JPWO2009017170A1 - Alumina powder, method for producing the same, and composition using the same - Google Patents

Alumina powder, method for producing the same, and composition using the same Download PDF

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JPWO2009017170A1
JPWO2009017170A1 JP2009525438A JP2009525438A JPWO2009017170A1 JP WO2009017170 A1 JPWO2009017170 A1 JP WO2009017170A1 JP 2009525438 A JP2009525438 A JP 2009525438A JP 2009525438 A JP2009525438 A JP 2009525438A JP WO2009017170 A1 JPWO2009017170 A1 JP WO2009017170A1
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JP5336374B2 (en
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田中　孝明
孝明 田中
國友　修
修 國友
貴久 水本
貴久 水本
寿 江崎
寿 江崎
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Denka Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/021—After-treatment of oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/90—Other morphology not specified above
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity

Abstract

耐湿信頼性を更に向上させたアルミナ粉末と、その製造方法と、それを用いた組成物、特に半導体封止材を提供する。１５０℃で１００時間の超純水抽出試験におけるＮａ＋の量が２０ｐｐｍ以下のアルミナ粉末、あるいは１５０℃で１００時間の超純水抽出試験におけるＬｉ＋、Ｎａ＋、Ｋ＋の総量が２０ｐｐｍ以下であり、平均粒子径が４５μｍ未満の粒子の平均円形度が０．９５以上であり、平均粒子径が１００μｍ以下のアルミナ粉末。また、電融アルミナ粉砕物を火炎中で熱処理することを特徴とするアルミナ粉末の製造方法。さらに、上記のようなアルミナ粉末を含有する樹脂又はゴムの組成物、特に半導体封止材。Provided are an alumina powder having further improved moisture resistance reliability, a production method thereof, and a composition using the same, particularly a semiconductor encapsulant. Alumina powder having an Na + amount of 20 ppm or less in an ultrapure water extraction test at 150 ° C. for 100 hours, or a total amount of Li +, Na +, K + in an ultrapure water extraction test at 150 ° C. for 100 hours in an average particle of 20 ppm or less An alumina powder having an average circularity of particles having a diameter of less than 45 μm of 0.95 or more and an average particle diameter of 100 μm or less. Moreover, the manufacturing method of the alumina powder characterized by heat-processing an electromelted alumina ground material in a flame. Furthermore, a resin or rubber composition containing the above alumina powder, particularly a semiconductor sealing material.

Description

本発明は耐湿信頼性の高いアルミナ粉末、その製造方法及び該アルミナ粉末を用いた組成物の用途に関する。   The present invention relates to an alumina powder having high moisture resistance reliability, a method for producing the same, and a use of a composition using the alumina powder.

近年、ＩＣ等の発熱性電子部品の高機能化と高速化の進展に伴い、それが搭載された電子機器の発熱量が増大しており、半導体封止材に対しても高い放熱特性が求められている。半導体封止材の放熱特性を高めるには、熱伝導性の高いアルミナ粉末をゴム又は樹脂に含有させればよいが、通常のバイヤー法アルミナ粉末にはＮａ＋が多量に存在するので半導体封止材の耐湿信頼性を著しく損なわせた。In recent years, with the advancement of high-function and high-speed heat-generating electronic components such as ICs, the amount of heat generated by electronic devices on which they are mounted is increasing, and high heat dissipation characteristics are also required for semiconductor encapsulants. It has been. To improve the heat dissipation characteristics of the semiconductor sealing material, a high alumina powder thermal conductivity may be contained in the rubber or resin, but the semiconductor sealing since the usual Bayer process alumina powder of Na + is present in a large amount The moisture resistance reliability of the material was significantly impaired.

これを解決するため、アルミナ粉末をイオン交換樹脂の存在下で水洗し、イオン性不純物を除去することが提案された（特許文献１参照）。その実施例には、９５℃で１００時間の超純水抽出試験によるＮａ＋の量が２ｐｐｍになったと記載されている。しかし、車輌などの半導体封止材には一段と高い信頼性が要求されており、１５０℃で１００時間のさらに厳しい超純水抽出試験において、Ｎａ＋の溶出量の少ないアルミナ粉末が求められている。特許文献１に記載の例では、このような過酷な抽出試験条件におけるＮａ＋の溶出量は３０ｐｐｍ程度となる。
特開２００５−２８１０６３号公報 In order to solve this, it has been proposed to wash the alumina powder in the presence of an ion exchange resin to remove ionic impurities (see Patent Document 1). The example states that the amount of Na + in the ultrapure water extraction test at 95 ° C. for 100 hours was 2 ppm. However, semiconductor sealing materials for vehicles and the like are required to have higher reliability, and alumina powder with a low Na + elution amount is required in a more severe ultrapure water extraction test at 150 ° C. for 100 hours. . In the example described in Patent Document 1, the elution amount of Na + under such severe extraction test conditions is about 30 ppm.
JP 2005-281063 A

本発明の目的は、耐湿信頼性を更に改善したアルミナ粉末と、その製造方法及びそれを用いた組成物、特に半導体封止材を提供することである。   An object of the present invention is to provide an alumina powder further improved in moisture resistance reliability, a production method thereof, and a composition using the same, particularly a semiconductor encapsulant.

本発明者等は上記課題を解決すべく検討したところ、電融アルミナ粉砕物を火炎処理し、好ましくは火炎処理物を水洗することによって、耐湿信頼性を更に改善したアルミナ粉末の提供が達成できることを見出した。
すなわち、本発明は以下の要旨を有するものである。The present inventors have studied to solve the above-mentioned problems, and it is possible to achieve provision of alumina powder having further improved moisture resistance reliability by subjecting the pulverized electrofused alumina to flame treatment, and preferably washing the flame-treated product with water. I found.
That is, the present invention has the following gist.

本発明は、以下の方法で測定されたＮａ＋の量が２０ｐｐｍ以下のアルミナ粉末である。
［Ｎａ＋の量の測定方法］
アルミナ粉末と超純水を質量比１：２の割合でステンレス製の耐圧密閉容器に封入し、温度１５０℃の雰囲気中で１００時間静置してから、２０℃で３０分間放冷した後、セルロースフィルターを用い濾過し、その濾液中のＬｉ＋、Ｎａ＋、Ｋ＋の量を原子吸光分光光度計にて測定したときのＮａ＋の量（Ｎａ＋の溶出量）である。なお、超純水にはＡＤＶＡＮＴＥＣ社製の商品名「ＲＦＤ２５０ＮＢ」を用い、原子吸光分光光度計には島津製作所社製の商品名「ＡＡ−６８００」を用いた。The present invention is an alumina powder in which the amount of Na + measured by the following method is 20 ppm or less.
[Method for measuring the amount of Na + ]
Alumina powder and ultrapure water were sealed in a pressure-resistant airtight container made of stainless steel at a mass ratio of 1: 2, left standing in an atmosphere at a temperature of 150 ° C. for 100 hours, and then allowed to cool at 20 ° C. for 30 minutes. The amount of Li + , Na + , and K + in the filtrate obtained by filtration using a cellulose filter is the amount of Na + (Na + elution amount) when measured with an atomic absorption spectrophotometer. In addition, the brand name “RFD250NB” manufactured by ADVANTEC was used for the ultrapure water, and the trade name “AA-6800” manufactured by Shimadzu Corporation was used for the atomic absorption spectrophotometer.

また、本発明は、上記方法で測定されたＬｉ＋、Ｎａ＋、Ｋ＋の総量が２０ｐｐｍ以下であり、平均粒子径が４５μｍ未満の粒子の平均円形度０．９５以上、特に０．９７以上であり、平均粒子径が１００μｍ以下、特に１０〜９５μｍであるアルミナ粉末である。In the present invention, the total amount of Li + , Na + , K + measured by the above method is 20 ppm or less, and the average circularity of particles having an average particle diameter of less than 45 μm is 0.95 or more, particularly 0.97 or more. And an alumina powder having an average particle size of 100 μm or less, particularly 10 to 95 μm.

また、本発明のアルミナ粉末においては、化学分析によるアルカリ金属の含有量が、Ｒ２Ｏ（ＲはＬｉ、Ｎａ、Ｋを表す。）換算で１質量％以下（０質量％を含む）であることが好ましい。また、平均粒子径が４５〜２００μｍの粒子の平均円形度が０．９５以上であることが好ましい。In the alumina powder of the present invention, the content of alkali metal by chemical analysis is 1% by mass or less (including 0% by mass) in terms of R 2 O (R represents Li, Na, K). It is preferable. Moreover, it is preferable that the average circularity of the particle | grains whose average particle diameter is 45-200 micrometers is 0.95 or more.

また、本発明は、電融アルミナ粉砕物を火炎中で熱処理することを特徴とするアルミナ粉末の製造方法である。本発明においては、火炎処理物を水洗することが好ましい。
また、化学分析によるアルカリ金属の含有量がＲ２Ｏ（ＲはＬｉ、Ｎａ、Ｋを表す。）換算で３質量％以下（０質量％を含む）の電融アルミナ粉砕物を火炎処理することが好ましい。Moreover, this invention is a manufacturing method of the alumina powder characterized by heat-processing an electromelted alumina ground material in a flame. In the present invention, it is preferable to wash the flame-treated product with water.
Also, flame-treating the pulverized fused alumina having a content of alkali metal by chemical analysis of 3% by mass or less (including 0% by mass) in terms of R 2 O (R represents Li, Na, K). Is preferred.

また、本発明は、本発明のアルミナ粉末をゴム又は樹脂に含有させてなる組成物、特に本発明のアルミナ粉末をエポキシ樹脂に含有させてなる半導体封止材である。   Moreover, this invention is a semiconductor sealing material made to contain the alumina powder of this invention in rubber | gum or resin, especially the epoxy resin containing the alumina powder of this invention.

本発明のアルミナ粉末の製造方法によれば、耐湿信頼性の高いアルミナ粉末が得られ、例えばアルミニウム配線を有する半導体素子を、１４０℃、３気圧の水蒸気雰囲気に曝しても３５０時間以上断線しない組成物、特に半導体封止材の製造が可能となる。   According to the method for producing alumina powder of the present invention, a highly moisture-resistant and reliable alumina powder is obtained. For example, a composition in which a semiconductor element having an aluminum wiring is not disconnected for 350 hours or more even when exposed to a steam atmosphere at 140 ° C. and 3 atmospheres. Manufacturing of a product, particularly a semiconductor encapsulant, is possible.

アルミナ粉末のＮａ＋の量（溶出量）が２０ｐｐｍを超えると著しく耐湿信頼性が低下する。Ｎａ＋の量は少ないほど好適であり、特に１０ｐｐｍ以下が好ましい。このようなアルミナ粉末は、電融アルミナ粉砕物を火炎処理することによって製造できる。より高い耐湿信頼性を実現するためには、Ｌｉ＋、Ｎａ＋、Ｋ＋の総量が２０ｐｐｍ以下であることが好ましい。When the amount of Na + (elution amount) in the alumina powder exceeds 20 ppm, the moisture resistance reliability is remarkably lowered. The smaller the amount of Na +, the more suitable, and 10 ppm or less is particularly preferable. Such an alumina powder can be produced by subjecting a pulverized fused alumina to a flame. In order to realize higher moisture resistance reliability, the total amount of Li + , Na + , and K + is preferably 20 ppm or less.

アルミナ粉末中のＬｉ＋、Ｎａ＋、Ｋ＋の含有量（溶出量）は、電融アルミナ粉砕物中のそれらの含有率によって増減できる。電融アルミナ粉砕物中のＮａ＋の含有量は、例えば原料となるバイヤー法アルミナ粉末を硫酸水溶液（例えば濃度１５質量％）に浸漬（例えば２４時間）させることによって低減できる。また、バイヤー法アルミナ粉末をアーク炉で溶融する際にＬｉ２Ｏ、Ｎａ２Ｏ、Ｋ２Ｏを添加することによってＬｉ＋、Ｎａ＋、Ｋ＋の含有量を増加させることができる。The content (elution amount) of Li + , Na + , and K + in the alumina powder can be increased or decreased depending on their content in the pulverized fused alumina. The content of Na + in the pulverized fused alumina can be reduced, for example, by immersing (for example, 24 hours) a Bayer method alumina powder as a raw material in a sulfuric acid aqueous solution (for example, concentration of 15% by mass). In addition, the content of Li + , Na + , and K + can be increased by adding Li 2 O, Na 2 O, and K 2 O when the Bayer method alumina powder is melted in an arc furnace.

アルミナ粉末の平均粒子径は、用途に応じて種々選択される。後記する本発明の製造方法によれば、平均粒子径が１００μｍ以下、特に１０〜９５μｍのアルミナ粉末を容易に製造することができる。平均粒子径は、電融アルミナ粉砕物の平均粒子径によって増減できる。平均粒子径が１００μｍ以下であると、球状化させやすいという点で好ましい。平均粒子径が１０μｍ以下では、火炎投入時に粒子を均一に分散させることが難しく、粒子を高度に球状化させることが難しい。粒子を高度に球状化させるという点からは、平均粒子径が１０μｍ以上であることが好ましい。   The average particle diameter of the alumina powder is variously selected depending on the application. According to the production method of the present invention described later, an alumina powder having an average particle size of 100 μm or less, particularly 10 to 95 μm, can be easily produced. The average particle diameter can be increased or decreased depending on the average particle diameter of the electrofused alumina pulverized product. An average particle diameter of 100 μm or less is preferable in that it is easy to make spherical. When the average particle size is 10 μm or less, it is difficult to uniformly disperse the particles when the flame is introduced, and it is difficult to make the particles highly spherical. From the viewpoint of highly spheroidizing the particles, the average particle diameter is preferably 10 μm or more.

平均粒子径は、レーザー回折式粒度分布測定機シーラスグラニュロメーター(ＣＩＬＡＳ社製、「モデル９２０」)を用いて測定した。平均粒子径２５〜４５μｍの粒子についてはサンプル２ｇ、４５〜１２０μｍの粒子についてはサンプル４ｇを秤量し、直接シーラスグラニュロメーターのサンプル導入部に投入する。シーラスグラニュロメーター粒度分布測定の設定は、屈折率に水（１．３３０）とアルミナ（１．７６８）を用い、ポンプ回転数は６０ｒｐｍで行った。
アルミナ粉末中の化学分析によるアルカリ金属の含有量を増やすとアルミナの融点を下げることができる。アルカリ金属の含有量が、Ｒ２Ｏ（ＲはＬｉ、Ｎａ、Ｋを表す。）換算で１質量％を超えると粒子同士の合着が進み円形度が低下する。より高い円形度を達成するためには、Ｒ２Ｏ換算で好ましくは０．８〜１質量％である。The average particle size was measured using a laser diffraction particle size distribution measuring machine Cirrus granometer (CILAS, “Model 920”). For particles having an average particle diameter of 25 to 45 μm, 2 g of sample is weighed, and for particles of 45 to 120 μm, 4 g of sample is weighed and directly put into the sample introduction part of the Cirrus granulometer. The Cirrus granulometer particle size distribution measurement was performed using water (1.330) and alumina (1.768) for the refractive index, and the pump rotation speed at 60 rpm.
Increasing the content of alkali metal by chemical analysis in the alumina powder can lower the melting point of alumina. When the content of the alkali metal exceeds 1% by mass in terms of R 2 O (R represents Li, Na, K), coalescence of the particles proceeds and the circularity decreases. In order to achieve higher circularity, it is preferably 0.8 to 1% by mass in terms of R 2 O.

樹脂又はゴムにアルミナ粉末を高充填するには、平均粒子径が４５μｍ未満のアルミナ粉末の平均円形度は０．９５以上が好ましく、特に０．９７以上が好ましい。なかでも、平均粒子径が４５〜２００μｍのアルミナ粉末の平均円形度が０．９５以上とすることによって、組成物の流動性を更に高めることができる。
アルミナ粉末の平均円形度は、火炎形成に用いる燃料ガス（例えばＬＰＧ）量、電融アルミナ粉砕物中のＬｉ＋、Ｎａ＋、Ｋ＋の含有率によって増減させることができる。平均粒子径が４５〜２００μｍの粒子の平均円形度を高めるには、電融アルミナ粉砕物の化学分析によるアルカリ金属の含有量が、Ｒ２Ｏ換算で３質量％以下（０質量％を含む）に調整しておくと容易となる。電融アルミナ粉砕物の化学分析によるアルカリ金属の含有量は、Ｒ２Ｏ換算で、３質量％以下が好ましい。In order to highly fill the alumina powder in the resin or rubber, the average circularity of the alumina powder having an average particle diameter of less than 45 μm is preferably 0.95 or more, particularly preferably 0.97 or more. Especially, the fluidity | liquidity of a composition can further be improved by making the average circularity of the alumina powder whose average particle diameter is 45-200 micrometers into 0.95 or more.
The average circularity of the alumina powder can be increased or decreased depending on the amount of fuel gas (for example, LPG) used for flame formation and the content of Li + , Na + , and K + in the electrofused alumina pulverized product. In order to increase the average circularity of particles having an average particle diameter of 45 to 200 μm, the content of alkali metal by chemical analysis of the fused alumina pulverized product is 3% by mass or less (including 0% by mass) in terms of R 2 O. It will be easier if you adjust it. The content of alkali metal by chemical analysis of the electrofused alumina pulverized product is preferably 3% by mass or less in terms of R 2 O.

化学分析によるアルカリ金属のＲ２Ｏ（ＲはＬｉ、Ｎａ、Ｋを表す。）換算量は、試料に対して４．５モル／リットルの硫酸１５ｍｌを加え、内壁が四フッ化エチレンでコーティングされたステンレス製耐圧密閉容器に封入し、温度２３０℃に保たれた電気乾燥機（例えばヤマト科学社製、商品名「ＤＳ−４４」）内で１７時間保持後、水で１００ｍｌに定容し、サンプルを調製した後、その濾液を原子吸光分光光度計（例えば島津製作所社製、商品名「ＡＡ−６８００」）で分析することによって測定する。この化学分析法は、電融アルミナ粉砕物中に含有されるアルカリ金属の含有量に相当するＲ２Ｏ（ＲはＬｉ、Ｎａ、Ｋを表す。）換算量の測定にも適用される。The amount of alkali metal converted to R 2 O (R represents Li, Na, K) by chemical analysis is 15 mol of 4.5 mol / liter sulfuric acid, and the inner wall is coated with tetrafluoroethylene. Sealed in a pressure-resistant airtight container made of stainless steel, kept in an electric dryer maintained at a temperature of 230 ° C. (for example, product name “DS-44” manufactured by Yamato Kagaku Co., Ltd.) for 17 hours, and then fixed to 100 ml with water. After preparing a sample, the filtrate is measured by analyzing with an atomic absorption spectrophotometer (for example, trade name “AA-6800” manufactured by Shimadzu Corporation). This chemical analysis method is also applied to the measurement of R 2 O (R represents Li, Na, K) equivalent amount corresponding to the content of alkali metal contained in the pulverized fused alumina.

平均円形度は、Ｓｙｓｍｅｘ社製のフロー式粒子像解析装置「ＦＰＩＡ−３０００」を用いて測定する。すなわち、２００ｍｌビーカーにアルミナ粉末４０ｇを計量し、イオン交換水を１００ｍｌ入れて撹拌した後、超音波洗浄器（例えばアズワン社製、商品名「超音波洗浄器強力型ＶＳ−１５０」）で３分間分散し、スラリーとする。次いで、受け皿を取り付けたＪＩＳ４５μｍ篩に前記のビーカー内のスラリーを入れた後、３００ｍｌのイオン交換水を篩の上から加え、その後、粒子径に応じて以下のように測定する。なお、平均円形度は、フロー式粒子像解析装置「ＦＰＩＡ−３０００」が、一個の粒子投影像の周囲長と粒子投影像の面積に相当する円の周囲長を解析し、下式により円形度を求め、３６０００個当たりの平均値を自動算出する。
円形度＝（粒子投影像の周囲長）／（粒子投影像の面積に相当する円の周囲長）
以下に、各平均粒子径における平均円形度の測定方法を示す。The average circularity is measured using a flow type particle image analyzer “FPIA-3000” manufactured by Sysmex. That is, 40 g of alumina powder is weighed in a 200 ml beaker, 100 ml of ion-exchanged water is added and stirred, and then for 3 minutes with an ultrasonic cleaner (for example, product name “Ultrasonic cleaner VS-150” manufactured by ASONE). Disperse into a slurry. Next, after the slurry in the beaker is put into a JIS 45 μm sieve equipped with a saucer, 300 ml of ion-exchanged water is added from above the sieve, and then measured according to the particle diameter as follows. The average degree of circularity is determined by the flow type particle image analyzer “FPIA-3000” analyzing the circumference of one particle projection image and the circumference of a circle corresponding to the area of the particle projection image. And an average value per 36000 pieces is automatically calculated.
Circularity = (perimeter of particle projection image) / (perimeter of circle corresponding to area of particle projection image)
Below, the measuring method of the average circularity in each average particle diameter is shown.

［平均粒子径が４５〜２００μｍの粒子の平均円形度］
５ｍｌの容器に篩上の粒子を０．１５〜０．２０ｇ計量し、プロピレングリコール２５質量％水溶液を５ｍｌ加えた後、超音波洗浄器で１０秒間分散させる。これをフロー式粒子像解析装置「ＦＰＩＡ−３０００」に全量入れ、（トータルカウント数３６０００個、繰返し測定回数１回）方式で測定し、粒子範囲を４５〜２００μｍ（円相当径／個数基準）として解析する。[Average circularity of particles having an average particle diameter of 45 to 200 μm]
0.15 to 0.20 g of particles on the sieve are weighed in a 5 ml container, 5 ml of a 25% by mass aqueous solution of propylene glycol is added, and then dispersed in an ultrasonic cleaner for 10 seconds. All of this is put into a flow type particle image analyzer “FPIA-3000” and measured by a (total count of 36000, repeated measurement once) method, and the particle range is set to 45 to 200 μm (equivalent circle diameter / number basis). To analyze.

［平均粒子径が４５μｍ未満の粒子の平均円形度］
前記の受け皿の中で沈降したスラリーを撹拌棒で撹拌してから、その０．５ｍｌを５ｍｌの容器に採取し、プロピレングリコール２５質量％水溶液を５ｍｌ加えた後、超音波洗浄器で１０秒間分散させる。これをフロー式粒子像解析装置「ＦＰＩＡ−３０００」に全量入れ、ＨＰＦモード／定量カウント（トータルカウント数３６０００個、繰返し測定回数１回）方式で測定し、粒子範囲を１．５〜４５μｍ（円相当径／個数基準）として解析する。[Average circularity of particles having an average particle diameter of less than 45 μm]
After stirring the slurry that has settled in the saucer with a stir bar, 0.5 ml of the slurry is collected in a 5 ml container, 5 ml of a 25% by weight aqueous solution of propylene glycol is added, and then dispersed for 10 seconds with an ultrasonic cleaner. Let All of this was put into a flow type particle image analyzer “FPIA-3000” and measured by the HPF mode / quantitative count (total count of 36,000, repeated measurement once) method, and the particle range was 1.5 to 45 μm (circle) (Equivalent diameter / number basis).

本発明のアルミナ粉末の製造方法は、原料粉末として、バイヤー法アルミナ粉末の代わりに電融アルミナ粉砕物を用いたこと以外は、常法（例えば特開平１１−５７４５１号公報）の火炎処理法と同じである。
概説すれば、電融アルミナ粉砕物を火炎に噴射し、得られた球状化物を排ガスと共にブロワーによってサイクロン、バグフィルター等の捕集装置に搬送し分級・捕集する。サイクロン品とバグフィルター品等を適宜混合して所望粒度のアルミナ粉末にする。火炎の形成は、水素、天然ガス、アセチレンガス、プロパンガス、ブタン等の燃料ガスと、空気、酸素等の助燃ガスとを、炉体に設定された燃焼バーナーから噴射して行う。The alumina powder production method of the present invention is a conventional flame treatment method (for example, JP-A No. 11-57451), except that as a raw material powder, pulverized electrofused alumina is used instead of the Bayer method alumina powder. The same.
Briefly, the fused alumina pulverized product is injected into a flame, and the resulting spheroidized product is transported to a collection device such as a cyclone or bag filter together with exhaust gas, and classified and collected. A cyclone product and a bag filter product are appropriately mixed to obtain alumina powder having a desired particle size. The formation of the flame is performed by injecting a fuel gas such as hydrogen, natural gas, acetylene gas, propane gas, or butane and an auxiliary combustion gas such as air or oxygen from a combustion burner set in the furnace body.

電融アルミナ破砕物とはバイヤー法仮焼アルミナの溶融固化物の粉砕物のことである。その平均粒子径は、所望するアルミナ粉末の平均粒子径に応じ、例えば平均粒子径が２００μｍ以下の範囲内で適宜選択される。   The electrofused alumina crushed material is a pulverized material of the melted and solidified product of the Bayer method calcined alumina. The average particle diameter is appropriately selected within the range where the average particle diameter is 200 μm or less, for example, according to the desired average particle diameter of the alumina powder.

アルミナ粉末の平均粒子径が４５〜２００μｍ粒子の平均円形度を０．９５以上にするには、電融アルミナ破砕物中の化学分析によるアルカリ金属の含有量をＲ２Ｏ換算（ＲはＬｉ、Ｎａ、Ｋを表す。）で３質量％以下（０質量％を含む）に調整しておくことが好ましい。Ｒ２Ｏ換算の含有量が３質量％を超えると、アルミナの融点が下がるので平均粒子径が４５μｍ以上の粒子の合着が生じ平均円形度０．９５以上の実現が困難となり、しかも、上記のような過酷条件（１５０℃で１００時間の超純水抽出試験）でのＬｉ＋、Ｎａ＋、Ｋ＋の総量が２０ｐｐｍを超える。アルカリ金属の電融アルミナ破砕物中の含有量の下限は、Ｒ２Ｏ換算で５００ｐｐｍであることが好ましい。In order to make the average circularity of particles having an average particle diameter of 45 to 200 μm of alumina powder 0.95 or more, the content of alkali metal by chemical analysis in the fused alumina crushed material is converted into R 2 O (R is Li, It is preferable to adjust to 3% by mass or less (including 0% by mass) with Na and K. When the content in terms of R 2 O exceeds 3% by mass, the melting point of alumina is lowered, so that particles having an average particle diameter of 45 μm or more are coalesced, making it difficult to realize an average circularity of 0.95 or more. The total amount of Li + , Na + , and K + under such severe conditions (extra pure water extraction test at 150 ° C. for 100 hours) exceeds 20 ppm. The lower limit of the content of the alkali metal crushed fused alumina is preferably 500 ppm in terms of R 2 O.

本発明の製造方法においては、電融アルミナ破砕物中のＲ２Ｏ量によってアルミナ粉末中のそれらの量を増減させることができる。
本発明においては、電融アルミナ破砕物の火炎処理物を水洗してＬｉ＋、Ｎａ＋、Ｋ＋を、特にＮａ＋を除去（低減も含む。以下同じ。）すれば更に本発明のアルミナ粉末の製造が容易となる。水洗には、原子吸光分光光度計において、Ｌｉ＋成分、Ｎａ＋成分、及びＫ＋成分が未検出であるｐＨが３〜７の超純水を用いることが好ましい。このような超純水は、純水製造装置（例えばＡＤＶＡＮＴＥＣ社製、商品名「ＲＦＤ２５０ＮＢ」）で製造されたイオン交換水に、例えば塩酸、酢酸、硫酸等の酸を添加し、ｐＨを調整することによって製造することができる。ｐＨが７を超えると、アルミナ粉末からのＬｉ＋、Ｎａ＋、Ｋ＋の除去効率が低下する。ｐＨが３未満であっても除去効率は大きく変わらないが、ｐＨ調整に用いた酸成分が残留する恐れがある。水洗に用いる超純水の好ましいｐＨの範囲は、３〜６である。In the production method of the present invention, the amount of the alumina powder can be increased or decreased depending on the amount of R 2 O in the electromelted alumina crushed material.
In the present invention, the flame-treated product of the fused alumina crushed material is washed with water to remove Li + , Na + , K + , particularly Na + (including reduction, the same shall apply hereinafter), and further the alumina powder of the present invention. Is easy to manufacture. For the washing with water, it is preferable to use ultrapure water having a pH of 3 to 7 in which Li + component, Na + component, and K + component are not detected in an atomic absorption spectrophotometer. Such ultrapure water adjusts pH by adding an acid such as hydrochloric acid, acetic acid or sulfuric acid to ion-exchanged water produced by a pure water production apparatus (eg, product name “RFD250NB” manufactured by ADVANTEC). Can be manufactured. When pH exceeds 7, the removal efficiency of Li <+> , Na <+> , K < + > from an alumina powder will fall. Even if the pH is less than 3, the removal efficiency does not change greatly, but the acid component used for pH adjustment may remain. The preferable pH range of ultrapure water used for water washing is 3-6.

水洗は、電融アルミナ破砕物の火炎処理物の水スラリーを調製し撹拌して行う。撹拌装置としては、ローター・ステーターシステム（槽の中心に固定棒が設置され、その周りを撹拌用ローターが回転する仕組みの撹拌装置）のような高い剪断能力を有するものが好ましい。その一例を示せば、アシザワ・ファインテック社製の商品名「スターディスパーサーＲＳＶ１７５」である。撹拌中に超音波を付与することは更に好ましい。   The washing with water is performed by preparing a water slurry of the flame-treated product of the fused alumina crushed material and stirring it. As the agitation device, a device having a high shearing ability such as a rotor / stator system (an agitation device in which a fixed rod is installed at the center of the tank and the agitation rotor rotates around) is preferable. One example is the product name “Star Disperser RSV175” manufactured by Ashizawa Finetech. It is more preferable to apply ultrasonic waves during stirring.

スラリーのアルミナ粉末濃度は攪拌装置の摩耗と生産性の観点から４５〜６０質量％であることが好ましく、４５〜５０質量％がより好ましい。またより多くのアルカリ金属イオンを水洗水の中に抽出させ、除去するという観点からスラリー温度は８０〜９５℃であることが好ましい。撹拌時間は１〜３時間程度である。その後、スラリーはフィルタープレスで脱水処理され、乾燥されてアルミナ粉末となる。乾燥時間は温度１２０〜１８０℃で１２〜６０時間程度である。乾燥機は通常の棚段乾燥機で十分である。   The alumina powder concentration of the slurry is preferably 45 to 60% by mass, more preferably 45 to 50% by mass, from the viewpoint of wear of the stirrer and productivity. Moreover, it is preferable that slurry temperature is 80-95 degreeC from a viewpoint of extracting more alkali metal ions in the washing water, and removing. The stirring time is about 1 to 3 hours. Thereafter, the slurry is dehydrated with a filter press and dried to form alumina powder. The drying time is about 12 to 60 hours at a temperature of 120 to 180 ° C. A normal shelf dryer is sufficient for the dryer.

本発明の組成物は、本発明のアルミナ粉末をゴム又は樹脂に含有させたものである。本発明の組成物は、各材料の所定量をブレンダーやヘンシェルミキサー等によりブレンドした後、加熱ロール、ニーダー、一軸又は二軸押し出し機等によって混練し冷却した後、粉砕することによって製造することができる。アルミナ粉末の含有率は用途によって異なり、その一例をあげれば４０〜９０体積％である。
本発明のアルミナ粉末をエポキシ樹脂に含有させたものは半導体封止材として好適である。半導体封止材の本発明のアルミナ粉末の含有率は７０〜９０体積％であることが好ましく、７５〜８５体積％がより好ましい。半導体の封止方法としては、トランスファーモールド、マルチプランジャーなどを採用することができる。The composition of the present invention is one in which the alumina powder of the present invention is contained in rubber or resin. The composition of the present invention can be produced by blending a predetermined amount of each material with a blender, Henschel mixer, etc., kneading with a heating roll, kneader, uniaxial or biaxial extruder, etc., cooling, and then pulverizing. it can. The content of the alumina powder varies depending on the application, and an example thereof is 40 to 90% by volume.
What contained the alumina powder of this invention in the epoxy resin is suitable as a semiconductor sealing material. It is preferable that the content rate of the alumina powder of this invention of a semiconductor sealing material is 70-90 volume%, and 75-85 volume% is more preferable. As a semiconductor sealing method, a transfer mold, a multi-plunger, or the like can be employed.

本発明の組成物に用いるゴムを例示すれば、シリコーンゴム、ウレタンゴム、アクリルゴム、エチレンプロピレンゴム、ウレタンゴム、エチレン酢酸ビニル共重合体などである。なかでも、シリコーンゴム、ウレタンゴム、アクリルゴムが好ましく用いられる。
また、本発明の組成物に用いる樹脂を例示すれば、エポキシ樹脂、フェノール樹脂、メラミン樹脂、ユリア樹脂、不飽和ポリエステル、フッ素樹脂、ポリイミド、ポリアミドイミド、ポリエーテルイミド等のポリアミド、ポリブチレンテレフタレート、ポリエチレンテレフタレート等のポリエステル、ポリフェニレンスルフィド、全芳香族ポリエステル、ポリスルホン、液晶ポリマー、ポリエーテルスルホン、ポリカーボネート、マレイミド変性樹脂、ＡＢＳ樹脂、ＡＡＳ（アクリロニトリル−アクリルゴム・スチレン）樹脂、ＡＥＳ（アクリロニトリル・エチレン・プロピレン・ジエンゴム−スチレン）樹脂などである。なかでも、エポキシ樹脂、フッ素樹脂、ポリフェニレンスルフィドが好ましく用いられる。Examples of the rubber used in the composition of the present invention include silicone rubber, urethane rubber, acrylic rubber, ethylene propylene rubber, urethane rubber, and ethylene vinyl acetate copolymer. Of these, silicone rubber, urethane rubber, and acrylic rubber are preferably used.
Examples of resins used in the composition of the present invention include epoxy resins, phenol resins, melamine resins, urea resins, unsaturated polyesters, fluororesins, polyimides, polyamideimides, polyetherimides, and other polyamides, polybutylene terephthalates, Polyester such as polyethylene terephthalate, polyphenylene sulfide, wholly aromatic polyester, polysulfone, liquid crystal polymer, polyethersulfone, polycarbonate, maleimide modified resin, ABS resin, AAS (acrylonitrile-acrylic rubber / styrene) resin, AES (acrylonitrile / ethylene / propylene) -Diene rubber-styrene) resin. Of these, epoxy resins, fluororesins, and polyphenylene sulfide are preferably used.

次に、実施例及び比較例により本発明をより具体的に説明するが、本発明は、以下の実施例に限定して解釈されるものではない。   EXAMPLES Next, although an Example and a comparative example demonstrate this invention more concretely, this invention is limited to a following example and is not interpreted.

実施例１〜２６、比較例１〜３
［電融アルミナ粉砕物の製造］
バイヤー法仮焼アルミナ粉末「Ｓ」（Ｎａ＋をＮａ２Ｏ換算で０．５質量％含有）をアーク炉で溶融・冷却・粉砕して、電融アルミナ粉砕物「Ｃ」、及び「Ｄ」を製造した。電融アルミナ粉砕物「Ｃ」、及び「Ｄ」の製造分けは粉砕時間を調整して行った。
バイヤー法仮焼アルミナ粉末「Ｓ」の５００ｋｇを硫酸水溶液（濃度１５質量％）、０．２５ｍ３に２４時間浸漬した後、水洗・乾燥してからアーク炉で溶融・冷却・粉砕して、電融アルミナ粉砕物「Ａ」、「Ｂ」及び「Ｑ」を製造した。電融アルミナ粉砕物「Ａ」、「Ｂ」及び「Ｑ」の製造分けは粉砕時間を調整して行った。Examples 1-26, Comparative Examples 1-3
[Production of pulverized electrofused alumina]
Bayer process calcined alumina powder “S” (containing 0.5% by mass of Na + in terms of Na 2 O) is melted, cooled and pulverized in an arc furnace, and electrofused alumina pulverized products “C” and “D” Manufactured. The production of the fused alumina pulverized products “C” and “D” was performed by adjusting the pulverization time.
After immersing 500 kg of Bayer method calcined alumina powder “S” in sulfuric acid aqueous solution (concentration: 15% by mass), 0.25 m 3 for 24 hours, washing, drying, melting, cooling and grinding in an arc furnace, Fused alumina pulverized products “A”, “B” and “Q” were produced. The production of the fused alumina pulverized products “A”, “B”, and “Q” was performed by adjusting the pulverization time.

また、バイヤー法仮焼アルミナ粉末「Ｓ」に、Ｎａ２Ｏ、Ｋ２Ｏ又はＬｉ２Ｏを添加したこと以外は、電融アルミナ粉砕物「Ａ」の製造と同様にして電融アルミナ粉砕物を製造した。電融アルミナ粉砕物「Ｅ」、「Ｆ」、「Ｋ」、「Ｌ」及び「Ｒ」はＮａ２Ｏを添加して、電融アルミナ粉砕物「Ｇ」、「Ｈ」、「Ｏ」及び「Ｐ」はＫ２Ｏを添加して、また電融アルミナ粉砕物「Ｉ」、「Ｊ」、「Ｍ」及び「Ｎ」はＬｉ２Ｏを添加して製造した。これらの製造分けは粉砕時間を調整して行った。Further, the fused alumina pulverized product is the same as the production of the fused alumina pulverized product “A” except that Na 2 O, K 2 O, or Li 2 O is added to the Bayer method calcined alumina powder “S”. Manufactured. Electrofused alumina pulverized products “E”, “F”, “K”, “L”, and “R” were added with Na 2 O, and the fused alumina pulverized products “G”, “H”, “O”, and “P” was prepared by adding K 2 O, and electrofused alumina pulverized products “I”, “J”, “M” and “N” were prepared by adding Li 2 O. These productions were performed by adjusting the pulverization time.

電融アルミナ粉砕物の平均粒子径及び化学分析によるアルカリ金属の含有量であるＲ２Ｏ（ＲはＬｉ、Ｎａ、Ｋを表す）換算量は、上記に従い測定した。それらの結果を表１に示す。Fused R 2 O mean a content of alkali metal by particle size and chemical analysis of alumina pulverized product (R represents Li, Na, and K) in terms of weight was measured in accordance with the above. The results are shown in Table 1.

［電融アルミナ粉砕物の火炎処理（アルミナ粉末の製造）］
電融アルミナ粉砕物（比較例１は、バイヤー法仮焼アルミナ粉末を使用した。）の火炎処理は特開２００１−１９９７１９号公報の図1に示す製造装置を用いて行った。燃料ガス（ＬＰＧ）と助燃ガス（Ｏ２ガス）の噴射量を表２のようにして火炎を形成した。電融アルミナ粉砕物又はバイヤー法仮焼アルミナ粉末は、その３０ｋｇ／Ｈｒを酸素ガス２０Ｎｍ３／Ｈｒに同伴させノズルから火炎中に噴射し、得られたアルミナ粉末をバグフィルターから回収した。[Flame treatment of pulverized electrofused alumina (production of alumina powder)]
The flame treatment of the electromelted alumina pulverized product (Comparative Example 1 used a Bayer method calcined alumina powder) was performed using the manufacturing apparatus shown in FIG. 1 of JP-A-2001-199719. A flame was formed with the injection amounts of fuel gas (LPG) and auxiliary combustion gas (O 2 gas) as shown in Table 2. The pulverized electrofused alumina or the Bayer method calcined alumina powder was jetted into a flame from a nozzle with 30 kg / Hr accompanied by oxygen gas 20 Nm 3 / Hr, and the obtained alumina powder was recovered from a bag filter.

［アルミナ粉末の水洗処理］
実施例２３及び２４を除き、実施例１〜２２、２５、２６、及び比較例１〜３ではアルミナ粉末を以下のようにして水洗処理した。すなわち、アルミナ粉末と、原子吸光分光光度計測定においてＬｉ＋成分、Ｎａ＋成分、及びＫ＋成分が未検出であるＰＨが７のイオン交換水とを混合して、アルミナ粉末濃度が４０質量％の水スラリーを調製し、撹拌混合装置（アシザワ・ファインテック社製、商品名「スターディスパーサーＲＳＶ１７５」）を用いて１時間撹拌した後、フィルタープレスで脱水処理をした。ケーキの含水率は全て２０質量％以下であった。このケーキを棚段乾燥機にて１５０℃で４８時間乾燥してアルミナ粉末を製造した。なお、水洗処理は、実施例１９〜２２及び比較例２、３では水スラリーの温度を５℃にして行い、それ以外では８５℃にして行った。[Washing treatment of alumina powder]
Except for Examples 23 and 24, in Examples 1-22, 25, 26, and Comparative Examples 1-3, the alumina powder was washed with water as follows. That is, alumina powder is mixed with ion-exchanged water having a pH of 7 in which Li + component, Na + component, and K + component are not detected in the atomic absorption spectrophotometer measurement, and the alumina powder concentration is 40% by mass. Was stirred for 1 hour using a stirring and mixing device (manufactured by Ashizawa Finetech, trade name “Star Disperser RSV175”), and then dehydrated with a filter press. All the moisture content of the cake was 20 mass% or less. The cake was dried at 150 ° C. for 48 hours with a shelf dryer to produce alumina powder. In addition, the water-washing process was performed by making the temperature of water slurry into 5 degreeC in Examples 19-22 and Comparative Examples 2 and 3, and making it 85 degreeC in other than that.

アルミナ粉末の平均円形度、１５０℃で１００時間の超純水抽出試験におけるＬｉ＋、Ｎａ＋、Ｋ＋の量、及び化学分析によるアルカリ金属の含有量であるＲ２Ｏ（ＲはＬｉ、Ｎａ、Ｋ）換算量は、上記方法に従って測定した。それらの結果を表２及び表３に示す。The average circularity of alumina powder, the amount of Li + , Na + , K + in an ultrapure water extraction test at 150 ° C. for 100 hours, and the content of alkali metal by chemical analysis, R 2 O (R is Li, Na , K) The converted amount was measured according to the above method. The results are shown in Tables 2 and 3.

つぎに、表４に示される配合物３０体積部とアルミナ粉末７０体積部を混合してエポキシ樹脂組成物を調製し、その耐湿信頼性と流動性を以下に従い評価した。それらの結果を表２及び表３に示す。   Next, 30 parts by volume of the formulation shown in Table 4 and 70 parts by volume of alumina powder were mixed to prepare an epoxy resin composition, and its moisture resistance reliability and fluidity were evaluated as follows. The results are shown in Tables 2 and 3.

［耐湿信頼性］
アルミニウム配線を有する１６ピンモニターＩＣをトランスファー成形し、硬化後２６０℃のハンダ浴に１０秒間浸漬した後、１４０℃、３気圧の水蒸気雰囲気中で３０Ｖ印加して、アルミニウム配線のオープン不良（断線）、又は成形物を超音波探査映像装置でモニタリングし、成形物にクラックが発生した個数の合計が試料個数（２０個）の５０％（１０個）になるまでの時間を測定し、表２及び表３に示した。時間が長いほど、耐湿信頼性が高いことを示す。[Moisture resistance reliability]
A 16-pin monitor IC with aluminum wiring is transfer molded, and after curing, immersed in a solder bath at 260 ° C. for 10 seconds, and then applied with 30 V in a steam atmosphere at 140 ° C. and 3 atmospheres, an aluminum wiring open failure (disconnection) Alternatively, the molded product is monitored with an ultrasonic imaging apparatus, and the time until the total number of cracks in the molded product reaches 50% (10) of the number of samples (20) is measured. It is shown in Table 3. The longer the time, the higher the moisture resistance reliability.

［流動性］
スパイラルフロー金型を用い、ＥＭＭＩ−６６（Ｅｐｏｘｙ Ｍｏｌｄｉｎｇ Ｍａｔｅｒｉａｌ Ｉｎｓｔｉｔｕｔｅ；Ｓｏｃｉｅｔｙ ｏｆ Ｐｌａｓｔｉｃ Ｉｎｄｕｓｔｒｙ）に準拠したスパイラルフロー測定用金型を取り付けたトランスファー成形機を用いて、二軸押出混練機で加熱混練して調製した半導体封止材料のスパイラルフロー値を測定した。トランスファー成形条件は、金型温度１７５℃、成形圧力７．４ＭＰａ、保圧時間９０秒とした。
スパイラルフロー値が、長ければ長いほど高い流動性を持つことを示す。[Liquidity]
Using a spiral flow mold, heat-kneading with a twin-screw extrusion kneader using a transfer molding machine equipped with a spiral flow measurement mold conforming to EMMI-66 (Epoxy Molding Material Institute; Society of Plastic Industry). The spiral flow value of the prepared semiconductor sealing material was measured. The transfer molding conditions were a mold temperature of 175 ° C., a molding pressure of 7.4 MPa, and a pressure holding time of 90 seconds.
The longer the spiral flow value, the higher the fluidity.

Figure 2009017170
Figure 2009017170

Figure 2009017170
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Figure 2009017170
Figure 2009017170

Figure 2009017170
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表１〜３から明らかなように、本発明のアルミナ粉末は比較例に比べて、１５０℃で１００時間の一段と厳しい超純水抽出試験において、Ｎａ＋の量の少ないものであり、それを用いて製造された組成物（半導体封止材）の耐湿信頼性が著しく向上した。As is apparent from Tables 1 to 3, the alumina powder of the present invention has a lower amount of Na + in the ultrapure water extraction test at 150 ° C. for 100 hours than in the comparative example. The moisture resistance reliability of the composition (semiconductor encapsulating material) produced in this manner was significantly improved.

本発明のアルミナ粉末は、ゴム又は樹脂組成物の充填材として使用され、該アルミナ粉末を含む組成物は、自動車、携帯電子機器、産業用機器、家庭用電化製品等のモールディングコンパウンドや放熱シート等に用いられる。特に、本発明の半導体封止材は、グラフィックチップ等の放熱特性が重要とされる用途で使用されるなど、産業上有用である。

なお、２００７年７月３１日に出願された日本特許出願２００７−１９９４０５号の明細書、特許請求の範囲、及び要約書の全内容をここに引用し、本発明の明細書の開示として、取り入れるものである。The alumina powder of the present invention is used as a filler of a rubber or resin composition, and the composition containing the alumina powder is used for molding compounds, heat dissipation sheets, etc. for automobiles, portable electronic devices, industrial devices, household appliances, etc. Used for. In particular, the semiconductor encapsulant of the present invention is industrially useful, such as being used in applications where heat dissipation characteristics such as graphic chips are important.

The entire contents of the specification, claims, and abstract of Japanese Patent Application No. 2007-199405 filed on July 31, 2007 are incorporated herein as the disclosure of the specification of the present invention. Is.

Claims (10)

以下の方法で測定されたＮａ＋の量が２０ｐｐｍ以下であることを特徴とするアルミナ粉末。
［Ｎａ＋の量の測定方法］
アルミナ粉末と超純水を質量比１：２の割合でステンレス製の耐圧密閉容器に封入し、温度１５０℃の雰囲気中で１００時間静置してから、２０℃で３０分間放冷した後、セルロースフィルターを用いて濾過し、その濾液中のＬｉ＋、Ｎａ＋、Ｋ＋の量を原子吸光分光光度計にて測定したときのＮａ＋の量。An alumina powder characterized in that the amount of Na + measured by the following method is 20 ppm or less.
[Method for measuring the amount of Na + ]
Alumina powder and ultrapure water were sealed in a pressure-resistant airtight container made of stainless steel at a mass ratio of 1: 2, left standing in an atmosphere at a temperature of 150 ° C. for 100 hours, and then allowed to cool at 20 ° C. for 30 minutes. The amount of Na + when filtered using a cellulose filter and the amount of Li + , Na + , K + in the filtrate was measured with an atomic absorption spectrophotometer. 請求項１に記載の方法で測定されたＬｉ＋、Ｎａ＋、Ｋ＋の総量が２０ｐｐｍ以下であり、平均粒子径が４５μｍ未満の粒子の平均円形度が０．９５以上、平均粒子径が１００μｍ以下であることを特徴とするアルミナ粉末。The total amount of Li + , Na + and K + measured by the method according to claim 1 is 20 ppm or less, the average circularity of particles having an average particle diameter of less than 45 μm is 0.95 or more, and the average particle diameter is 100 μm. An alumina powder characterized by: 化学分析によるアルカリ金属の含有量が、Ｒ２Ｏ（ＲはＬｉ、Ｎａ、Ｋを表す。）換算で１質量％（０質量％を含む）以下である請求項１又は２に記載のアルミナ粉末。The alumina powder according to claim 1 or 2, wherein the content of the alkali metal by chemical analysis is 1% by mass (including 0% by mass) or less in terms of R 2 O (R represents Li, Na, K). . 平均粒子径が４５〜２００μｍの粒子の平均円形度が０．９５以上である請求項１〜３のいずれかに記載のアルミナ粉末。   The alumina powder according to any one of claims 1 to 3, wherein particles having an average particle diameter of 45 to 200 µm have an average circularity of 0.95 or more. 電融アルミナ粉砕物を火炎中で熱処理することを特徴とするアルミナ粉末の製造方法。   A method for producing an alumina powder, comprising heat treating a pulverized electrofused alumina in a flame. 電融アルミナ粉砕物を火炎中で熱処理した後、水洗する請求項５に記載の製造方法。   The manufacturing method according to claim 5, wherein the pulverized fused alumina is heat-treated in a flame and then washed with water. 化学分析によるアルカリ金属の含有量が、Ｒ２Ｏ（ＲはＬｉ、Ｎａ、Ｋを表す。）換算で３質量％以下（０質量％を含む）の電融アルミナ粉砕物を用いる請求項５又は６に記載の製造方法。The fused alumina pulverized product having an alkali metal content by chemical analysis of 3% by mass or less (including 0% by mass) in terms of R 2 O (R represents Li, Na, K) is used. 6. The production method according to 6. 請求項１〜４のいずれかに記載のアルミナ粉末をゴム又は樹脂に含有させてなることを特徴とする組成物。   A composition comprising the alumina powder according to any one of claims 1 to 4 contained in a rubber or a resin. 前記樹脂がエポキシ樹脂である請求項８に記載の組成物。   The composition according to claim 8, wherein the resin is an epoxy resin. 請求項９に記載の組成物を用いてなることを特徴とする半導体封止材。   A semiconductor encapsulant comprising the composition according to claim 9.
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