００重量部と硬化剤（三菱化学株式会社製ＪＥＲキュア１１３）３２重量部との混合物
平均粒径８０μmの窒化アルミニウム：古河電子株式会社製ＪＥＲ−８０
平均粒径２０μmの窒化アルミニウム：株式会社トクヤマ製
平均粒径５μmの窒化アルミニウム：株式会社トクヤマ製
平均長径１８μmの鱗片状窒化硼素粉末：電気化学株式会社ＢＮ−ＳＧＰ
平均長径２μmの鱗片状窒化硼素粉末：電気化学株式会社ＢＮ−ＳＰ３−７。
Base resin: Mixture of 100 parts by weight of epoxy resin (JER807 manufactured by Mitsubishi Chemical Corporation) and 32 parts by weight of curing agent (JER Cure 113 manufactured by Mitsubishi Chemical Corporation) Aluminum nitride having an average particle size of 80 μm: JER manufactured by Furukawa Electronics Co., Ltd. -80
Aluminum nitride having an average particle diameter of 20 μm: manufactured by Tokuyama Corporation Aluminum nitride having an average particle diameter of 5 μm: manufactured by Tokuyama Corporation Scale-like boron nitride powder having an average major diameter of 18 μm: BN-SGP, Electrochemical Co., Ltd.
Scale-like boron nitride powder having an average major axis of 2 μm: Electrochemical Co., Ltd. BN-SP3-7.
実施例１
本例は、基材樹脂としてエポキシ樹脂を用いて樹脂組成物の作製する例である。
具体的には基材樹脂１００重量部と、平均粒径８０μmの窒化アルミニウム３５１重量部と、平均長径１８μmの鱗片状窒化硼素粉末３９重量部とを自転・公転ミキサー（株式会社シンキー製ＡＲＥ−５００）にて混合して樹脂組成物を得た。
Example 1
This example is an example of producing a resin composition using an epoxy resin as a base resin.
Specifically, 100 parts by weight of the base resin, 351 parts by weight of aluminum nitride having an average particle diameter of 80 μm, and 39 parts by weight of scaly boron nitride powder having an average major diameter of 18 μm were mixed with a rotating / revolving mixer (ARE-500 manufactured by Shinky Corporation). ) To obtain a resin composition.
これを金型に注型し、熱プレスを使用し、温度:１２０℃、圧力：５ＭＰａ、保持時間：1時間の条件で硬化させ、直径１０ｍｍ、厚さ１ｍｍのシートを作製した。レーザーフラッシュ法にて熱伝導率を測定した。走査型電子顕微鏡（ＪＳＭ−５３００：ＪＥＯＬ社製）を用い、シート状成形体の断面撮影を行い、視野内の任意の２００個の鱗片状窒化硼素粉末粒子の配向度を測定した。測定した結果を表１に示した。 This was poured into a mold and cured using a hot press under conditions of temperature: 120 ° C., pressure: 5 MPa, holding time: 1 hour, and a sheet having a diameter of 10 mm and a thickness of 1 mm was produced. The thermal conductivity was measured by a laser flash method. Using a scanning electron microscope (JSM-5300: manufactured by JEOL), a cross-sectional image of the sheet-like molded body was taken, and the degree of orientation of any 200 scaly boron nitride powder particles in the field of view was measured. The measurement results are shown in Table 1.
実施例２〜５
表１に示す窒化アルミニウム、窒化硼素粉末の種類及び基材樹脂、窒化アルミニウム、窒化硼素粉末の量を使用し、それ以外は実施例１と同様にして、得られた樹脂組成物の熱伝導率及び窒化硼素粉末粒子の配向度を測定した結果を表１に示した。
Examples 2-5
The thermal conductivity of the obtained resin composition was the same as in Example 1 except that the types of aluminum nitride and boron nitride powder and the amounts of base resin, aluminum nitride, and boron nitride powder shown in Table 1 were used. The results of measuring the degree of orientation of the boron nitride powder particles are shown in Table 1.
比較例１〜３
表１に示す窒化アルミニウム、窒化硼素粉末の種類及び基材樹脂、窒化アルミニウム、窒化硼素粉末の量を使用し、それ以外は実施例１と同様にして、得られた樹脂組成物の熱伝導率及び窒化硼素粉末粒子の配向度を測定した結果を表１に示した。
Comparative Examples 1-3
The thermal conductivity of the obtained resin composition was the same as in Example 1 except that the types of aluminum nitride and boron nitride powder and the amounts of base resin, aluminum nitride, and boron nitride powder shown in Table 1 were used. The results of measuring the degree of orientation of the boron nitride powder particles are shown in Table 1.
比較例４〜５
表１に示す窒化硼素粉末の種類及び基材樹脂、窒化硼素粉末の量を使用し、それ以外は実施例１と同様にして、得られた樹脂組成物の熱伝導率及び窒化硼素粉末粒子の配向度を測定した結果を表１に示した。
Comparative Examples 4-5
The type of boron nitride powder and the amount of the base resin and boron nitride powder shown in Table 1 were used, and otherwise the same as in Example 1, the thermal conductivity of the obtained resin composition and the boron nitride powder particles The results of measuring the degree of orientation are shown in Table 1.
比較例６〜８
表１に示す窒化アルミニウムの種類及び基材樹脂、窒化アルミニウムの量を使用し、それ以外は実施例１と同様にして、得られた樹脂組成物の熱伝導率を測定した結果を表１に示した。
Comparative Examples 6-8
Table 1 shows the results of measuring the thermal conductivity of the obtained resin composition in the same manner as in Example 1 except that the type of aluminum nitride and the base resin and the amount of aluminum nitride shown in Table 1 were used. Indicated.
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