JP2007277079A - 窒化アルミニウム焼結体およびその製造方法 - Google Patents
窒化アルミニウム焼結体およびその製造方法 Download PDFInfo
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Abstract
【解決手段】本発明に係る中空形状の窒化アルミニウム焼結体は、可視光領域における光線透過率が87%以上であることを特徴としている。このような透光性の改善された窒化アルミニウム焼結体は、通常の窒化アルミニウム焼結体を、不活性雰囲気中1300〜1400℃で1時間以上熱処理することで得られる。
【選択図】なし
Description
(1)可視光領域における光線透過率が87%以上である中空形状の窒化アルミニウム焼結体。
(3)窒化アルミニウム焼結体を、不活性雰囲気中1300〜1400℃で1時間以上熱処理することを特徴とする透光性の改善された窒化アルミニウム焼結体の製造方法。
本発明に係る窒化アルミニウム焼結体は、その可視光領域における光線透過率が87%以上、好ましくは88〜96%、さらに好ましくは90〜96%、特に好ましくは91〜96%の範囲にある。
次に本発明に係る窒化アルミニウム焼結体の製造方法について説明するが、本発明の窒化アルミニウム焼結体は、上記物性を有する限り、その製造方法は特に限定はされない。
原料焼結体は、窒化アルミニウム粉末と焼結助剤との混合物を所定形状に成形し、成形体を還元雰囲気下で焼成することにより製造される。本発明において、具体的には、上記混合物を中空形状、プレート状等に成形した後、上記焼成により所定形状の原料焼結体が製造される。これらのうちで、上記混合物を中空形状に成形した後、上記焼成により中空形状の原料焼結体を製造することが好ましい。
どのアルカリ土類系酸化物や、Y2O3、CeO2、Ho2O3、Yb2O3、Gd2O3、Nb2O3、Sm2O3、Dy2O3などの希土類系酸化物を例示することができるが、最も一般的
に使用されるものは、酸化イットリウム(Y2O3)である。また、上記焼結助剤は、必ずしも酸化物である必要はなく、例えば炭酸塩、硝酸塩、リン酸塩などであってもよい。また、焼結助剤の添加量は、窒化アルミニウム粉末100重量部当たり2重量部〜20重量部の範囲が好ましい。2重量部より少ないと窒化アルミニウム焼結体の高純度化が実現されず、光透過率や熱伝導率といった特性が低下する。さらに、20重量部を超えた場合も、添加した焼結助剤が効率的に揮散できず、光透過率や熱伝導率といった特性が低下する。
圧成形することにより、成形体を作製することができる。
脱脂は、空気中、窒素中、水素中等の任意の雰囲気で加熱することにより行うことができるが、残留炭素量の調整がし易い、窒素中で脱脂を行うことが好ましい。また、脱脂温度は、有機バインダーの種類によっても異なるが、一般には、300〜900℃、特に300〜700℃が好適である。尚、圧縮成形法のように、有機バインダーを用いずに成形を行った場合には、上記の脱脂工程は不要である。
、焼成は、還元雰囲気下で行われる。
上記還元性雰囲気を実現する方法としては、焼成用の容器内に、成形体とともにカーボン発生源を共存させる方法、焼成用の容器としてカーボン製のものを用いる方法等が挙げられるが、その中でも、得られる焼結体の熱伝導率や色ムラ等を勘案すると、成形体とカーボン発生源とを焼成用の容器内に共存させる方法が好適である。
い状態を意味し、具体的には、窒素やアルゴン等の不活性ガス雰囲気を意味する。中性雰囲気下での焼成は、例えば密閉容器内を不活性ガスに置換することにより行われる。また、密閉容器としては、窒化アルミニウム、窒化ホウ素等のセラミックスや、タングステン[W]、モリブデン[Mo]等の非炭素製の材料よりなる容器が使用され、特に、耐久性の点から窒化アルミニウム、窒化ホウ素等のセラミックス製の容器が好ましい。また、カーボン質の容器内面を、上記した非カーボン質でガスを透過しない材料で被覆したものも使用することができる。要するに、密閉容器内空間に、成形体中の残存炭素以外に炭素源を存在させない状態で焼成が行われればよい。
また、1300〜1400℃で1時間以上熱処理した後、1400℃以上に昇温して熱処理すると、1300〜1400℃での熱処理により焼結体の透光性が向上しても、その後の高温での熱処理により再び透光性が低下するため好ましくない。
10L/分、さらに好ましくは0.5〜2L/分程度である。
以下本発明を実施例により説明するが、本発明はこれら実施例に限定されるものではない。
1)光透過率
管状の窒化アルミニウム焼結体の光透過率は、窒化アルミニウム焼結体を直径10mm、厚み0.9mmの管形状に加工し、図1に示す透過率測定装置を用いて測定した。
金属不純物濃度(金属元素濃度)は、窒化アルミニウム焼結体を粉砕し粉末状にした後、硝酸及びリン酸を加え加熱分解し、島津製作所製「ICPS−1000−II」を使用して溶液のICP発光分析により定量した。
した。
原料焼結体1:透過率82%の管状の窒化アルミニウム焼結体であり、焼結体中の酸素濃度は600ppm、炭素濃度100ppm、金属不純物濃度100ppm以下のものを用いた。
上記原料焼結体1〜3を、電気炉(タングステン炉)で、窒素ガス流量1L/分で、AlN製治具にセットし、表1記載の温度にて5時間熱処理を行った。昇温速度は、10℃/分とした。得られた熱処理後の焼結体の光線透過率を表1に示す。
上記原料焼結体1〜3を、電気炉(タングステン炉)で、窒素ガス流量1L/分で、AlN製治具にセットし、表2記載の温度にて2時間熱処理を行った。昇温速度は、10℃/分とした。得られた熱処理後の焼結体の光線透過率を表2に示す。
Claims (3)
- 可視光領域における光線透過率が87%以上である中空形状の窒化アルミニウム焼結体。
- 請求項1に記載の中空形状の窒化アルミニウム焼結体からなる光源用カバー。
- 窒化アルミニウム焼結体を、不活性雰囲気中1300〜1400℃で1時間以上熱処理することを特徴とする透光性の改善された窒化アルミニウム焼結体の製造方法。
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US9216906B2 (en) * | 2013-12-25 | 2015-12-22 | National Chung Shan Institute Of Science And Technology | Method for manufacturing aluminum nitride powder |
KR102339563B1 (ko) * | 2014-06-02 | 2021-12-16 | 주식회사 미코세라믹스 | 플라즈마 화학기상증착 장치용 배플 구조물 및 이의 제조 방법 |
EP3311480B1 (en) * | 2015-06-16 | 2020-02-12 | Danfoss Editron Oy | Method and arrangement for adjusting the magnetization of a permanent magnet machine |
CN111364104A (zh) * | 2020-04-23 | 2020-07-03 | 哈尔滨科友半导体产业装备与技术研究院有限公司 | 一种氮化铝单晶生长用高纯原料的制备方法 |
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JPH10245267A (ja) * | 1997-03-06 | 1998-09-14 | Denki Kagaku Kogyo Kk | 窒化アルミニウム基板及びその用途 |
JP2001102476A (ja) * | 1999-09-30 | 2001-04-13 | Toshiba Corp | セラミックス基板およびその製造方法 |
JP2005119953A (ja) * | 2003-09-25 | 2005-05-12 | Tokuyama Corp | 窒化アルミニウム焼結体及びその製造方法 |
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JP2013212993A (ja) * | 2007-09-03 | 2013-10-17 | Tokuyama Corp | 改質窒化アルミニウム焼結体の製造方法 |
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CN101400625A (zh) | 2009-04-01 |
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WO2007105728A1 (ja) | 2007-09-20 |
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