JP5057193B2 - 均質性、緻密性が高くかつ高硬度の立方晶窒化ホウ素焼結体の製造法 - Google Patents
均質性、緻密性が高くかつ高硬度の立方晶窒化ホウ素焼結体の製造法 Download PDFInfo
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- JP5057193B2 JP5057193B2 JP2011023662A JP2011023662A JP5057193B2 JP 5057193 B2 JP5057193 B2 JP 5057193B2 JP 2011023662 A JP2011023662 A JP 2011023662A JP 2011023662 A JP2011023662 A JP 2011023662A JP 5057193 B2 JP5057193 B2 JP 5057193B2
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- boron nitride
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Description
「(1) メタリン酸ナトリウムの含有割合が、立方晶窒化ホウ素原料粉末との合量に占める重量割合で0.1〜5%となるように、メタリン酸ナトリウム水溶液中に立方晶窒化ホウ素原料粉末を分散させ、立方晶窒化ホウ素原料粉末中の二次粒子を解膠した後、この分散液を乾燥して水分を除去した後成形体を作製し、次いで、該成形体を真空中で加熱して残留するメタリン酸ナトリウムを除去し、その後、該成形体を超臨界流体源とともに、5GPa以上かつ1400℃以上の高圧高温条件下で焼結することを特徴とする立方晶窒化ホウ素焼結体の製造法。
を特徴とするものである。
cBN原料粉末の前処理:
この発明では、cBN原料粉末として微粒の原料粉末を使用するが、粒径が大きくなると焼結が困難になることから、その粒径は、2μm以下であることが望ましい。
清浄化:
上記前処理で得た成形体を、例えば、固体のポリ塩化ビニリデン、ポリ塩化ビニル及びポリエチレンの1種または2種以上からなる超臨界流体源と一緒Zrカプセルに装填し、cBNの熱力学安定領域である5GPa以上かつ1400℃以上の条件(従来条件に比して、比較的低圧低温条件)で超臨界流体で清浄化しつつ焼結すると、成形体中に二次粒子が存在しないために、cBN微粒の隙間にまで超臨界流体が浸透し、cBN粒子表面が十分に活性化され、焼結助剤を添加することなく、均質でかつcBN微粒子相互が強固に結合した緻密な高硬度を有するcBN焼結体が形成される。
焼結条件:
従来のcBN焼結体の製造においては、6GPa以上かつ1700℃以上の超高圧高温条件下で焼結が行われていたが、この発明では、焼結助剤を添加することなく、しかも、従来技術に比して比較的緩和された条件、即ち、5GPa以上かつ1400℃以上(好ましくは、5〜7GPa、1400〜1900℃で焼結時間5〜30分)という、従来条件に比して、比較的低圧低温条件においても焼結を行うことができ、しかも、このような緩和された条件で焼結することによって、異常粒成長が生じることもなく、均質、緻密、微粒な焼結組織を有し、高硬度を有するcBN焼結体を得ることができる。
分散剤としてのメタリン酸ナトリウムを、表1に示す所定量、蒸留水200mlに添加し、ホットスターラーにて、回転数:150rpm,プレート温度100℃で1時間加熱・撹拌する。
焼結:
上記で得られた成形体をそれぞれ0.2g、表2に示す所定量の超臨界流体源(ポリ塩化ビニリデン)と一緒に、図1に示すZrカプセルに充填し、ベルト型超高圧発生装置にて、表3に示すcBNの熱力学安定領域である所定圧力、所定温度で焼結することにより、本発明のcBN焼結体1〜10(以下、本発明焼結体1〜10という)を製造した。
2:成形体
3:Zr箔
4:ポリ塩化ビニリデン
5:黒鉛円盤
Claims (2)
- メタリン酸ナトリウムの含有割合が、立方晶窒化ホウ素原料粉末との合量に占める重量割合で0.1〜5%となるように、メタリン酸ナトリウム水溶液中に立方晶窒化ホウ素原料粉末を分散させ、立方晶窒化ホウ素原料粉末中の二次粒子を解膠した後、この分散液を乾燥して水分を除去した後成形体を作製し、次いで、該成形体を真空中で加熱して残留するメタリン酸ナトリウムを除去し、その後、該成形体を超臨界流体源とともに、5GPa以上かつ1400℃以上の高圧高温条件下で焼結することを特徴とする立方晶窒化ホウ素焼結体の製造法。
- 上記超臨界流体源は、固体のポリ塩化ビニリデン、ポリ塩化ビニル及びポリエチレンの1種または2種以上からなることを特徴とする請求項1に記載の立方晶窒化ホウ素焼結体の製造法。
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Cited By (1)
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US9174892B2 (en) | 2010-01-19 | 2015-11-03 | Uop Llc | Process for increasing a mole ratio of methyl to phenyl |
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JP5500508B2 (ja) * | 2010-03-31 | 2014-05-21 | 三菱マテリアル株式会社 | 微粒多結晶ダイヤモンド焼結体の製造法 |
GB201311849D0 (en) | 2013-07-02 | 2013-08-14 | Element Six Ltd | Super-hard constructions and methods for making and processing same |
US10350734B1 (en) | 2015-04-21 | 2019-07-16 | Us Synthetic Corporation | Methods of forming a liquid metal embrittlement resistant superabrasive compact, and superabrasive compacts and apparatuses using the same |
US11066334B2 (en) * | 2016-06-29 | 2021-07-20 | Schlumberger Technology Corporation | Binderless cBN sintering with cubic press |
CA3170276A1 (en) * | 2018-01-23 | 2019-08-01 | Us Synthetic Corporation | Corrosion resistant bearing elements, bearing assemblies, bearing apparatuses, and motor assemblies using the same |
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US3661521A (en) * | 1970-02-13 | 1972-05-09 | Gen Electric | Refining of cubic boron nitride |
JP2590413B2 (ja) * | 1989-11-17 | 1997-03-12 | 科学技術庁無機材質研究所長 | 透光性高純度立方晶窒化ほう素焼結体の製造法 |
ES2020104A6 (es) | 1990-01-23 | 1991-07-16 | Ercros Sa | Materiales ceramicos composites para aplicaciones ingenieriles de alta temperatura y severas condiciones de choque termico y su procedimiento de fabricacion. |
JP3784464B2 (ja) * | 1996-07-10 | 2006-06-14 | 三菱化工機株式会社 | 超臨界流体を洗浄流体とする洗浄方法 |
JP3818751B2 (ja) * | 1997-09-24 | 2006-09-06 | シャープ株式会社 | 超臨界流体洗浄装置 |
JP3880201B2 (ja) * | 1998-06-19 | 2007-02-14 | 電気化学工業株式会社 | 窒化ホウ素粉末及びその製造方法 |
JP5002886B2 (ja) * | 2004-07-09 | 2012-08-15 | 住友電気工業株式会社 | 立方晶窒化ホウ素多結晶体の製造方法 |
JP4811853B2 (ja) * | 2005-09-06 | 2011-11-09 | 独立行政法人物質・材料研究機構 | 高純度立方晶窒化ホウ素焼結体の製造法 |
JP2007314380A (ja) * | 2006-05-26 | 2007-12-06 | Toray Ind Inc | セラミックス成形球体及びセラミックス球体の製造方法 |
US20090053089A1 (en) | 2007-08-20 | 2009-02-26 | Heraeus Inc. | HOMOGENEOUS GRANULATED METAL BASED and METAL-CERAMIC BASED POWDERS |
JP5239576B2 (ja) * | 2008-07-22 | 2013-07-17 | 三菱マテリアル株式会社 | 高硬度かつ高靭性を有する高純度窒化ホウ素焼結体の製造法 |
JP4983891B2 (ja) | 2009-11-05 | 2012-07-25 | カシオ計算機株式会社 | 保護板一体型表示パネルの製造方法 |
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US9174892B2 (en) | 2010-01-19 | 2015-11-03 | Uop Llc | Process for increasing a mole ratio of methyl to phenyl |
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CN102190496B (zh) | 2016-05-11 |
CN102190496A (zh) | 2011-09-21 |
EP2354110B1 (en) | 2014-06-25 |
EP2354110A2 (en) | 2011-08-10 |
EP2354110A3 (en) | 2012-11-28 |
JP2011184290A (ja) | 2011-09-22 |
US8657893B2 (en) | 2014-02-25 |
US20110192093A1 (en) | 2011-08-11 |
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