JP4307451B2 - Boron nitride powder, production method and use thereof - Google Patents
Boron nitride powder, production method and use thereof Download PDFInfo
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本発明は、窒化ホウ素粉末、その製造方法及び用途に関する。 The present invention relates to boron nitride powder, a method for producing the same, and use thereof.
窒化ホウ素（ＢＮ）粉末は、熱伝導性、電気絶縁性、化学的安定性等に優れており、固体潤滑剤、離型剤、焼結体原料などに利用されている。これらに適用するには、窒化ホウ素粉末は水スラリーに調製されることが多い。水スラリーに要求される特性は、低粘度かつ高濃度である。 Boron nitride (BN) powder is excellent in thermal conductivity, electrical insulation, chemical stability, and the like, and is used as a solid lubricant, a release agent, a sintered body raw material, and the like. For these applications, boron nitride powder is often prepared in a water slurry. The properties required for the water slurry are low viscosity and high concentration.
普通に入手できる市販の窒化ホウ素粉末を用いた水スラリーの濃度は、２５℃粘度が１０００〜７５００ｍＰａ・ｓであるときに１５〜３０質量％であり、更なる低粘度かつ高濃度の要求があった。また、このような水スラリーを調製するには、多くの添加剤を必要としており（特許文献１）、それによる問題、例えば高温下で使用される離型剤では有機化合物の分解物が製品に混入することによる着色の問題があった。窒化ホウ素粉末をシランカップリング剤で処理する提案もあるが（特許文献２）、ＢＮ結晶は厚み（ｃ軸）方向の長さに対する幅（ａ軸）方向の長さの比で表される扁平度（以下、「アスペクト比」という。）が小さいので、ＯＨ基をａ軸に存在させることが困難であり、十分な表面処理の効果はなかった。
本発明の目的は、低粘度かつ高濃度の水スラリーを調製することのできる窒化ホウ素粉末とその製造方法、及び２５℃粘度が７５００ｍＰａ・ｓ以下にして窒化ホウ素粉末濃度が４０質量％以上である低粘度かつ高濃度の窒化ホウ素の水スラリーを提供することである。 An object of the present invention is to provide a boron nitride powder capable of preparing a low-viscosity and high-concentration water slurry, a method for producing the same, and a 25 ° C. viscosity of 7500 mPa · s or less and a boron nitride powder concentration of 40% by mass or more. It is to provide a low viscosity and high concentration aqueous boron nitride slurry.
本発明は、以下に定義される表面酸素量に対する以下に定義される内部酸素量の質量比（内部酸素量／表面酸素量の質量比）が０．８〜１．１であり、内部酸素量と表面酸素量の合計が０．４〜０．６質量％であることを特徴とする窒化ホウ素粉末である。この場合において、窒化ホウ素粉末の平均アスペクト比が５〜１２であることが好ましい。
[内部酸素量の定義]
酸素／窒素同時分析装置を用い、試料をヘリウム雰囲気中、昇温速度４．６℃／秒で室温から３０００℃まで加熱しながら酸素量と窒素量を測定した場合、窒素が検出される間に検知された酸素量の総和。
[表面酸素量の定義]
上記測定において、窒素が検出されない間に検知された酸素量の総和。
In the present invention, the mass ratio of the internal oxygen content defined below to the surface oxygen content defined below (internal oxygen content / mass ratio of the surface oxygen content) is 0.8 to 1.1, and the internal oxygen content. And the total amount of surface oxygen is 0.4 to 0.6% by mass. In this case, the average aspect ratio of the boron nitride powder is preferably 5-12.
[Definition of internal oxygen content]
When oxygen and nitrogen were measured using a simultaneous oxygen / nitrogen analyzer and the sample was heated from room temperature to 3000 ° C. at a heating rate of 4.6 ° C./second in a helium atmosphere, nitrogen was detected. Total amount of oxygen detected.
[Definition of surface oxygen content]
In the above measurement, the total amount of oxygen detected while nitrogen was not detected.
また、本発明は、平均アスペクト比が５〜１２の窒化ホウ素粉末を、酸素を含む雰囲気下、攪拌翼を有する攪拌混合機にて、平均アスペクト比を減じない程度に混合し、表面酸素を増加させることを特徴とする窒化ホウ素粉末の製造方法である。 In the present invention, boron nitride powder having an average aspect ratio of 5 to 12 is mixed in an oxygen-containing atmosphere with a stirring mixer having a stirring blade so as not to reduce the average aspect ratio, thereby increasing surface oxygen. It is a manufacturing method of the boron nitride powder characterized by making it.
また、本発明は、平均アスペクト比が５〜１２の窒化ホウ素粉末を、１０〜１５容量％の酸素を含む雰囲気下、上羽根と下羽根の攪拌翼を有する攪拌混合機、好ましくは上羽根が２枚平羽根パドル翼で、下羽根が２枚ファウドラー型翼である攪拌混合機にて、１５００〜２０００ｒｐｍで１０〜２０分間混合し、表面酸素を増加させることを特徴とする窒化ホウ素粉末の製造方法である。 In addition, the present invention provides a stirring mixer having an upper blade and a lower blade with an average aspect ratio of 5 to 12 in an atmosphere containing oxygen of 10 to 15% by volume, preferably an upper blade. Production of boron nitride powder characterized in that the surface oxygen is increased by mixing for 10 to 20 minutes at 1500 to 2000 rpm in a stirring mixer having two flat blade paddle blades and two lower blades being a Faudler type blade. Is the method.
さらに、本発明は、上記窒化ホウ素粉末を４０質量％以上含有し、２５℃粘度が７５００ｍＰａ・ｓ以下であることを特徴とする窒化ホウ素粉末の水スラリーである。 Furthermore, the present invention is an aqueous slurry of boron nitride powder characterized by containing 40% by mass or more of the boron nitride powder and having a viscosity at 25 ° C. of 7500 mPa · s or less.
本発明によれば、２５℃粘度が７５００ｍＰａ・ｓ以下にして窒化ホウ素粉末濃度が４０質量％以上である低粘度かつ高濃度の窒化ホウ素の水スラリーを調製することができる窒化ホウ素粉末とその製造方法が提供される。また、本発明によれば、上記特性を有する低粘度かつ高濃度の窒化ホウ素の水スラリーが提供される。 According to the present invention, a boron nitride powder capable of preparing a low-viscosity and high-concentration boron nitride water slurry having a viscosity at 25 ° C. of 7500 mPa · s or less and a boron nitride powder concentration of 40% by mass or more, and its production A method is provided. In addition, according to the present invention, a low-viscosity and high-concentration boron nitride water slurry having the above characteristics is provided.
本発明の窒化ホウ素粉末は、内部酸素量／表面酸素量の質量比が０．８〜１．１である。この比が０．８未満であると、表面への酸化膜の膜厚が過剰となって、熱伝導性が損なわれる。また、この比が１．１をこえると、内部酸素が過剰であるため、フォノンによる熱伝導性が損なわれる。内部酸素量／表面酸素量の質量比が０．８〜１．１であっても、内部酸素と表面酸素の合計が０．４質量％未満であると、表面酸素量が少ないために水中での分散性が不十分となり、また０．６質量％をこえると表面への酸化膜が過剰となって、熱伝導性が損なわれる。なお、窒化ホウ素粉末の平均アスペクト比は、水への分散性の点から、５〜１２であることが好ましい。 The boron nitride powder of the present invention has an internal oxygen content / surface oxygen content mass ratio of 0.8 to 1.1. When this ratio is less than 0.8, the thickness of the oxide film on the surface becomes excessive, and the thermal conductivity is impaired. On the other hand, if this ratio exceeds 1.1, the internal oxygen is excessive, and the thermal conductivity due to phonons is impaired. Even if the mass ratio of the amount of internal oxygen / the amount of surface oxygen is 0.8 to 1.1, the total amount of internal oxygen and surface oxygen is less than 0.4% by mass. Insufficient dispersibility, and if it exceeds 0.6% by mass, the oxide film on the surface becomes excessive and the thermal conductivity is impaired. In addition, it is preferable that the average aspect-ratio of boron nitride powder is 5-12 from the point of the dispersibility to water.
本明細書において、内部酸素量及び表面酸素量は以下のように定義される。酸素／窒素同時分析装置として、堀場製作所社製「酸素・窒素同時分析計 ＥＭＧＡ−６４０W」を用いた。
[内部酸素量の定義]
酸素／窒素同時分析装置を用い、試料をヘリウム雰囲気中、昇温速度４．６℃／秒で室温から３０００℃まで加熱しながら酸素量と窒素量を測定した場合、窒素が検出される間に検知された酸素量の総和。
[表面酸素量の定義]
上記測定において、窒素が検出されない間に検知された酸素量の総和。
In this specification, the amount of internal oxygen and the amount of surface oxygen are defined as follows. As an oxygen / nitrogen simultaneous analyzer, “Oxygen / nitrogen simultaneous analyzer EMGA-640W” manufactured by HORIBA, Ltd. was used.
[Definition of internal oxygen content]
When oxygen and nitrogen were measured using a simultaneous oxygen / nitrogen analyzer and the sample was heated from room temperature to 3000 ° C. at a heating rate of 4.6 ° C./second in a helium atmosphere, nitrogen was detected. Total amount of oxygen detected.
[Definition of surface oxygen content]
In the above measurement, the total amount of oxygen detected while nitrogen was not detected.
本発明の窒化ホウ素粉末は、本発明の窒化ホウ素粉末の製造方法によって製造することができる。本発明の窒化ホウ素粉末の製造方法は、攪拌翼を有する攪拌混合機を用い、酸素を含む雰囲気下、窒化ホウ素粉末の平均アスペクト比を減じないようにして混合し、表面酸素を増加させることを特徴とするものである。具体的には、平均アスペクト比が５〜１２の窒化ホウ素粉末を、１０〜１５容量％の酸素を含む雰囲気下、上羽根が２枚平羽根パドル翼、下羽根が２枚ファウドラー型翼の攪拌翼を有する攪拌混合機にて、１５００〜２０００ｒｐｍで１０〜２０分間混合し、表面酸素を増加させることが好ましい。 The boron nitride powder of the present invention can be produced by the method for producing a boron nitride powder of the present invention. The method for producing boron nitride powder according to the present invention uses a stirrer / mixer having a stirring blade to increase the surface oxygen by mixing in an oxygen-containing atmosphere without reducing the average aspect ratio of the boron nitride powder. It is a feature. Specifically, a boron nitride powder having an average aspect ratio of 5 to 12 is stirred in an atmosphere containing 10 to 15% by volume of oxygen, the upper blade is two flat blade paddle blades, and the lower blade is two fiddler blades. It is preferable to increase the surface oxygen by mixing for 10 to 20 minutes at 1500 to 2000 rpm in a stirring mixer having blades.
上羽根、下羽根を例示すれば、２枚平羽根、２枚平羽根パドル翼、２枚角度付平羽根、２枚ファウドラー型翼、２枚ピッチ付平羽根、２枚湾曲羽根等（「化学工学便覧」化学工学協会１９８８年発行改訂第五版 ８９１頁〜８９６頁）であり、これらを適宜組み合わせて使用する。これらのうち、好ましい上羽根は、２枚平羽根、２枚平羽根パドル翼、２枚角度付平羽根であり、特に２枚平羽根パドル翼が好ましい。また、好ましい下羽根は、２枚ファウドラー型翼、２枚ピッチ付平羽根、２枚湾曲羽根であり、特に２枚ファウドラー型翼が好ましい。このような攪拌翼を有する攪拌混合機の一例には、ヘンシェルミキサー（カワタ社製商品名「ＳＵＰＥＲ ＭＩＸＥＲ（型式：Ｇ−１００）」がある。 Examples of upper and lower blades are: 2 flat blades, 2 flat blade paddle blades, 2 angled flat blades, 2 fowler blades, 2 pitch flat blades, 2 curved blades, etc. Engineering Handbook ”Chemical Engineering Society 1988 Revised 5th Edition, pages 891 to 896), which are used in appropriate combination. Among these, preferable upper blades are two flat blades, two flat blade paddle blades, and two flat blades with an angle, and particularly preferably two flat blade paddle blades. Further, the preferred lower blade is a two-fouler type blade, a two-blade flat blade, and a two-curved blade, and particularly preferably a two-fouler blade. An example of a stirring mixer having such a stirring blade is a Henschel mixer (trade name “SUPER MIXER (model: G-100) manufactured by Kawata Corporation)”.
原料の窒化ホウ素粉末の平均アスペクト比を５〜１２にしたのは、この範囲にある窒化ホウ素粉末であれば、攪拌翼を有する攪拌混合機で混合した際、平均アスペクト比が減じることがあっても、それが著しく少なくして表面酸素を増加させることができるからである。しかも、得られた窒化ホウ素粉末の水への分散性が良好となるからである。なお、原料の窒化ホウ素粉末の内部酸素量と表面酸素は、いずれも０．１５〜０．３０質量％であることが好ましい。 The average aspect ratio of the raw material boron nitride powder was set to 5 to 12 if the boron nitride powder is in this range, the average aspect ratio may be reduced when mixed with a stirring mixer having a stirring blade. This is because it can significantly reduce the surface oxygen. Moreover, the dispersibility of the obtained boron nitride powder in water is improved. In addition, it is preferable that both the amount of internal oxygen and surface oxygen of the raw material boron nitride powder are 0.15 to 0.30 mass%.
窒化ホウ素粉末の表面酸素を増やすために、攪拌混合は酸素を含む雰囲気で行われる。好ましくは、酸素が１０〜１５容量％で、残部が非酸化不活性ガス、好ましくは窒素である雰囲気下で行われる。このような雰囲気であれば、内部酸素／表面酸素の質量比が０．８〜１．１である窒化ホウ素粉末を容易に製造することができる。表面酸素量の調整は、窒化ホウ素粉末の攪拌混合機への投入量、回転数、撹拌時間、雰囲気の酸素濃度などによって行うことができる。 In order to increase the surface oxygen of the boron nitride powder, stirring and mixing are performed in an atmosphere containing oxygen. Preferably, it is carried out in an atmosphere with 10-15% oxygen by volume and the balance being a non-oxidizing inert gas, preferably nitrogen. In such an atmosphere, a boron nitride powder having an internal oxygen / surface oxygen mass ratio of 0.8 to 1.1 can be easily produced. The surface oxygen amount can be adjusted by adjusting the amount of boron nitride powder charged into the stirring mixer, the number of rotations, the stirring time, the oxygen concentration in the atmosphere, and the like.
従来、アトライターミルなどの媒体撹拌式粉砕機を用い、窒化ホウ素粉末を大気中で粉砕することが提案されているが（特開平１０−１９４７１１号公報）、この方法では窒化ホウ素粒子が劈開してしまうので、内部酸素量／表面酸素量の質量比が０．８未満となり、水への分散性が悪化する。そのため、窒化ホウ素粉末を４０質量％以上含有する水スラリーの２５℃粘度を、７５００ｍＰａ・ｓ以下にすることができなかった。たとえば、１４６００ｍＰａ・ｓ程度であった。 Conventionally, it has been proposed to pulverize boron nitride powder in the atmosphere using a medium stirring pulverizer such as an attritor mill (Japanese Patent Laid-Open No. 10-194711). However, in this method, boron nitride particles are cleaved. Therefore, the mass ratio of the amount of internal oxygen / the amount of surface oxygen becomes less than 0.8, and the dispersibility in water deteriorates. Therefore, the 25 degreeC viscosity of the water slurry containing 40 mass% or more of boron nitride powders could not be made 7500 mPa · s or less. For example, it was about 14600 mPa · s.
本発明の水スラリーは、本発明の窒化ホウ素粉末を４０質量％以上含有させたものであって、２５℃における粘度が７５００ｍＰａ・ｓ以下であり、条件を選べば１０００〜７５００ｍＰａ・ｓにもなる。このような水スラリーは、従来にない低粘度かつ高濃度である。 The water slurry of the present invention contains 40% by mass or more of the boron nitride powder of the present invention, has a viscosity at 25 ° C. of 7500 mPa · s or less, and can be 1000 to 7500 mPa · s if conditions are selected. . Such a water slurry has an unprecedented low viscosity and high concentration.
水スラリーは、本発明の窒化ホウ素粉末と水を、例えばパドル型撹拌混合機（例えば新東科学社製商品名「スリーワンモータ（型式：ＢＬ１０００）」）を用い、回転数５００〜６００ｒｐｍで２〜３分間混合することによって調製することができる。 The water slurry is obtained by mixing the boron nitride powder of the present invention and water with a paddle type stirring mixer (for example, trade name “three one motor (model: BL1000)” manufactured by Shinto Kagaku Co., Ltd.) at a rotational speed of 500 to 600 rpm. It can be prepared by mixing for 3 minutes.
実施例１
窒化ホウ素粉末原料として市販品（電気化学工業社製商品名「デンカボロンナイトライド グレード名ＳＧＰ」）を用いた。この窒化ホウ素粉末は、内部酸素量が０．２３質量％、表面酸素量が０．１９質量％（内部酸素量／表面酸素量の質量比が１．２、内部酸素量と表面酸素量の合計が０．４２質量％）であり、平均アスペクト比が９．７である。一方、攪拌翼を有する攪拌混合機として、市販のヘンシェルミキサー（カワタ社製商品名「ＳＵＰＥＲ ＭＩＸＥＲ（型式：Ｇ−１００）」容積１００Ｌ）を準備した。これは、上羽根が２枚平羽根パドル翼、下羽根が２枚ファウドラー型翼の攪拌翼を有する攪拌混合機である。上羽根と下羽根は、両者が重なり合わないように７ｃｍの間隔を設け、９０°ずらして攪拌棒に設置されている。
Example 1
A commercially available product (trade name “DENCABORON NITRIDE GRADE NAME SGP” manufactured by Denki Kagaku Kogyo Co., Ltd.) was used as the boron nitride powder raw material. The boron nitride powder has an internal oxygen content of 0.23% by mass and a surface oxygen content of 0.19% by mass (the internal oxygen content / mass ratio of the surface oxygen content is 1.2, the total of the internal oxygen content and the surface oxygen content). 0.42 mass%) and the average aspect ratio is 9.7. On the other hand, as a stirring mixer having a stirring blade, a commercially available Henschel mixer (trade name “SUPER MIXER (model: G-100)” volume 100 L, manufactured by Kawata Corporation) was prepared. This is a stirrer / mixer having two flat blade paddle blades for the upper blade and two fouller blades for the lower blade. The upper blades and the lower blades are placed on the stirring bar with an interval of 7 cm so that they do not overlap each other and shifted by 90 °.
窒化ホウ素粉末原料の１０ｋｇを攪拌混合機に仕込み、酸素が１３容量％、窒素が８７容量％の雰囲気下、１７４５ｒｐｍで１５．５分間撹拌混合して、平均アスペクト比を著しく減じることなく窒化ホウ素粉末の表面酸素を増加させる処理を行った。処理後の窒化ホウ素粉末の内部酸素量と表面酸素量及び平均アスペクト比を以下に従って測定した。また、処理後の窒化ホウ素粉末の４０質量％を蒸留水に分散させてなる水スラリーを調製し粘度を測定した。水スラリーの混合には、新東科学社製商品名「スリーワンモータ（型式：ＮＺ−１１００）」を用いた。 10 kg of boron nitride powder raw material is charged into a stirring mixer and stirred and mixed at 1745 rpm for 15.5 minutes in an atmosphere of 13 vol% oxygen and 87 vol% nitrogen, and the boron nitride powder is not significantly reduced in average aspect ratio. The surface oxygen was increased. The internal oxygen content, surface oxygen content and average aspect ratio of the treated boron nitride powder were measured as follows. Further, a water slurry was prepared by dispersing 40% by mass of the treated boron nitride powder in distilled water, and the viscosity was measured. The trade name “Three-One Motor (model: NZ-1100)” manufactured by Shinto Kagaku Co., Ltd. was used for mixing the water slurry.
（１）内部酸素量と表面酸素量：試料２０ｍｇを秤量し、堀場製作所社製「酸素・窒素同時分析計 ＥＭＧＡ−６４０W」を使用して測定した。
（２）平均アスペクト比：二次電子組成像を画像処理システム（日本アビオニクス社製「ＳＰＩＣＯＡ−２」）によって２値化し、３００個の粒子についてそれぞれの二次元画像により長軸及び短軸を測定し平均アスペクト比を求めた。
（３）水スラリー粘度：温度２５℃における粘度を、Ｂ型粘度計（東京計器社製ＢＨ）のＮｏ．４のスピンドルを用い、回転数１０ｒｐｍで測定した。
(1) Internal oxygen amount and surface oxygen amount: 20 mg of a sample was weighed and measured using “Oxygen / nitrogen simultaneous analyzer EMGA-640W” manufactured by Horiba, Ltd.
(2) Average aspect ratio: A secondary electron composition image is binarized by an image processing system (“SPICOA-2” manufactured by Nippon Avionics Co., Ltd.), and the major axis and minor axis of each of 300 particles are measured by respective two-dimensional images. The average aspect ratio was determined.
(3) Water slurry viscosity: Viscosity at a temperature of 25 ° C. Measurement was performed at a rotation speed of 10 rpm using a spindle No. 4.
実施例２、３
実施例１で得られた窒化ホウ素粉末の５０質量％又は７０質量％を水に分散させたこと以外は、実施例１と同様にして水スラリーを調製した。
Examples 2 and 3
A water slurry was prepared in the same manner as in Example 1 except that 50% by mass or 70% by mass of the boron nitride powder obtained in Example 1 was dispersed in water.
実施例４、５
攪拌混合の雰囲気を、酸素量が１０容量％又は１５容量％を含み、残部がいずれも窒素である雰囲気としたこと以外は、実施例１と同様にして水スラリーを調製した。
Examples 4 and 5
A water slurry was prepared in the same manner as in Example 1 except that the atmosphere of stirring and mixing was an atmosphere containing 10% by volume or 15% by volume of oxygen with the balance being nitrogen.
実施例６
攪拌混合機を、上羽根が２枚角度付平羽根、下羽根が２枚ピッチ付平羽根にしたこと以外は、実施例１と同様にして水スラリーを調製した。
Example 6
A water slurry was prepared in the same manner as in Example 1 except that the stirring blade was replaced by two flat blades with an upper blade and two flat blades with a lower blade.
実施例７、８
攪拌翼の回転数を、１５００ｒｐｍ又は２０００ｒｐｍとしたこと以外は、実施例１と同様にして水スラリーを調製した。
Examples 7 and 8
A water slurry was prepared in the same manner as in Example 1 except that the rotation speed of the stirring blade was 1500 rpm or 2000 rpm.
実施例９、１０
攪拌翼の回転時間を、１０分又は２０分としたこと以外は、実施例１と同様にして水スラリーを調製した。
Examples 9, 10
A water slurry was prepared in the same manner as in Example 1 except that the rotation time of the stirring blade was 10 minutes or 20 minutes.
比較例１〜３
撹拌混合処理を行わなかった窒化ホウ素粉末原料を用いたこと以外は、実施例１、実施例２又は実施例３と同様にして水スラリーを調製した。
Comparative Examples 1-3
A water slurry was prepared in the same manner as in Example 1, Example 2 or Example 3 except that the boron nitride powder raw material that was not subjected to the stirring and mixing treatment was used.
比較例４
攪拌混合機のかわりに媒体撹拌式粉砕機（三井鉱山社製商品名「アトライタ（型式：ＭＡ１０ＳＥ）」アトライターミル）を用いたこと以外は、実施例１と同様にして水スラリーを調製した。
Comparative Example 4
A water slurry was prepared in the same manner as in Example 1 except that a medium stirring pulverizer (trade name “Attritor (model: MA10SE)” Attritor Mill manufactured by Mitsui Mining Co., Ltd.) was used instead of the stirring mixer.
比較例５
窒化ホウ素粉末原料を分級し、平均粒子径を３μｍとした窒化ホウ素粉末原料を用いたこと以外は、実施例１と同様にして水スラリーを調製した。
Comparative Example 5
A water slurry was prepared in the same manner as in Example 1 except that the boron nitride powder raw material was classified and the boron nitride powder raw material having an average particle diameter of 3 μm was used.
比較例６
窒化ホウ素粉末原料を分級し、平均粒子径を１３μｍとした窒化ホウ素粉末原料を用いたこと以外は、実施例１と同様にして水スラリーを調製した。
Comparative Example 6
A water slurry was prepared in the same manner as in Example 1 except that the boron nitride powder raw material was classified and the boron nitride powder raw material having an average particle diameter of 13 μm was used.
比較例７
攪拌混合の雰囲気を、酸素量が８容量％を含み、残部が窒素である雰囲気としたこと以外は、実施例１と同様にして水スラリーを調製した。
Comparative Example 7
A water slurry was prepared in the same manner as in Example 1 except that the atmosphere of stirring and mixing was an atmosphere containing 8% by volume of oxygen and the balance being nitrogen.
比較例８、９
攪拌翼の回転数を、１２００ｒｐｍ又は２３００ｒｐｍとしたこと以外は、実施例１と同様にして水スラリーを調製した。
Comparative Examples 8 and 9
A water slurry was prepared in the same manner as in Example 1 except that the rotating speed of the stirring blade was 1200 rpm or 2300 rpm.
比較例１０、１１
攪拌翼の回転時間を、５分又は２５分としたこと以外は、実施例１と同様にして水スラリーを調製した。
Comparative Examples 10 and 11
A water slurry was prepared in the same manner as in Example 1 except that the rotation time of the stirring blade was 5 minutes or 25 minutes.
以上の結果を表１、表２に示す。 The above results are shown in Tables 1 and 2.
本発明の窒化ホウ素粉末は、例えばグリース、電子部品の放熱材等に使用することができる。また、本発明の窒化ホウ素粉末の水スラリーは、例えば離型剤等に使用することができる。 The boron nitride powder of the present invention can be used, for example, as grease, a heat dissipating material for electronic parts, and the like. Moreover, the water slurry of the boron nitride powder of this invention can be used for a mold release agent etc., for example.
Claims (3)
[内部酸素量の定義]
酸素／窒素同時分析装置を用い、試料をヘリウム雰囲気中、昇温速度４．６℃／秒で室温から３０００℃まで加熱しながら酸素量と窒素量を測定した場合、窒素が検出される間に検知された酸素量の総和。
[表面酸素量の定義]
上記測定において、窒素が検出されない間に検知された酸素量の総和。 Boron nitride powder having an average aspect ratio of 5 to 12 is mixed at 1500 to 2000 rpm for 10 to 20 minutes in an agitation mixer having upper and lower agitating blades in an atmosphere containing 10 to 15% by volume of oxygen. The mass ratio of the internal oxygen amount defined below to the surface oxygen amount defined below (internal oxygen amount / mass ratio of surface oxygen amount) is 0.8 to 1.1. The method for producing a boron nitride powder, wherein the total amount of internal oxygen and surface oxygen is 0.4 to 0.6% by mass.
[Definition of internal oxygen content]
When oxygen and nitrogen were measured using a simultaneous oxygen / nitrogen analyzer and the sample was heated from room temperature to 3000 ° C. at a heating rate of 4.6 ° C./second in a helium atmosphere, nitrogen was detected. Total amount of oxygen detected.
[Definition of surface oxygen content]
In the above measurement, the total amount of oxygen detected while nitrogen was not detected .
The mass ratio of the internal oxygen amount defined in claim 1 to the surface oxygen amount defined in claim 1 (internal oxygen amount / mass ratio of surface oxygen amount) is 0.8 to 1.1, and the internal oxygen amount And 40% by mass or more of boron nitride powder having an average aspect ratio of 5 to 12 and a viscosity at 25 ° C. of 7500 mPa · s or less. An aqueous slurry of boron nitride powder characterized by the following ( but no additives are used) .
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