JP2002348116A - Alumina particle and method for producing the same - Google Patents
Alumina particle and method for producing the sameInfo
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- JP2002348116A JP2002348116A JP2001163188A JP2001163188A JP2002348116A JP 2002348116 A JP2002348116 A JP 2002348116A JP 2001163188 A JP2001163188 A JP 2001163188A JP 2001163188 A JP2001163188 A JP 2001163188A JP 2002348116 A JP2002348116 A JP 2002348116A
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- Prior art keywords
- alumina
- alumina particles
- round
- particles according
- producing
- Prior art date
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、丸み状のアルミナ
粒子に関し、特に電子部品の封止材料、充填剤、仕上げ
ラッピング材、又は耐火物、ガラス、セラミックスおよ
びそれらを含む複合材における骨材等に有用な、低摩耗
性かつフロー特性に優れたアルミナ粒子を工業的に安価
で製造する方法およびその製法により得られた丸み状ア
ルミナ粒子及びそれを含有する高熱伝導性ゴム・プラス
チック組成物に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a round alumina particle, and more particularly to a sealing material for electronic parts, a filler, a finishing wrapping material, or a refractory, an aggregate in glass, ceramics, and a composite material containing them. For industrially inexpensive production of alumina particles having low abrasion properties and excellent flow characteristics useful for rubber, round alumina particles obtained by the production method, and high thermal conductive rubber / plastic compositions containing the same It is.
【０００２】[0002]
【従来の技術】近年、電子部品の高集積化、高密度化に
伴って、チップ当りの電力消費量も増大の一途にあり、
発生した熱を効率良く放熱し、電子部品素子の温度上昇
を少なくすることが重要な開発課題になっている。そし
て、半導体の絶縁封止材料や、部品を実装する基板材
料、放熱スペーサーなどの充填剤として、熱伝導性の優
れたアルミナ、特にコランダム（α−アルミナ）が注目
され、さまざまな分野で使用されている。2. Description of the Related Art In recent years, the power consumption per chip has been steadily increasing with the increasing integration and density of electronic components.
It is an important development task to efficiently radiate the generated heat and reduce the temperature rise of the electronic component element. Alumina with excellent thermal conductivity, especially corundum (α-alumina), has been attracting attention as a filler for semiconductor insulating sealing materials, substrate materials for mounting components, and heat radiation spacers, and is used in various fields. ing.
【０００３】このようなコランダム粒子としては、電融
アルミナ、焼結アルミナなどの粉砕品に、水酸化アルミ
ニウムを単独で、または結晶促進剤として公知の他の薬
剤を併用して添加し、焼成することでカッティングエッ
ジを有しない、形状が球状化したコランダム粒子が提案
されている（特開平５−２９４６１３号公報）。As such corundum particles, aluminum hydroxide is added alone or in combination with another known agent as a crystallization accelerator to a pulverized product such as fused alumina or sintered alumina, followed by firing. Accordingly, corundum particles having no cutting edge and having a spherical shape have been proposed (JP-A-5-294613).
【０００４】また、バイヤー法のアルミナを高温プラズ
マや酸水素炎中に噴射し、溶融させながら急冷すること
により丸み化する、いわゆる溶射法が知られているが、
この場合は、熱原単位が大きく、経済的でないばかり
か、得られるアルミナはα−アルミナが主成分ながら、
δ−アルミナなどを副生物として含み、熱伝導率を小さ
くするため、好ましくない。A so-called thermal spraying method is known in which the alumina of the Bayer method is injected into a high-temperature plasma or an oxyhydrogen flame, and is melted and rapidly cooled while being rounded.
In this case, not only is the heat unit large and not economical, but also the obtained alumina is mainly α-alumina,
It contains δ-alumina or the like as a by-product and is not preferable because it lowers the thermal conductivity.
【０００５】一方、コランダム粒子としては電融アルミ
ナや焼結アルミナの粉砕品が知られているが、いずれも
鋭いカッティングエッジを持つ不定形状の粒子であり、
ゴム・プラッスチックに充填する際、混練機、成形金型
等の磨耗が大きく好ましくない。[0005] On the other hand, pulverized products of fused alumina and sintered alumina are known as corundum particles, all of which are irregular shaped particles having a sharp cutting edge.
When filling rubber and plastic, the abrasion of a kneading machine, a molding die and the like is large, which is not preferable.
【０００６】[0006]
【発明が解決しようとする課題】上記公報に記載されて
いる方法によれば、カッティングエッジを有しない、平
均粒子径５〜３５μｍの球状コランダム粒子が得られて
いるものの、工業規模で安価に大量生産する為にはいく
つかの問題点があった。According to the method described in the above publication, spherical corundum particles having an average particle diameter of 5 to 35 μm having no cutting edge are obtained, but they are inexpensive on an industrial scale in large quantities. There were some problems in producing.
【０００７】該公報によれば、特定粒径を有する電融ア
ルミナおよび／又は焼結アルミナの粉砕品に、ハロゲン
化合物、硼素化合物及びアルミナ水和物の１種又は２種
以上を添加し、１０００〜１５５０℃で熱処理する方法
が開示されているものの、焼成物は焼成容器中で強固な
集塊を形成する。According to the publication, one or two or more of a halogen compound, a boron compound and an alumina hydrate are added to a pulverized product of fused alumina and / or sintered alumina having a specific particle size, and a powder of 1000 or more is added. Although a method of heat treatment at 1550 ° C. is disclosed, the fired product forms a strong agglomerate in the firing vessel.
【０００８】さらに、アルミナ水和物を添加することに
よリ、この集塊の硬さは低下することが開示されている
もの特性として充分ではない。特に、工業的規模で大量
生産するために、大きな焼成容器を使用した場合、焼成
物は焼成容器の大きさに対応した塊となり、その塊を解
砕・粉砕するにあたり、何段にもわたって解砕処理を実
施せねばならず、非常にコスト高であった。Further, it is disclosed that the addition of alumina hydrate lowers the hardness of the agglomerate, but this is not sufficient as a characteristic. In particular, when a large firing vessel is used for mass production on an industrial scale, the fired material becomes a lump corresponding to the size of the firing vessel, and when the lump is crushed and pulverized, it takes several stages. Crushing treatment had to be performed, which was very expensive.
【０００９】さらに、焼成物が、焼成容器内面に強固に
付着しているため、焼成容器からの排出も容易ではな
く、機械的応力をかけて取り出す等の処置を施す必要が
あった。この場合、焼成容器にかかる力も強大で、焼成
容器自身が破損してしまうなど、経済的でなかった。Further, since the fired product is firmly attached to the inner surface of the firing vessel, it is not easy to discharge the fired product from the firing vessel, and it is necessary to take measures such as taking out by applying a mechanical stress. In this case, the force applied to the firing container is also large, and the firing container itself is not economical, for example, being damaged.
【００１０】[0010]
【課題を解決するための手段】本発明者は、上記の従来
技術に鑑み、鋭意研究した結果、球状コランダム粒子の
製造方法において、熱処理の前段で、混合組成物を一旦
造粒し、その後焼成することによリ、上記課題を解決
し、本発明を完成するに至った。すなわち、本発明は以
下の手段によって達成される。Means for Solving the Problems In view of the above prior art, the present inventor has conducted intensive studies. As a result, in a method for producing spherical corundum particles, the mixed composition was granulated once before the heat treatment and then fired. By doing so, the above-mentioned problems have been solved, and the present invention has been completed. That is, the present invention is achieved by the following means.
【００１１】[１]平均粒子径が５〜３５μｍである電融
アルミナおよび／又は焼結アルミナと、ハロゲン化合
物、硼素化合物及びアルミナ水和物からなる群から選ば
れた少なくとも１種とを含む組成物を造粒した後、１０
００〜１６００℃で加熱処理し、次いで解砕する工程を
有することを特徴とする丸み状アルミナ粒子の製造方
法。 [２]解砕する工程の前又は後において、さらに酸で洗浄
する工程を含むことを特徴とする前項１記載の丸み状ア
ルミナ粒子の製造方法。 [３]酸で洗浄する工程後に、純水で洗浄し、乾燥する工
程を含むことを特徴とする前項２記載の丸み状アルミナ
粒子の製造方法。[1] A composition containing fused alumina and / or sintered alumina having an average particle size of 5 to 35 μm and at least one selected from the group consisting of halogen compounds, boron compounds and alumina hydrates. After granulating the product, 10
A method for producing round alumina particles, comprising a step of performing a heat treatment at 00 to 1600 ° C. and then crushing. [2] The method for producing round alumina particles according to the above [1], further comprising a step of washing with an acid before or after the step of crushing. [3] The method for producing round alumina particles according to the above item 2, comprising a step of washing with pure water and a step of drying after the step of washing with acid.
【００１２】[４]乾燥する工程が、減圧式の乾燥手段で
行われることを特徴とする前項３に記載の丸み状アルミ
ナ粒子の製造方法。 [５]電融アルミナおよび／又は焼結アルミナの粉砕品の
平均粒子径が、１０μｍ〜２５μｍである前項１乃至４
の何れか１項に記載の丸み状アルミナ粒子の製造方法。 [６]ハロゲン化合物が、AlF3、NaF、CaF2、MgF2及びNa3
AlF6からなる群から選ばれた少なくとも１種であること
を特徴とする前項１乃至５の何れか１項に記載の丸み状
アルミナ粒子の製造方法。 [７]硼素化合物が、B2O3、H3BO3、mNa2O・nB2O3及び硼
フッ素化合物からなる群から選ばれた少なくとも１種で
あることを特徴とする前項１乃至６の何れか１項記載の
丸み状アルミナ粒子の製造方法。[4] The method for producing round alumina particles according to the above item 3, wherein the drying step is performed by a drying means of a reduced pressure type. [5] The average particle diameter of the pulverized product of fused alumina and / or sintered alumina is from 10 μm to 25 μm.
The method for producing round alumina particles according to any one of the above. [6] The halogen compounds are AlF 3 , NaF, CaF 2 , MgF 2 and Na 3
6. The method for producing round alumina particles according to any one of the above items 1 to 5, wherein the method is at least one selected from the group consisting of AlF6. [7] The above-mentioned items 1 to 6, wherein the boron compound is at least one selected from the group consisting of B 2 O 3 , H 3 BO 3 , mNa 2 O · nB 2 O 3 and a boron-fluorine compound. The method for producing round alumina particles according to any one of the above.
【００１３】[８]アルミナ水和物が、水酸化アルミニウ
ム、アルミナゲル、非晶質水酸化アルミニウム及びアル
ミニウム化合物の部分水和物なる群から選ばれた少なく
とも１種であることを特徴とする前項１乃至７の何れか
１項に記載の丸み状アルミナ粒子の製造方法。 [９]電融アルミナ、焼結アルミナ、アルミナ水和物のα
線放射量が、０.０１c/cm2・hr以下であることを特徴と
する前項１乃至８の何れか１項に記載の丸み状アルミナ
粒子の製造方法。 [１０]造粒後の粒子径が、１〜３０ｍｍφであることを
特徴とする前項１乃至９の何れか１項に記載の丸み状ア
ルミナ粒子の製造方法。 [１１]水および／又は有機物水溶液を、造粒時にアルミ
ナ水和物に対して５〜５０質量％添加することを特徴と
する前項１乃至１０の何れか１項に記載の丸み状アルミ
ナ粒子の製造方法。[8] The preceding paragraph, wherein the alumina hydrate is at least one selected from the group consisting of aluminum hydroxide, alumina gel, amorphous aluminum hydroxide and partial hydrates of aluminum compounds. The method for producing round alumina particles according to any one of 1 to 7. [9] α of fused alumina, sintered alumina, alumina hydrate
9. The method for producing round alumina particles according to any one of the above items 1 to 8, wherein the linear radiation amount is 0.01 c / cm 2 · hr or less. [10] The method for producing round alumina particles according to any one of the above items 1 to 9, wherein the particle diameter after granulation is 1 to 30 mmφ. [11] The round alumina particles according to any one of [1] to [10] above, wherein 5 to 50% by mass of water and / or an organic solution is added to the alumina hydrate during granulation. Production method.
【００１４】[１２]前項１乃至１１の何れか１項に記載
の製造方法で得られた丸み状アルミナ粒子。 [１３]平均粒子径が５〜３５μｍである前項１２に記載
の丸み状アルミナ粒子。 [１４]α線放射量が ０.０１c/cm2・hr以下である前項
１３に記載丸み状アルミナ粒子。 [１５]前項１３又は１４に記載の丸み状アルミナ粒子を
含むことを特徴とする高熱伝導性ゴム組成物。 [１６]前項１３又は１４に記載の丸み状アルミナ粒子を
含むことを特徴とする高熱伝導性プラスチック組成物。[12] Round alumina particles obtained by the production method according to any one of the above items 1 to 11. [13] The round alumina particles according to the above item 12, having an average particle diameter of 5 to 35 μm. [14] The round alumina particles according to the above [13], which has an α-ray radiation amount of 0.01 c / cm 2 · hr or less. [15] A highly thermally conductive rubber composition comprising the round alumina particles according to the above item 13 or 14. [16] A highly thermally conductive plastic composition comprising the round alumina particles according to the above item 13 or 14.
【００１５】[0015]
【発明の実施の形態】以下、本発明について詳述する。
本発明は、平均粒子径が５〜３５μｍである電融アルミ
ナおよび／又は焼結アルミナと、ハロゲン化合物、硼素
化合物及びアルミナ水和物からなる群から選ばれた少な
くとも１種とを含む組成物を造粒した後、１０００〜１
６００℃で加熱処理し、次いで解砕することを特徴とす
る丸み状アルミナ粒子の製造方法を提供する。BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, the present invention will be described in detail.
The present invention provides a composition comprising fused alumina and / or sintered alumina having an average particle size of 5 to 35 μm and at least one selected from the group consisting of a halogen compound, a boron compound and alumina hydrate. After granulation, 1000-1
Provided is a method for producing round alumina particles, which is heat-treated at 600 ° C. and then crushed.
【００１６】本発明において出発原料として用いられる
アルミナ粗粒は、公知の製造方法で製造される、電融ア
ルミナあるいは焼結アルミナのいずれの粉砕品でも良
く、電融アルミナあるいは焼結アルミナの粒度分布は、
平均粒子径が５μｍ乃至３５μｍ、好ましくは１０μｍ
乃至２５μｍの範囲のもので、さらに好ましくは最大粒
子径は１５０μｍを超えず、望ましくは７５μｍ以下の
特性の物がよい。The alumina coarse particles used as a starting material in the present invention may be either pulverized fused alumina or sintered alumina produced by a known production method, and the particle size distribution of fused alumina or sintered alumina may be used. Is
Average particle size is 5 μm to 35 μm, preferably 10 μm
The maximum particle size is preferably not more than 150 μm, and more preferably 75 μm or less.
【００１７】平均粒子径が５μｍ未満の場合は、公知の
方法で丸みのある粒子形状が得られるため、本発明の製
造方法を適用する必要がない。また、出発原料であるア
ルミナ粗粒の丸み化を促進するために、必要に応じて、
予め丸み化促進剤としてアルミナ水和物を電融アルミナ
あるいは焼結アルミナに混合して加熱処理する。When the average particle diameter is less than 5 μm, a rounded particle shape can be obtained by a known method, so that it is not necessary to apply the production method of the present invention. Further, in order to promote the rounding of alumina coarse particles as a starting material, if necessary,
Alumina hydrate is previously mixed with electrofused alumina or sintered alumina as a rounding accelerator and heat-treated.
【００１８】アルミナ水和物としては、ギブサイト、バ
イヤライト、ベーマイト、ダイアスポアなどの水酸化ア
ルミニウム、アルミナゲル、擬ベーマイトなどの非晶質
の水酸化アルミニウム、さらには部分的に表面が水和さ
れた酸化アルミニウム（アルミナ）などのアルミニウム
化合物の部分水和物なども使用されるが、特に水酸化ア
ルミニウムやアルミナゲルあるいは熱反応性の良い微粒
アルミナが好ましい。経済的な観点からは、バイヤー法
水酸化アルミニウム（ギブサイト）が好ましく、その平
均粒子径が１０μｍ以下のものが最適である。Examples of the alumina hydrate include aluminum hydroxide such as gibbsite, bayerite, boehmite and diaspore, amorphous aluminum hydroxide such as alumina gel and pseudo-boehmite, and a partially hydrated surface. Although a partial hydrate of an aluminum compound such as aluminum oxide (alumina) is also used, aluminum hydroxide, alumina gel or fine alumina having good thermal reactivity is particularly preferable. From an economic viewpoint, the Bayer method aluminum hydroxide (gibbsite) is preferable, and the one having an average particle diameter of 10 μm or less is optimal.
【００１９】本発明者らの観察によると、前記丸み化促
進剤は、後述する必要に応じて添加する他の薬剤と相乗
的にアルミナ粗粒に作用し、不規則な鋭いカッテイング
エッジに選択的に作用（吸収され）し、アルミナ粗粒を
丸み化するという驚くべき現象が認められた。According to the observations of the present inventors, the rounding accelerator acts on the alumina coarse particles synergistically with other chemicals to be added as necessary, which will be described later, and selectively acts on the irregular sharp cutting edge. A surprising phenomenon of acting on (absorbing) and rounding the alumina coarse particles was observed.
【００２０】かかる丸み化促進剤の添加量は、電融アル
ミナあるいは焼結アルミナの粉砕品の粒度分布等により
異なり、制限できるものではないが、例えば水酸化アル
ミニウムを添加する場合には、アルミナ換算で電融アル
ミナおよび／または焼結アルミナに対して、５〜３００
質量％の範囲が好ましい。さらに、この添加量は、５０
〜１５０質量％の範囲が好ましい。前記添加量が５質量
％未満では、集塊の凝集力が強くなり、また、３００質
量％を超えると、過剰の水酸化アルミニウムが遊離し、
微粒のアルミナとして製品中に混入する恐れがある。The amount of the rounding accelerator added depends on the particle size distribution of the electrofused alumina or the sintered alumina and is not limited. 5 to 300 for fused alumina and / or sintered alumina
The range of mass% is preferred. Further, the amount added is 50
The range of -150 mass% is preferable. When the addition amount is less than 5% by mass, the cohesive force of the agglomerate becomes strong, and when it exceeds 300% by mass, excess aluminum hydroxide is liberated,
There is a possibility that fine alumina is mixed into the product.
【００２１】熱処理前の造粒工程で必要に応じて添加す
る他の薬剤としては、アルミナの結晶成長促進剤として
公知の化合物を単独または、併用して用いられる。この
結晶成長促進剤として、例えば、AlF3、NaF、CaF2、Na3
AlF6、MgF2からなる群より選ばれた少なくとも１種のフ
ッ素化合物で好ましく代表されるハロゲン化合物および
／またはB2O3、H3BO3、ｍNa2O・ｎＢ2Ｏ3、硼フッ素化
合物からなる群より選ばれた少なくとも１種の硼素化合
物が良い。As other chemicals to be added as needed in the granulation step before the heat treatment, compounds known as crystal growth promoters for alumina may be used alone or in combination. As this crystal growth promoter, for example, AlF 3 , NaF, CaF 2 , Na 3
AlF 6, halogen compound is preferably represented by at least one fluorine compound selected from the group consisting of MgF 2 and / or B 2 O 3, H 3 BO 3, mNa 2 O · nB 2 O 3, the boron fluorine compound At least one boron compound selected from the group consisting of
【００２２】特に、フッ素化合物と硼素化合物の併用、
もしくは硼フッ素化合物が好ましい。薬剤の添加量は、
加熱温度、炉内の滞留時間、加熱炉の種類により異なり
制限できるものではないが、例えば効果的な添加濃度は
全アルミナ分に対して０．１〜４質量％、好ましくは１
〜３質量％の範囲である。これら電融アルミナ及び／又
は焼結アルミナの粉砕品と、ハロゲン化合物、硼素化合
物及びアルミナ水和物からなる群より選ばれた少なくと
も１種とを含む組成物は、混合処理されて造粒後に加熱
される。In particular, a combination of a fluorine compound and a boron compound,
Alternatively, a borofluorine compound is preferable. The amount of drug added
The heating temperature, the residence time in the furnace, and the type of the heating furnace are different and cannot be limited.
-3% by mass. A composition containing the pulverized product of the fused alumina and / or the sintered alumina and at least one selected from the group consisting of a halogen compound, a boron compound, and an alumina hydrate is mixed and heated after granulation. Is done.
【００２３】また、上記の製法においてウラン・トリア
等の放射性元素の少ない電融アルミナ又は焼結アルミ
ナ、水酸化アルミニウム等を用いることにより低α線放
射量の丸み状アルミナ粒子を製造することができる。即
ち、本発明において使用される電融アルミナ、焼結アル
ミナ、アルミナ水和物は、α線放射量が、０.０１c/cm2
・hr以下の物がよい。Further, in the above-mentioned production method, by using fused alumina or sintered alumina containing little radioactive elements such as uranium and thoria, aluminum hydroxide, etc., it is possible to produce round alumina particles having a low α-ray radiation amount. . That is, the fused alumina, sintered alumina, and alumina hydrate used in the present invention have an α-ray emission of 0.01 c / cm 2.
・ Thing less than hr is good.
【００２４】α線放射量の少ない（0.01c/cm2・hr）丸
み状アルミナは、高集積度IC、LSI、VLSIの樹脂封止材
フィラーとして用いる場合、α線によるメモリー素子の
誤操作（いわゆるソフトエラー）を防止する目的のため
に特に有用である。When round alumina having a small amount of α-ray radiation (0.01 c / cm 2 · hr) is used as a resin sealing filler for highly integrated ICs, LSIs and VLSIs, erroneous operation of a memory element by α-rays (so-called This is particularly useful for the purpose of preventing soft errors.
【００２５】本発明で得られた丸み状アルミナは、若干
のカッテイングエッジが残存するものの、ゴム・プラス
チックに充填する際に混練機や成形時の金型の摩耗は実
使用上問題とならない粗大コランダム粒子である。The round alumina obtained by the present invention has a coarse cutting edge which does not pose a practical problem in kneaders or molds when filling rubber or plastic, although some cutting edges remain. Particles.
【００２６】次に、混合方法については、各々の成分が
均一に混合さえできれば良く、特に限定されるものでは
なく、粉体混合法として一般的な方法が利用できる。前
記方法として、例えば、ロッキングブレンダー、ナウタ
ーミキサー、リボンミキサー、V型ブレンダー、ヘンシ
ェルミキサーなどの混合装置が挙げられるが、それ以外
にも、ボールミル、振動ミルなどの粉砕機を使用しても
良い。The mixing method is not particularly limited as long as each component can be uniformly mixed, and a general method can be used as a powder mixing method. Examples of the method include a mixing device such as a rocking blender, a Nauter mixer, a ribbon mixer, a V-type blender, and a Henschel mixer.In addition, a ball mill or a crusher such as a vibration mill may be used. .
【００２７】また、混合時に水、アルコール等の溶媒
（媒体）を添加することも可能である。 これらの混合
組成物は、次に造粒処理される。造粒物は完全な球状で
ある必要はなく、焼成容器に充填した際に造粒物間に一
定以上の空隙を有する構造であればその形は制限されな
い。It is also possible to add a solvent (medium) such as water or alcohol during mixing. These mixed compositions are then granulated. The granulated material does not need to be perfectly spherical, and its shape is not limited as long as it has a certain gap or more between the granulated materials when filled in a firing vessel.
【００２８】具体的には、焼成容器への充填密度が造粒
物の理論密度の０．２５〜０．５０倍の範囲であれば良
い。また、好ましい範囲は、０．２５〜０．３０倍であ
る。０．５０倍よりも大きいと、焼成物は焼成容器と一
体化した強固な集塊となるため、好ましくなく、０．２
５倍より小さいと、焼成物は造粒物単位には簡単に解せ
るものの、充填密度が低すぎる為、焼成効率が悪くて経
済的でない。Specifically, the packing density in the firing container may be in the range of 0.25 to 0.50 times the theoretical density of the granulated product. Further, a preferable range is 0.25 to 0.30 times. If it is larger than 0.50 times, the fired product becomes a strong agglomerate integrated with the firing container, so that it is not preferable.
If the ratio is less than 5 times, the fired product can be easily understood in units of granules, but the packing density is too low, so that the firing efficiency is poor and it is not economical.
【００２９】造粒物の大きさについては、焼成後の解砕
を容易にするためには、小さい方が良いが、小さすぎる
と、前述の充填範囲を逸脱する為、好ましくない。焼成
容器の大きさに応じて、適当な大きさを選定すれば良い
が、一般的には、投影円相当径で１〜３０mmφ、好まし
くは５〜２０mmφである。ここで、投影円相当径とは、
粉体工学便覧（粉体工学会編)等に記載されているHeywo
od径である。The size of the granulated material is preferably small in order to facilitate the disintegration after firing, but too small is not preferable because it deviates from the above-mentioned filling range. An appropriate size may be selected according to the size of the firing vessel, but generally, the projected circle equivalent diameter is 1 to 30 mmφ, preferably 5 to 20 mmφ. Here, the projected circle equivalent diameter is
Heywo listed in Powder Engineering Handbook (edited by the Powder Engineering Society)
od diameter.
【００３０】造粒の方法については、上記の造粒物が作
製できれば、何ら手段には限定されない。造粒装置とし
ては、例えば、撹拌混合型造粒機、流動層造粒機、圧縮
型造粒機などが用いられるが、パン型造粒機等が経済的
観点から好ましい。The granulation method is not limited to any means as long as the above-mentioned granulated material can be produced. As the granulating device, for example, a stirring-mixing-type granulator, a fluidized-bed granulator, a compression-type granulator and the like are used, and a pan-type granulator is preferable from an economic viewpoint.
【００３１】造粒の際に、必要に応じて、水、アルコー
ルなどの液媒体、あるいは、ポリビニルアルコール（PV
A）やポリアクリル系樹脂等の有機バインダー溶液を添
加してもよい。有機バインダーを添加することは、造粒
品が適度な強度を有するため、ハンドリング時の造粒品
の崩壊等が少なく好ましい。造粒品にそれほどの強度が
必要ない場合には、経済的観点から水を添加することが
最適である。At the time of granulation, if necessary, a liquid medium such as water or alcohol, or polyvinyl alcohol (PV)
An organic binder solution such as A) or a polyacrylic resin may be added. Addition of an organic binder is preferable because the granulated product has an appropriate strength, and therefore, the granulated product is less likely to collapse during handling. If the granulated product does not require much strength, it is best to add water from an economic point of view.
【００３２】前記液媒体や有機バインダーの添加量につ
いては、使用する粗大アルミナ粒子の粒子径、水酸化ア
ルミニウムを添加する場合には、その粒子径、添加量等
により、適宜選択すればよいが、好ましい範囲は水酸化
アルミニウムの添加量に対して５〜５０質量％であり、
２５〜４０質量％が最適である。 ５０質量％より多い
と、組成物全体が流動化し、造粒できなくなるので、好
ましくない。 ５質量％より少ないと、造粒物の強度が
著しく低下し、崩壊するため、もはや、造粒物としての
形態をなさなくなるので、好ましくない。The amount of the liquid medium or the organic binder to be added may be appropriately selected depending on the particle size of the coarse alumina particles to be used and the particle size and the amount of aluminum hydroxide when aluminum hydroxide is added. A preferred range is 5 to 50% by mass relative to the amount of aluminum hydroxide added,
25 to 40% by mass is optimal. If the amount is more than 50% by mass, the whole composition is fluidized and cannot be granulated, which is not preferable. If the amount is less than 5% by mass, the strength of the granulated material is remarkably reduced and disintegrated, so that it no longer forms a granulated material, which is not preferable.
【００３３】造粒品は次いで、熱処理される。熱処理工
程において、前記有機バインダーは焼失する。熱処理に
使用される加熱炉の種類としては、単窯、トンネル窯、
ロータリーキルンのような公知の手段で良く、加熱温度
は１０００℃以上であれば本発明の目的は達成される。
特に好ましい加熱処理温度範囲は１３５０℃以上、１６
００℃以下である。１６００℃を超えると、粒子間の凝
集力が強くなり、一次粒子への解砕が容易に進まなくな
る。[0033] The granulated product is then heat treated. In the heat treatment step, the organic binder is burned off. The types of heating furnaces used for heat treatment include single kilns, tunnel kilns,
A known means such as a rotary kiln may be used, and the object of the present invention is achieved if the heating temperature is 1000 ° C. or higher.
A particularly preferred heat treatment temperature range is 1350 ° C. or higher,
It is below 00 ° C. When the temperature exceeds 1600 ° C., the cohesive force between the particles increases, and the crushing into primary particles does not easily proceed.
【００３４】加熱炉の滞留時間は加熱温度によって異な
るが、３０分以上、好ましくは１時間乃至３時間程度の
滞留時間が必要である。かかる方法により、製造された
粗大アルミナ粒子は、二次凝集粒の形態をとるため、公
知の粉砕手段、例えばボールミル、振動ミル、ジェット
ミルなどによる解砕を経て所望の粒度分布の丸み状アル
ミナ粒子が得られる。Although the residence time of the heating furnace varies depending on the heating temperature, a residence time of 30 minutes or more, preferably about 1 to 3 hours is required. The coarse alumina particles produced by such a method are rounded alumina particles having a desired particle size distribution through pulverization by a known pulverizing means, for example, a ball mill, a vibration mill, a jet mill, etc., in order to take the form of secondary aggregated particles. Is obtained.
【００３５】ICなどの封止材などイオン性不純物を嫌う
用途に使用する場合には、得られたアルミナ粉体をその
解砕前、または解砕後、あるいはその両者にて水、酸、
アルカリなどで洗浄することも可能である。When used for applications that dislike ionic impurities such as sealing materials for ICs, the obtained alumina powder is subjected to water, acid, or the like before or after crushing, or both.
It is also possible to wash with an alkali or the like.
【００３６】洗浄方法については、特に限定されるもの
ではないが、上記の製法で得られる球状アルミナ粒子の
典型的なイオン性不純物はF、B、Nａなどの元素が主成
分である為、酸性液中に球状アルミナ粒子を懸濁し、所
定時間経過後、ろ別し、純水などで洗浄後、乾燥するこ
とが好ましい。使用する酸については、ＨＣｌ、ＨNO 3
などの酸（１塩基酸）では、ろ過速度が低い場合があ
り、酸の中でも多塩基酸が好ましい。特に経済的観点か
らクエン酸、リン酸、硫酸等が好ましい。The washing method is not particularly limited.
Not, but of the spherical alumina particles obtained by the above manufacturing method
Typical ionic impurities are mainly composed of elements such as F, B and Na.
Minutes, suspend the spherical alumina particles in the acid solution,
After a certain period of time, filter, wash with pure water and dry.
Is preferred. HCl, HNO Three
For such acids (monobasic acids), the filtration speed may be low.
Of these acids, polybasic acids are preferred. Especially economic point of view
Citric acid, phosphoric acid, sulfuric acid and the like are preferred.
【００３７】酸濃度は特に限定されず、スラリー状態で
のｐＨが酸性領域であれば良く、一般的には０．０１Ｎ
〜５Ｎであり、好ましくは０.１〜１Ｎの範囲である。
０．０１Ｎ以下ではスラリーのｐＨがアルカリ性になる
場合があり、好ましくなく、１Ｎ以上では、経済的でな
いばかりか、添加した酸がアルミナ中に残存するために
好ましくない。The acid concentration is not particularly limited, as long as the pH in the slurry state is in an acidic range, generally 0.01 N
To 5N, preferably in the range of 0.1 to 1N.
If the pH is less than 0.01 N, the pH of the slurry may be alkaline, which is not preferable. If the pH is 1 N or more, it is not economical and the added acid remains in alumina, which is not preferable.
【００３８】粉体と液との割合（スラリー濃度）につい
ても特に限定されず、反応容器の撹拌力、形状等により
適宜選定すれば良く、通常は50〜1000ｇ／リットル、好
ましくは、200〜800ｇ／リットル、さらに好ましくは30
0〜600ｇ／リットルである。1000ｇ／リットルよりも固
形分が多いと、沈降等が著しく、５０ｇ／リットルより
も固形分が少ないと、効率的でない。The ratio between the powder and the liquid (slurry concentration) is not particularly limited, and may be appropriately selected depending on the stirring power and the shape of the reaction vessel, and is usually 50 to 1000 g / liter, preferably 200 to 800 g. / Liter, more preferably 30
It is 0 to 600 g / liter. When the solid content is more than 1000 g / liter, sedimentation and the like are remarkable, and when the solid content is less than 50 g / liter, it is not efficient.
【００３９】酸処理温度についても、特に限定されない
が、通常は６０℃以上、好ましくは８０℃以上である。
６０℃より低いと、抽出不純物量が少ないだけでなく、
ろ過速度も遅くなり好ましくない。The acid treatment temperature is also not particularly limited, but is usually 60 ° C. or higher, preferably 80 ° C. or higher.
If the temperature is lower than 60 ° C., not only is the amount of extracted impurities small, but also
The filtration speed is also slow, which is not preferable.
【００４０】ろ過の方法についても、特に限定されず、
ドラムフィルター、ホリゾンタルフィルター、水平ベル
トフィルターなどの真空ろ過機、加圧ドラムフィルタ
ー、リーフフィルター、フィルタープレスなどの加圧ろ
過機、ベルトプレス、スクリュープレスなどの圧搾ろ過
機、さらには、スクリューデカンターなどの遠心沈降
機、遠心ろ過機などが用いられる。The method of filtration is not particularly limited, either.
Vacuum filters such as drum filters, horizontal filters, horizontal belt filters, etc., pressure filters such as pressurized drum filters, leaf filters, filter presses, press filters such as belt presses and screw presses, and screw decanters etc. A centrifugal settler, a centrifugal filter or the like is used.
【００４１】洗浄水量については、要求される不純物レ
ベルに応じて適宜選定すればいいが、通常はアルミナ１
ｋｇあたり、１リットル以上、好ましくは1〜３リット
ルである。１リットル未満では、不純物が残存する為に
好ましくなく、３リットルを超える量は経済的でない。The amount of washing water may be appropriately selected according to the required impurity level.
It is 1 liter or more, preferably 1 to 3 liters per kg. If the amount is less than 1 liter, impurities remain, which is not preferable. An amount exceeding 3 liters is not economical.
【００４２】洗浄されたケーキの乾燥方法については、
残水量が０．１質量％以下に乾燥できれば特に限定する
ものではなく、汎用の乾燥機が使用できる。このような
乾燥機としては、箱型乾燥機、トンネル型乾燥機、バン
ド型乾燥機、流動乾燥機、バドルドライヤーなどの、粉
体乾燥に使用できるものを、適宜用いれば良い。Regarding the method of drying the washed cake,
There is no particular limitation as long as the residual water content can be dried to 0.1% by mass or less, and a general-purpose dryer can be used. As such a dryer, a box dryer, a tunnel dryer, a band dryer, a fluid dryer, a paddle dryer, and the like that can be used for powder drying may be appropriately used.
【００４３】また、乾燥時に高温化にさらされると、粉
体中のアルカリイオンの拡散速度が上昇し、粉体表面に
移行するため、できるだけ低温で乾燥させることが好ま
しく、そのような乾燥機としては、減圧下（減圧式）で
加熱する振動流動乾燥機が最適である。If the powder is exposed to a high temperature during drying, the diffusion rate of the alkali ions in the powder increases, and the powder moves to the powder surface. Therefore, it is preferable to dry the powder at a temperature as low as possible. The best is a vibrating fluidized dryer that heats under reduced pressure (reduced pressure method).
【００４４】本発明の製造方法で製造される丸み状アル
ミナ粒子は、好ましくはゴムやプラスチックに充填さ
れ、高熱伝導性ゴム組成物や高熱伝導性プラスチック組
成物として利用される。特にその含有量は、８０質量％
以上が好ましい。The round alumina particles produced by the production method of the present invention are preferably filled in rubber or plastic and used as a highly thermally conductive rubber composition or a highly thermally conductive plastic composition. Particularly, the content is 80% by mass.
The above is preferred.
【００４５】本発明においては、前記高熱伝導性プラス
チック組成物を構成するプラスチック（樹脂）には制限
されず公知な樹脂が適用されるが、例えば、不飽和ポリ
エステル樹脂、アクリル樹脂、ビニルエステル樹脂、エ
ポキシ樹脂等、キシレンホルムアルデヒド樹脂、グアナ
ミン樹脂、ジアリルフタレート樹脂、フェノール樹脂、
フラン樹脂、ポリイミド樹脂、メラミン樹脂、ユリア樹
脂等が挙げられる。好ましくは、不飽和ポリエステル樹
脂、アクリル樹脂、ビニルエステル樹脂、エポキシ樹脂
等が例示できる。In the present invention, a known resin is applied without being limited to the plastic (resin) constituting the high thermal conductive plastic composition. For example, unsaturated polyester resin, acrylic resin, vinyl ester resin, Epoxy resin, xylene formaldehyde resin, guanamine resin, diallyl phthalate resin, phenol resin,
Furan resin, polyimide resin, melamine resin, urea resin and the like can be mentioned. Preferably, an unsaturated polyester resin, an acrylic resin, a vinyl ester resin, an epoxy resin and the like can be exemplified.
【００４６】本発明においては、前記高熱伝導性ゴム組
成物を構成するゴム素材（ゴム成分等）には制限され
ず、公知なゴム素材が適用される。以下、実施例・比較
例によって、本発明を具体的に説明するが、本発明はこ
れらの実施例に限定されるものではない。In the present invention, the rubber material (rubber component and the like) constituting the high thermal conductive rubber composition is not limited, and a known rubber material is applied. Hereinafter, the present invention will be described specifically with reference to Examples and Comparative Examples, but the present invention is not limited to these Examples.
【００４７】[0047]
【実施例】（充填密度の測定方法）造粒品の充填密度は
以下の方法で求めた。すなわち、造粒品を静かにシリン
ダー内に充填し、その時の体積と重量から見かけの比重
を算出し、配合品の組成比から計算される理論密度との
比で表した。EXAMPLES (Method of measuring packing density) The packing density of the granulated product was determined by the following method. That is, the granulated product was gently filled into a cylinder, the apparent specific gravity was calculated from the volume and weight at that time, and the ratio was expressed as a ratio to the theoretical density calculated from the composition ratio of the blended product.
【００４８】（実施例１〜５、比較例１）市販の焼結ア
ルミナ粉砕品（平均粒子径２５μｍ、最大粒子径７５μ
ｍ ）１００質量部に対して、無水フッ化アルミニウム
（森田化学（株）製）及び硼酸（U.S.Borax Inc.製）
をそれぞれ２．５質量部、水酸化アルミニウム（昭和電
工（株）製、平均粒子径１μｍ）を５０質量部添加、V
型ブレンダーを用い混合後、パン型造粒装置にて、表１
に示す条件で造粒した。また、造粒物の充填密度を測定
し表１に示した。次いで、造粒物をコランダムームライ
ト質の耐熱焼成容器に装入し、トンネルキルン炉内で最
高温度１３８０℃、滞留時間３時間で加熱処理した。耐
熱焼成容器(１０個中)から、排出時に破損した耐熱焼成
容器の割合（サヤ破損率）を求め表１に示した。さら
に、焼成物の硬さを、表１中の内容で相対値比較した
（５段階で相対評価）。そして、粗砕物をボールミルに
て、表１に示す時間解砕し、粒度分布をマイクロトラッ
ク粒度分析計で測定した。(Examples 1 to 5, Comparative Example 1) Commercially available pulverized sintered alumina (average particle diameter 25 μm, maximum particle diameter 75 μm)
m) Anhydrous aluminum fluoride (Morita Chemical Co., Ltd.) and boric acid (USBorax Inc.) per 100 parts by mass
And 2.5 parts by mass of each, and 50 parts by mass of aluminum hydroxide (manufactured by Showa Denko KK, average particle diameter 1 μm) were added.
After mixing using a mold blender, the mixture was mixed with a pan-type granulator as shown in Table 1.
The granulation was carried out under the conditions shown in FIG. The packing density of the granulated product was measured and the results are shown in Table 1. Next, the granulated product was charged into a corundum humorous heat-resistant sintering vessel, and heat-treated in a tunnel kiln furnace at a maximum temperature of 1380 ° C. and a residence time of 3 hours. From the heat-resistant sintering containers (out of 10), the ratio of the heat-resistant sintering containers that were damaged at the time of discharge (shear damage rate) was determined and shown in Table 1. Further, the hardness of the fired product was compared with a relative value based on the contents in Table 1 (relative evaluation in five steps). The crushed material was crushed by a ball mill for the time shown in Table 1, and the particle size distribution was measured by a Microtrac particle size analyzer.
【００４９】（比較例２）水酸化アルミニウムを添加せ
ず、造粒処理を実施しなかった以外は実施例１と同様に
実施した。結果は表１に示した。Comparative Example 2 The same operation as in Example 1 was carried out except that no aluminum hydroxide was added and the granulation treatment was not carried out. The results are shown in Table 1.
【００５０】（比較例３）水酸化アルミニウムの添加量
を３００質量部とした以外は、比較例１と同様に実施し
た。結果は表１に示した。(Comparative Example 3) The same operation as in Comparative Example 1 was carried out except that the addition amount of aluminum hydroxide was changed to 300 parts by mass. The results are shown in Table 1.
【００５１】[0051]
【表１】 [Table 1]
【００５２】（実施例６〜１２）実施例５で得られたア
ルミナ粒子について、表２に示す条件にて、洗浄処理を
実施した。ろ過機としては、水平型ベルトフイルターを
用いた。ろ過速度は、別途ブフナー漏斗を用い所定量の
スラリーをろ過、洗浄した際のろ過時間測定し、
「（１）極めて速い」〜「（５）極めて遅い」までの５
段階で評価した。乾燥機は実施例１０を除いて、箱型乾
燥機を使用し、実施例１０については、振動流動乾燥機
を用いた。導電率については粉体２０ｇを精製水１００
ｍｌに懸濁させたスラリーについて、室温で測定した。
イオン性不純物量については、１００℃の温湯にて、２
時間抽出し、液中不純物量から算出した。(Examples 6 to 12) The alumina particles obtained in Example 5 were washed under the conditions shown in Table 2. A horizontal belt filter was used as a filter. Filtration speed, a predetermined amount of slurry was separately filtered using a Buchner funnel, and the filtration time when washing was measured.
5 from "(1) extremely fast" to "(5) extremely slow"
It was evaluated on a scale. Except for Example 10, a box-shaped dryer was used as the dryer. In Example 10, a vibrating fluidized dryer was used. Regarding the electrical conductivity, 20 g of powder was added to 100 parts of purified water.
The slurry suspended in ml was measured at room temperature.
About the amount of ionic impurities,
It was extracted for a time and calculated from the amount of impurities in the liquid.
【００５３】[0053]
【表２】 [Table 2]
【００５４】実施例１３ 市販の低α線タイプのアルミナ（昭和電工（株）製、α
線放射量0.01c/cm2・hr以下）を電融して得たインゴッ
トを放射性元素のコンタミが混入しない条件で解砕・粉
砕・分級して得た平均粒子径３０μｍの電融アルミナ粗
大粒子（α線放射線量0.005c/cm2・hr）２５０ｇを添加
し、実施例１と同様に焼成・解砕を実施したところ、造
粒粒子径が1〜5ｍｍ、充填密度が0.31（相対比）、焼成
物は容易に手でほぐれる硬さであり、解砕時間１５分、
平均粒子径が３３μｍであって、α線放射量が0.004c/c
m2・hrの丸み状アルミナ粒子が得られた。Example 13 Commercially available low α ray type alumina (manufactured by Showa Denko KK, α
(Emission of 0.01 c / cm 2 · hr or less of linear radiation) Electrolytic alumina coarse particles with an average particle diameter of 30 μm obtained by crushing, pulverizing, and classifying ingots obtained by electrofusing radioactive elements without contamination. (Α-ray radiation dose 0.005 c / cm 2 · hr) 250 g was added, and calcination and crushing were carried out in the same manner as in Example 1. The granulated particle diameter was 1 to 5 mm and the packing density was 0.31 (relative ratio). The calcined product has a hardness that can be easily loosened by hand, and has a crushing time of 15 minutes.
The average particle diameter is 33 μm, and the amount of α-ray radiation is 0.004 c / c.
Round alumina particles of m 2 · hr were obtained.
【００５５】（実施例１４）実施例８と同様にして、実
施例１３で調製した低α線タイプのアルミナを使用し
て、表２に示す実施例８の条件にて、洗浄処理を実施し
たところ、導電率４μＳ／ｃｍ、Ｎａ+濃度が５ｐｐ
ｍ、ＳＯ4 2-濃度が７ｐｐｍであった。(Example 14) In the same manner as in Example 8, the cleaning treatment was performed under the conditions of Example 8 shown in Table 2 using the low α-ray type alumina prepared in Example 13. However, the conductivity is 4 μS / cm and the Na + concentration is 5 pp.
m, SO 4 2− concentration was 7 ppm.
【００５６】[0056]
【発明の効果】本発明の製造方法により、丸み状の粗大
アルミナ粒子を安価に工業的に生産することが可能とな
り、本製造方法で製造された丸み状アルミナ粒子は、優
れた流動性を示すだけでなく、実質的に機械装置の摩耗
が問題にならない丸み状の粗大粒子である。According to the production method of the present invention, it is possible to industrially produce round coarse alumina particles at low cost, and the round alumina particles produced by this production method exhibit excellent fluidity. Not only that, it is a rounded coarse particle that substantially does not cause a problem of mechanical device wear.
───────────────────────────────────────────────────── フロントページの続き Ｆターム(参考） 4G076 AA02 CA01 CA03 CA26 CA29 CA36 CA37 DA02 DA30 FA02 4J002 AC001 BF051 BG001 CC031 CC041 CC121 CC161 CC181 CC191 CD001 CD201 CF211 CM041 DE146 FA08 FD016 ──────────────────────────────────────────────────続 き Continued on the front page F term (reference) 4G076 AA02 CA01 CA03 CA26 CA29 CA36 CA37 DA02 DA30 FA02 4J002 AC001 BF051 BG001 CC031 CC041 CC121 CC161 CC181 CC191 CD001 CD201 CF211 CM041 DE146 FA08 FD016
Claims (16)
ミナおよび／又は焼結アルミナと、ハロゲン化合物、硼
素化合物及びアルミナ水和物からなる群から選ばれた少
なくとも１種とを含む組成物を造粒した後、１０００〜
１６００℃で加熱処理し、次いで解砕する工程を有する
ことを特徴とする丸み状アルミナ粒子の製造方法。1. A composition comprising fused alumina and / or sintered alumina having an average particle size of 5 to 35 μm and at least one selected from the group consisting of halogen compounds, boron compounds and alumina hydrate. After granulating, 1000-
A method for producing round alumina particles, comprising a step of performing heat treatment at 1600 ° C. and then crushing.
酸で洗浄する工程を含むことを特徴とする請求項１記載
の丸み状アルミナ粒子の製造方法。2. The method for producing round alumina particles according to claim 1, further comprising a step of washing with an acid before or after the step of crushing.
燥する工程を含むことを特徴とする請求項２記載の丸み
状アルミナ粒子の製造方法。3. The method for producing round alumina particles according to claim 2, further comprising a step of washing with pure water and drying after the step of washing with acid.
れることを特徴とする請求項３に記載の丸み状アルミナ
粒子の製造方法。4. The method for producing round alumina particles according to claim 3, wherein the drying step is performed by a drying means of a reduced pressure type.
粉砕品の平均粒子径が、１０μｍ〜２５μｍである請求
項１乃至４の何れか１項に記載の丸み状アルミナ粒子の
製造方法。5. The method for producing round alumina particles according to claim 1, wherein the average particle size of the pulverized product of fused alumina and / or sintered alumina is 10 μm to 25 μm.
2及びNa3AlF6からなる群から選ばれた少なくとも１種で
あることを特徴とする請求項１乃至５の何れか１項に記
載の丸み状アルミナ粒子の製造方法。6. The method according to claim 1, wherein the halogen compound is AlF 3 , NaF, CaF 2 , MgF
The method for producing round alumina particles according to any one of claims 1 to 5, wherein the method is at least one selected from the group consisting of 2 and Na 3 AlF 6 .
3及び硼フッ素化合物からなる群から選ばれた少なくと
も１種であることを特徴とする請求項１乃至６の何れか
１項記載の丸み状アルミナ粒子の製造方法。7. The boron compound is B 2 O 3 , H 3 BO 3 , mNa 2 O · nB 2 O
The method for producing round alumina particles according to any one of claims 1 to 6, wherein the method is at least one selected from the group consisting of 3 and a borofluoride compound.
アルミナゲル、非晶質水酸化アルミニウム及びアルミニ
ウム化合物の部分水和物なる群から選ばれた少なくとも
１種であることを特徴とする請求項１乃至７の何れか１
項に記載の丸み状アルミナ粒子の製造方法。8. The method according to claim 8, wherein the alumina hydrate is aluminum hydroxide,
8. A method according to claim 1, wherein the at least one selected from the group consisting of alumina gel, amorphous aluminum hydroxide and partial hydrates of aluminum compounds.
The method for producing round alumina particles according to the above item.
和物のα線放射量が、０.０１c/cm2・hr以下であること
を特徴とする請求項１乃至８の何れか１項に記載の丸み
状アルミナ粒子の製造方法。9. The method according to claim 1, wherein the amount of α-ray radiation of the fused alumina, the sintered alumina, and the alumina hydrate is 0.01 c / cm 2 · hr or less. 3. The method for producing round alumina particles according to 1.).
ることを特徴とする請求項１乃至９の何れか１項に記載
の丸み状アルミナ粒子の製造方法。10. The method for producing round alumina particles according to claim 1, wherein the particle diameter after granulation is 1 to 30 mmφ.
にアルミナ水和物に対して５〜５０質量％添加すること
を特徴とする請求項１乃至１０の何れか１項に記載の丸
み状アルミナ粒子の製造方法。11. The round shape according to claim 1, wherein 5 to 50% by mass of water and / or an aqueous solution of an organic substance is added to the alumina hydrate during granulation. A method for producing alumina particles.
製造方法で得られた丸み状アルミナ粒子。12. Round alumina particles obtained by the production method according to claim 1. Description:
１２に記載の丸み状アルミナ粒子。13. The round alumina particles according to claim 12, having an average particle diameter of 5 to 35 μm.
ある請求項１３に記載丸み状アルミナ粒子。14. The round alumina particles according to claim 13, having an α-ray radiation amount of 0.01 c / cm 2 · hr or less.
ミナ粒子を含むことを特徴とする高熱伝導性ゴム組成
物。15. A highly thermally conductive rubber composition comprising the round alumina particles according to claim 13 or 14.
ミナ粒子を含むことを特徴とする高熱伝導性プラスチッ
ク組成物。16. A highly thermally conductive plastic composition comprising the round alumina particles according to claim 13 or 14.
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| US10/363,669 US7053018B2 (en) | 2001-05-30 | 2002-05-28 | Spherical alumina particles and production process thereof |
| PCT/JP2002/005156 WO2002098796A1 (en) | 2001-05-30 | 2002-05-28 | Spherical alumina particles and production process thereof |
| CNB028019741A CN100469698C (en) | 2001-05-30 | 2002-05-28 | Alumina particle and method for producing same |
| HK04103978.6A HK1061008A1 (en) | 2001-05-30 | 2004-06-03 | Spherical alumina particles and production process thereof |
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| JP2005022963A (en) * | 2003-06-12 | 2005-01-27 | Showa Denko Kk | Method of producing alumina particle, and composition |
| JP2005263529A (en) * | 2004-03-17 | 2005-09-29 | Sumitomo Chemical Co Ltd | Method for producing activated alumina having low alkali content |
| WO2009017170A1 (en) * | 2007-07-31 | 2009-02-05 | Denki Kagaku Kogyo Kabushiki Kaisha | Alumina powder, process for producing the same, and composition containing the same |
| WO2009133904A1 (en) * | 2008-04-30 | 2009-11-05 | 電気化学工業株式会社 | Alumina powder, process for production of the same, and resin compositions containing the same |
| JP2010126385A (en) * | 2008-11-26 | 2010-06-10 | Denki Kagaku Kogyo Kk | Spherical alumina powder and method for producing the same |
| US7789330B2 (en) | 2004-03-15 | 2010-09-07 | Showa Denko K.K. | Roundish fused alumina particles, production process thereof, and resin composition containing the particles |
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| US7789330B2 (en) | 2004-03-15 | 2010-09-07 | Showa Denko K.K. | Roundish fused alumina particles, production process thereof, and resin composition containing the particles |
| JP2005263529A (en) * | 2004-03-17 | 2005-09-29 | Sumitomo Chemical Co Ltd | Method for producing activated alumina having low alkali content |
| WO2009017170A1 (en) * | 2007-07-31 | 2009-02-05 | Denki Kagaku Kogyo Kabushiki Kaisha | Alumina powder, process for producing the same, and composition containing the same |
| JP5336374B2 (en) * | 2007-07-31 | 2013-11-06 | 電気化学工業株式会社 | Method for producing alumina powder |
| WO2009133904A1 (en) * | 2008-04-30 | 2009-11-05 | 電気化学工業株式会社 | Alumina powder, process for production of the same, and resin compositions containing the same |
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| KR101505237B1 (en) * | 2008-04-30 | 2015-03-23 | 덴키 가가쿠 고교 가부시기가이샤 | Alumina powder, process for production of the same, and resin compositions containing the same |
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| JP2010126385A (en) * | 2008-11-26 | 2010-06-10 | Denki Kagaku Kogyo Kk | Spherical alumina powder and method for producing the same |
| WO2017047452A1 (en) * | 2015-09-16 | 2017-03-23 | 大日精化工業株式会社 | Alumina-based heat conductive oxide and method for producing same |
| JP6121074B1 (en) * | 2015-09-16 | 2017-04-26 | 大日精化工業株式会社 | Alumina-based thermally conductive oxide and method for producing the same |
| KR20180040654A (en) * | 2015-09-16 | 2018-04-20 | 다이니치 세이카 고교 가부시키가이샤 | Alumina-based thermally conductive oxides and method for manufacturing the same |
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| KR102070215B1 (en) * | 2015-09-16 | 2020-01-29 | 다이니치 세이카 고교 가부시키가이샤 | Alumina-based thermally conductive oxides and method for producing same |
| US11459276B2 (en) | 2015-09-16 | 2022-10-04 | Dainichiseika Color & Chemicals Mfg. Co., Ltd. | Alumina-based heat conductive oxide and method for producing same |
| JP6209695B1 (en) * | 2017-03-02 | 2017-10-04 | 大日精化工業株式会社 | Alumina-based thermally conductive oxide and method for producing the same |
| WO2018159608A1 (en) * | 2017-03-02 | 2018-09-07 | 大日精化工業株式会社 | Alumina-based thermally conductive oxide and method for producing same |
| JP2018145025A (en) * | 2017-03-02 | 2018-09-20 | 大日精化工業株式会社 | Alumina-based heat conductive oxide and method for producing the same |
| US11072735B2 (en) | 2019-02-18 | 2021-07-27 | Admatechs Co., Ltd. | Particulate material and thermal conductive substance |
| JP7406444B2 (en) | 2020-04-22 | 2023-12-27 | 株式会社アドマテックス | Method for producing spherical particle material |
Also Published As
| Publication number | Publication date |
|---|---|
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| HK1061008A1 (en) | 2004-09-03 |
| CN1463251A (en) | 2003-12-24 |
| JP4920141B2 (en) | 2012-04-18 |
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