JP4481019B2 - Mixed powder and its use - Google Patents
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Description
本発明は、混合粉末及びそれを含有させた組成物に関する。詳しくは、例えばコンピューターなどの情報処理機器におけるＩＣ、ＬＳＩ、ＣＰＵ、ＭＰＵ及びプラズマディスプレイ等の画像表示用ＩＣの半導体素子により発生する熱を効率よく放出するのに有用な放熱部材等を製造するのに用いられる混合粉末と、それを樹脂又はゴムに含有させてなる組成物、特に放熱部材に関する。 The present invention relates to a mixed powder and a composition containing the same. Specifically, for example, a heat radiating member useful for efficiently releasing heat generated by a semiconductor element of an image display IC such as an IC, LSI, CPU, MPU and plasma display in information processing equipment such as a computer is manufactured. The present invention relates to a mixed powder used in the above and a composition containing the mixed powder in a resin or rubber, particularly a heat dissipation member.
近年、情報処理機器は、携帯用使用の薄型サイズのものが好まれるようになった。それに伴い、半導体素子も高密度化・小型化され、そこから発生する熱も増加の一途をたどり、それを効率よく除去することが重要な問題となっている。 In recent years, information processing equipment has come to be preferred for portable use. Along with this, the density and size of semiconductor elements have also been increased, and the heat generated therefrom has been increasing, and it has become an important problem to efficiently remove them.
従来、半導体素子より発生した熱の除去は、半導体素子を放熱シートを介して放熱フィンに取り付けることによって行われている。情報処理機器の小型化、薄型化により、放熱フィン等を取り付けるスペースがない場合には、情報処理機器のケース等に直接伝熱する方式が取られており、この場合には、半導体素子とケースの間に、そのスペースを埋める厚みを有した熱伝導性フィラー含有のシリコーン硬化物からなる柔らかな放熱スペーサーが用いられている。 Conventionally, the heat generated from the semiconductor element is removed by attaching the semiconductor element to the heat radiation fin via the heat radiation sheet. If there is no space to attach heat radiating fins due to downsizing and thinning of information processing equipment, a method of directly transferring heat to the case of information processing equipment is taken. In between, a soft heat dissipation spacer made of a cured silicone containing a heat conductive filler having a thickness to fill the space is used.
放熱スペーサー（以下、「スペーサー」ともいう。）の熱伝導性を高めるにあたり、窒化アルミニウム、窒化ケイ素等の熱伝導性フィラーを高充填する方法では（特許文献１）、それらの粉末に特有な粒子形状から大変なことであり、分級・粉砕等に多大な労力・時間が必要となるので、これらの粉末を単独で用いて熱伝導性を高めるには限界がきている。
本発明の目的は、更なる高熱伝導性を有するゴム又は樹脂の組成物、特に例えば放熱シート、スペーサー等の放熱部材を提供することであり、それに使用される粉末を提供することである。 An object of the present invention is to provide a rubber or resin composition having a further high thermal conductivity, in particular, a heat radiating member such as a heat radiating sheet or a spacer, and to provide a powder used therefor.
すなわち、本発明は、セラミックス粉末と金属粉末の混合粉末からなり、平均球形度が０．８５以上、平均粒子径が５０μｍ以下であり、しかも上記セラミックス粉末には頻度粒度分布において少なくとも２つの極大値があり、また上記金属粉末の頻度粒度分布における極大値が上記セラミックス粉末の極大値の間にあることを特徴とする混合粉末である。この場合において、頻度粒度分布において、セラミックス粉末の極大値が２０〜５０μｍの間と０．３〜０．７μｍの間に存在し、金属粉末の極大値が１〜１０μｍの間に存在する。また、２０〜５０μｍの粒子含有率が４０〜６０体積％、１〜１０μｍの粒子含有率が１０〜３０体積％、０．３〜０．７μｍの粒子含有率が１〜５体積％である。更には、セラミックス粉末がアルミナ粉末、金属粉末がアルミニウム粉末である。 That is, the present invention comprises a mixed powder of a ceramic powder and a metal powder, has an average sphericity of 0.85 or more and an average particle diameter of 50 μm or less, and the ceramic powder has at least two maximum values in the frequency particle size distribution. In addition, the mixed powder is characterized in that the maximum value in the frequency particle size distribution of the metal powder is between the maximum values of the ceramic powder. In this case, in the frequency particle size distribution, the maximum value of the ceramic powder exists between 20 to 50 μm and 0.3 to 0.7 μm, and the maximum value of the metal powder exists between 1 to 10 μm . Further, the particle content of 20 to 50 μm is 40 to 60% by volume, the particle content of 1 to 10 μm is 10 to 30% by volume, and the particle content of 0.3 to 0.7 μm is 1 to 5% by volume . Furthermore, the ceramic powder is an alumina powder, and the metal powder is an aluminum powder .
また、本発明は、上記いずれかの混合粉末を樹脂又はゴムに含有させてなることを特徴とする組成物である。この場合において、樹脂又はゴムがシリコーン硬化物であることを特徴とする放熱部材である。 In addition, the present invention is a composition comprising any one of the above mixed powders contained in a resin or rubber. In this case, the heat dissipation member is characterized in that the resin or rubber is a cured silicone.
本発明によれば、更なる高熱伝導性を有するゴム又は樹脂組成物、特に例えば放熱シート、スペーサー等の放熱部材が提供される。また、各種のゴム又は樹脂に絶縁性かつ熱伝導性を付与する粉末が提供される。 According to the present invention, a rubber or resin composition having further high thermal conductivity, in particular, a heat radiating member such as a heat radiating sheet or a spacer is provided. Moreover, the powder which provides insulation and heat conductivity to various rubber | gum or resin is provided.
本発明の混合粉末（以下、「充填剤」ともいう。）は、セラミックス粉末と金属粉末からなり、平均球形度が０．８５以上、平均粒子径が５０μｍ以下の混合粉末で構成されている。球形度が０．８５未満又は平均粒子径が５０μｍ超であると、粒子同士の接触が著しくなり、樹脂又はゴムの組成物（以下、単に「組成物」ともいう。）特にスペーサーの表面の凹凸が大きくなって界面熱抵抗が増大し更なる高熱伝導率化は達成しづらくなる。 The mixed powder of the present invention (hereinafter also referred to as “filler”) is composed of a ceramic powder and a metal powder, and is composed of a mixed powder having an average sphericity of 0.85 or more and an average particle diameter of 50 μm or less. When the sphericity is less than 0.85 or the average particle diameter is more than 50 μm, the contact between the particles becomes remarkable, and a resin or rubber composition (hereinafter also simply referred to as “composition”), particularly unevenness on the surface of the spacer. As the thermal resistance increases, the interfacial thermal resistance increases, making it difficult to achieve higher thermal conductivity.
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）に取り込むことによって測定することができる。すなわち、画像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）と同一の周囲長をもつ真円を想定すると、ＰＭ＝２πｒ、Ｂ＝πｒ２であるから、Ｂ＝π×（ＰＭ／２π）２となり、個々の粒子の球形度は、球形度＝Ａ／Ｂ＝Ａ×４π／（ＰＭ）２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する。 The average sphericity is measured by taking a particle image taken with a stereomicroscope, for example, “Model SMZ-10” (Nikon Corp.) or a scanning electron microscope, into an image analyzer (for example, Nihon Avionics Corp.). can do. That is, the projected area (A) and the perimeter (PM) of the particle are measured from the image. 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. Thus, 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 Can be calculated as sphericity = A / B = A × 4π / (PM) 2 . The sphericity of 200 arbitrary particles thus obtained is obtained, and the average value is defined as the average sphericity.
平均粒子径と頻度粒度分布は、市販の粒度測定装置、例えばＬ＆Ｎ社製粒度分布計「マイクロトラックＳＰ−Ａ」を用いて測定することができる。 The average particle size and frequency particle size distribution can be measured using a commercially available particle size measuring device, for example, a particle size distribution meter “Microtrac SP-A” manufactured by L & N.
つぎに、本発明の充填剤を構成するセラミックス粉末は、頻度粒度分布において少なくとも２つの極大値を有し、また金属粉末はその頻度粒度分布における極大値が上記セラミックス粉末の極大値の間に存在するように構成されている。このようにすることによって、組成物の表面に粒子の大きなセラミックス粉末が多く存在させることができるので組成物が導電性となるのを緩和することができ、しかもセラミックス粉末同士、金属粉末同士、セラミックス粉末と金属粉末の粒子間の接触が大きくなって熱伝導性が向上する。また、高価格である金属粉末の使用量を軽減できるので低コスト化にも寄与する。 Next, the ceramic powder constituting the filler of the present invention has at least two maximum values in the frequency particle size distribution, and the metal powder has a maximum value in the frequency particle size distribution between the maximum values of the ceramic powder. Is configured to do. By doing so, a large amount of large-sized ceramic powder can be present on the surface of the composition, so that the composition becomes less conductive, and ceramic powders, metal powders, ceramics The contact between the particles of the powder and the metal powder is increased and the thermal conductivity is improved. In addition, the amount of expensive metal powder used can be reduced, which contributes to cost reduction.
本発明においては、セラミックス粉末の頻度粒度分布の極大値が２０〜５０μｍ（以下、「セラミックス粉末ａ」という。）と、０．３〜０．７μｍ（以下、「セラミックス粉末ｂ」という。）であり、金属粉末の頻度粒度分布の極大値がこれらのセラミックス粉末の頻度粒度分布の極大値の間の１〜１０μｍ（以下、「金属粉末ａ」という。）にあることが好ましい。中でも、セラミックス粉末ａの含有率が４０〜６０体積％であり、セラミックス粉末ｂの含有率が１〜５体積％であり、金属粉末ａの含有率が１０〜３０体積％であることが好ましい。特に好ましくは、セラミックス粉末ａの含有率が４５〜５５体積％であり、セラミックス粉末ｂが０．４〜０．６μｍの間にあってその含有率が２〜４体積％であり、金属粉末ａの含有率が１５〜２５体積％である。 In the present invention, the maximum values of the frequency particle size distribution of the ceramic powder are 20 to 50 μm (hereinafter referred to as “ceramic powder a”) and 0.3 to 0.7 μm (hereinafter referred to as “ceramic powder b”). The maximum value of the frequency particle size distribution of the metal powder is preferably 1 to 10 μm (hereinafter referred to as “metal powder a”) between the maximum values of the frequency particle size distribution of these ceramic powders. Especially, it is preferable that the content rate of the ceramic powder a is 40-60 volume%, the content rate of the ceramic powder b is 1-5 volume%, and the content rate of the metal powder a is 10-30 volume%. Particularly preferably, the content of the ceramic powder a is 45 to 55% by volume, the content of the ceramic powder b is between 0.4 to 0.6 μm and the content is 2 to 4% by volume, and the content of the metal powder a The rate is 15-25% by volume.
本発明ではセラミックス粉末ｂの役割が特に重要であり、その極大値が０．３μｍ未満にあるか又はその含有率が５体積％超であると、組成物の流動性が低下するか又は組成物内でそれが偏析する。一方、セラミックス粉末ｂの極大値が０．７μｍ超にあるか又はその含有率が１体積％未満であると、微粉が少なくなって粒子間の接触が少なくなる。 In the present invention, the role of the ceramic powder b is particularly important, and if the maximum value is less than 0.3 μm or the content is more than 5% by volume, the fluidity of the composition decreases or the composition Within it segregates. On the other hand, when the maximum value of the ceramic powder b is more than 0.7 μm or the content thereof is less than 1% by volume, the fine powder is reduced and the contact between the particles is reduced.
本発明の充填剤は、セラミックス粉末ａ、セラミックス粉末ｂ及び金属粉末ａを所定量混合することによって製造することができる。これらの粉末による合計が１００体積％に満たないときには、球形度が０．８５以上、平均粒子径が５０μｍ以下のセラミックス粉末を混合する。これによって、更なる導電性を緩和させ、熱伝導率を向上させることができる。 The filler of the present invention can be produced by mixing predetermined amounts of ceramic powder a, ceramic powder b, and metal powder a. When the total of these powders is less than 100% by volume, ceramic powder having a sphericity of 0.85 or more and an average particle diameter of 50 μm or less is mixed. Thereby, further electrical conductivity can be relaxed and thermal conductivity can be improved.
本発明に使用されるセラミックス粉末としては、例えばアルミナ、マグネシア、カルシア、カルシウムアルミネート、スピネル等の酸化物粉末、窒化硼素、窒化珪素、窒化アルミニウム、炭化珪素、炭化ホウ素、炭素等の非酸化物粉末等を例示することができるが、好ましくは球状アルミナ粉末である。また、金属粉末としては、アルミニウム、銅、銀、金、モリブデン、タングステン等が使用されるが、好ましくはアルミニウム粉末である。 Examples of the ceramic powder used in the present invention include oxide powders such as alumina, magnesia, calcia, calcium aluminate, and spinel, and non-oxides such as boron nitride, silicon nitride, aluminum nitride, silicon carbide, boron carbide, and carbon. Examples of the powder include a spherical alumina powder. As the metal powder, aluminum, copper, silver, gold, molybdenum, tungsten, or the like is used, and aluminum powder is preferable.
本発明の組成物に用いられる樹脂又はゴムとしては、例えばシリコーン樹脂、ポリエチレン、ポリプロピレン、エチレン・酢酸ビニル共重合体、硬化性アクリル樹脂、硬化性エポキシ樹脂、シリコーンゴム等が例示され、特に耐熱性が優れることから、シリコーン硬化物が好ましい。組成物中の充填剤の含有率は、用途により例えば３０〜９５体積％の割合とすることができる。 Examples of the resin or rubber used in the composition of the present invention include silicone resin, polyethylene, polypropylene, ethylene / vinyl acetate copolymer, curable acrylic resin, curable epoxy resin, and silicone rubber. Is preferable, a silicone cured product is preferable. The content rate of the filler in a composition can be made into the ratio of 30-95 volume% by the use, for example.
シリコーン硬化物としては、一般的な電子材料用途に使用されているシリコーン、例えば付加反応により加硫する液状シリコーン樹脂、過酸化物を加硫に用いる熱加硫型ミラブルタイプのシリコーン樹脂等を不都合なく用いることができる。組成物の用途がスペーサー等の放熱部材であるときは、半導体素子の発熱面と放熱フィン等の放熱面との密着性が要求されるため、シリコーンの中でも柔軟性を有する付加反応型液状シリコーンの使用が望ましい。付加反応型液状シリコーンの具体例としては、例えば一分子中にビニル基とＨ−Ｓｉ基の両方を有する一液性のシリコーン、又は末端あるいは側鎖にビニル基を有するオルガノポリシロキサンと末端あるいは側鎖に２個以上のＨ−Ｓｉ基を有するオルガノポリシロキサンとの二液性のシリコーン等を挙げることができる。このような付加反応型液状シリコーンの市販品としては、例えば東芝シリコーン社製、商品名「ＸＥ８５３０」などがある。シリコーン硬化物の柔軟性は、付加反応によって形成される架橋密度によって調整することができる。 Examples of cured silicone products include silicones that are used in general electronic material applications, such as liquid silicone resins that are vulcanized by addition reactions, and heat-curing millable type silicone resins that use peroxides for vulcanization. Can be used. When the application of the composition is a heat radiating member such as a spacer, the adhesion between the heat generating surface of the semiconductor element and the heat radiating surface such as a heat radiating fin is required. Use is desirable. Specific examples of the addition reaction type liquid silicone include, for example, a one-part silicone having both a vinyl group and an H-Si group in one molecule, or an organopolysiloxane having a vinyl group at the terminal or side chain and the terminal or side. A two-part silicone with an organopolysiloxane having two or more H-Si groups in the chain can be exemplified. Examples of commercially available products of such addition reaction type liquid silicone include a product name “XE8530” manufactured by Toshiba Silicone Co., Ltd. The flexibility of the silicone cured product can be adjusted by the crosslink density formed by the addition reaction.
本発明の組成物は、原料の混合・成形・硬化工程を経て製造される。混合には、ロールミル、ニーダー、バンバリーミキサー等の混合機が用いられる。成形方法はドクターブレード法が好ましいが、ゴム又は樹脂の粘度によって押し出し法・プレス法・カレンダーロール法等を用いることができる。硬化温度は、５０〜２００℃が望ましい。硬化は、一般的な熱風乾燥機、遠赤外乾燥機、マイクロ波乾燥機等を用いて行われる。 The composition of the present invention is produced through a raw material mixing / molding / curing process. For mixing, a mixer such as a roll mill, a kneader, or a Banbury mixer is used. A doctor blade method is preferable as the molding method, but an extrusion method, a press method, a calender roll method, or the like can be used depending on the viscosity of rubber or resin. The curing temperature is preferably 50 to 200 ° C. Curing is performed using a general hot air dryer, far-infrared dryer, microwave dryer or the like.
本発明の放熱部材は、シリコーン硬化物に充填剤を例えば３０〜９５体積％存在させたものであり、その厚みは０．１〜６ｍｍ、特に０．２〜３ｍｍが一般的である。その平面形状は、半導体素子と密着できる形状ないし、半導体素子を埋没できる形状であれば、特に制限されるものではなく、例えば三角形、四角形、六角形などの多角形、円形、楕円軽等の任意の形状を用いることができ、更には半導体素子が密着ないしは埋没しやすいように凹凸を付けることもできる。 The heat radiating member of the present invention has a silicone cured product in which a filler is present in an amount of, for example, 30 to 95% by volume, and the thickness thereof is generally 0.1 to 6 mm, particularly 0.2 to 3 mm. The planar shape is not particularly limited as long as it is a shape that can be in close contact with a semiconductor element or a shape that can be embedded in a semiconductor element. In addition, the semiconductor element can be provided with unevenness so that the semiconductor element is easily adhered or buried.
実施例１ 比較例１〜３
シリコーンＡ液（ビニル基を有するオルガノポリシロキサン）と、シリコーンＢ液（Ｈ−Ｓｉ基を有するオルガノポリシロキサン）の二液の付加重合型液状シリコーン（東芝シリコーン社製、商品名「ＸＥ８５３０」）と、表１に示されるセラミックス粉末と金属粉末を表２で示すような割合で配合した。得られた樹脂組成物を、室温において真空脱泡した後、ドクターブレード法にて厚さ１ｍｍのシートに成形した後、１２０℃の乾燥機に６時間静置して加硫・硬化させ、スペーサーを作製し、以下に従い、（１）熱伝導率と（２）体積抵抗率を測定した。また、平均球形度は上記方法によって画像解析して求め、セラミックス粉末と金属粉末の平均粒子径、頻度粒度分布における極大値をもつ粒子径は、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。それらの結果を表２に示す。
Example 1 Comparative Examples 1-3
Two-part addition polymerization type liquid silicone (trade name “XE8530” manufactured by Toshiba Silicone Co., Ltd.) of silicone A liquid (organopolysiloxane having vinyl group) and silicone B liquid (organopolysiloxane having H—Si group) The ceramic powder and metal powder shown in Table 1 were blended in the proportions shown in Table 2. The obtained resin composition was vacuum degassed at room temperature, then formed into a sheet having a thickness of 1 mm by the doctor blade method, and then left to stand in a dryer at 120 ° C. for 6 hours to be vulcanized and cured. In accordance with the following, (1) thermal conductivity and (2) volume resistivity were measured. The average sphericity is obtained by image analysis according to the above method. The average particle diameter of ceramic powder and metal powder, and the particle diameter having the maximum value in the frequency particle size distribution are the particle size distribution meter “Microtrac SP-A” manufactured by L & N. It measured using. The results are shown in Table 2.
（１）熱伝導率：スペーサーをＴＯ−３型銅製ヒーターケースと銅板との間に挟み、スペーサー厚みの１０％を圧縮した後、銅製ヒーターケースに電力５Ｗをかけて４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、熱伝導率（Ｗ／ｍ・ｋ）＝｛電力（Ｗ）×厚み（ｍ）｝／｛温度差（ｋ）×測定面積（ｍ２）｝、にて熱伝導率を算出した。
（２）体積抵抗率：ヒューレットパッカード社製ハイ・レジスタンス・メータ「４３３９Ａ」を用いて印加電圧５００Ｖで測定した。
(1) Thermal conductivity: A spacer is sandwiched between a TO-3 type copper heater case and a copper plate, and after compressing 10% of the spacer thickness, the copper heater case is kept at power for 5 minutes and held for 4 minutes. The temperature difference between the case and the copper plate is measured, and thermal conductivity (W / m · k) = {power (W) × thickness (m)} / {temperature difference (k) × measurement area (m 2 )} The thermal conductivity was calculated.
(2) Volume resistivity: Measured at an applied voltage of 500 V using a high resistance meter “4339A” manufactured by Hewlett-Packard Company.
本発明の充填剤は各種の樹脂又はゴムに絶縁性かつ熱伝導性を付与するために使用される。本発明の組成物は各種伝熱部材の製造用材料として使用される。本発明の放熱部材は例えば放熱シート、スペーサー等として使用される。 The filler of the present invention is used for imparting insulating properties and thermal conductivity to various resins or rubbers. The composition of the present invention is used as a material for producing various heat transfer members. The heat radiating member of the present invention is used as, for example, a heat radiating sheet or a spacer.
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| WO2008053536A1 (en) * | 2006-10-31 | 2008-05-08 | Denki Kagaku Kogyo Kabushiki Kaisha | Alumina powder, process for producing the same, and use thereof |
| JP2010155870A (en) * | 2007-04-20 | 2010-07-15 | Denki Kagaku Kogyo Kk | Thermally conductive compound and method for producing the same |
| WO2011067328A1 (en) * | 2009-12-04 | 2011-06-09 | Abb Research Ltd | A high voltage surge arrester |
| TWI462831B (en) * | 2010-10-06 | 2014-12-01 | Hitachi Chemical Co Ltd | Multilayered resin sheet and method for producing the same, resin sheet laminate and method for producing the same, harded resin sheet, multilayered resin sheet with metal foil, and semiconductor device |
| JP5431595B2 (en) * | 2011-03-28 | 2014-03-05 | 日立化成株式会社 | Resin composition, resin sheet, resin sheet cured product, resin sheet laminate, resin sheet laminate cured product and method for manufacturing the same, semiconductor device, and LED device |
| TW201515819A (en) * | 2013-10-17 | 2015-05-01 | Ho-Chang Lee | Method for manufacturing steering wheel cover |
| WO2018131486A1 (en) * | 2017-01-13 | 2018-07-19 | デンカ株式会社 | Thermally conductive resin composition, heat dissipation sheet, heat dissipation member and method for producing same |
| US20210238368A1 (en) | 2018-06-05 | 2021-08-05 | Teijin Limited | Composite particles and production method therefor |
| CN113993939B (en) | 2019-06-24 | 2024-07-16 | 信越化学工业株式会社 | High thermal conductivity silicone composition and cured product thereof |
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| JPS56834A (en) * | 1979-06-15 | 1981-01-07 | Showa Denko Kk | Additive for high-molecular material |
| JP2003309235A (en) * | 2002-04-18 | 2003-10-31 | Denki Kagaku Kogyo Kk | Heat radiating member and power module |
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| JPS56834A (en) * | 1979-06-15 | 1981-01-07 | Showa Denko Kk | Additive for high-molecular material |
| JP2003309235A (en) * | 2002-04-18 | 2003-10-31 | Denki Kagaku Kogyo Kk | Heat radiating member and power module |
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