JP5406565B2 - 酸化アルミニウム焼結体、その製法及び半導体製造装置部材 - Google Patents
酸化アルミニウム焼結体、その製法及び半導体製造装置部材 Download PDFInfo
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Description
実施例1〜9及び比較例1〜6のアルミニウム焼結体を作製し、その評価を行った。以下にその内容を詳説する。
原料粉末は、以下のものを使用した。Al2O3粉末は、純度99.5%以上の市販粉末で、平均粒径0.6μmの粉末を使用した。酸化ユウロピウム等の酸化物粉末は、市販の純度99.9%以上で、平均粒径が2μm以下のものを使用した。AlN粉末は、不純物酸素が0.87w%で、平均粒径が1.1μmであるものを使用した。なお、原料粉末の平均粒径はレーザ回折法によって測定した値である。
各粉末を表1に示す重量部となるように秤量し、イソプロピルアルコールを溶媒とし、ポリエチレン製のポット、直径5mmのアルミナ玉石を用いて4時間湿式混合した。混合後スラリーを取り出し、窒素気流中110℃で乾燥した。その後30メッシュの篩に通し、調合粉末とした。なお、必要に応じて調合粉末を450℃で5時間以上、大気雰囲気中で熱処理し、湿式混合中に混入したカーボン成分を焼失除去した。
調合粉末を、200kgf/cm2の圧力で一軸加圧成形し、φ50mmの円盤状成形体を作製し、焼成用黒鉛モールドに収納した。成形体の厚さは表1に示すとおりである。この厚さはノギスを用いて測定した。なお、今回20mmの厚さの成形体を得るには、1体につき70〜75gの調合粉末を使用した。
焼成はホットプレス法を用いた。プレス圧力200kgf/cm2以下とし、雰囲気は、室温から通常1600℃までは真空とし、その後焼成終了まで1.5kgf/cm2の窒素ガスを導入した。焼成温度は表1に示すとおりである。焼成は、焼成温度で2時間保持することにより終了した。
得られた焼結体の厚さをノギスで測定後、各種評価用に加工し、以下の評価を行った。
(1)嵩密度
純水を媒体としたアルキメデス法により測定した。
(2)強度
JIS R1601に準じて4点曲げ試験を行い、強度を算出した。なお、表1中の数字は1桁目を四捨五入して表記した。
(3)体積抵抗率
JIS C2141に準じた方法により、大気中、室温にて測定した。試験片形状はφ50mm×0.5〜1mmとし、主電極は直径20mm、ガード電極は内径30mm、ガード電極は外径40mm、印加電極は直径40mmとなるよう各電極を銀で形成した。印加電圧は2kV/mmとし、電圧を印加して1分経過後の電流値を読み取り、その電流値から室温体積抵抗率を算出した。また、サンプルの室温体積抵抗率ρoutは、図1に示す外側部分(焼成面から深さ1mmのところから深さ2mmのところまで)の室温体積抵抗率であり、室温体積抵抗率ρinは、図1に示す内側部分(焼成面から深さ3mmのところから深さ4mmのところまで)の室温体積抵抗率である。内外比ρin/ρoutは、これらの測定値に基づいて算出した。表中の室温体積抵抗率は、ρoutの値を採用した。
(4)結晶相
結晶層はX線回折装置により同定した。測定条件はCuK α、50kV、300mA、2θ=10−70°とし、測定装置は回転対陰極型X線回折装置(理学電機製のRINT)を使用した。なお、表1中、ReAl12O19/ReAl11O18は、添加したCeやPrが固溶した構造もしくはピークが重なって分離が困難な状態を表し、ReはEu,Ce,Prなどの希土類元素を表す。
Claims (8)
- ユウロピウムと窒素とを含有し、焼結体全体にわたってX線回折プロファイルにてEuAl12O19と一致するピークを有する板状結晶が分散しており、
厚さが10mm以上であり、
焼成面から深さ1mmのところから深さ2mmのところまでの外側部分の室温体積抵抗率(ρout)に対する、焼成面から深さ3mmのところから深さ4mmのところまでの内側部分の室温体積抵抗率(ρin)の比(ρin/ρout)が1.5以下であり、
前記外側部分の室温体積抵抗率(ρout)が1×10 8 Ω・cm以上である、
酸化アルミニウム焼結体。 - 前記焼結体全体にわたってEuAlO3と一致するピークを有する結晶がみられない、請求項1に記載の酸化アルミニウム焼結体。
- 前記外側部分の室温体積抵抗率(ρout)が1×10 14 Ω・cm以下である、請求項1又は2に記載の酸化アルミニウム焼結体。
- アルミナ粉末、ユウロピウム化合物粉末及び窒化アルミニウム粉末を含む混合粉末を所定形状の成形体に成形し、該成形体を非酸化性雰囲気下、1600℃以上1800℃以下でホットプレス焼成することにより、請求項1〜3のいずれか1項に記載の酸化アルミニウム焼結体を得る、酸化アルミニウム焼結体の製法。
- 前記混合粉末はアルミナ100重量部に対してユウロピウム化合物を酸化物換算で2.7〜8重量部含む、請求項4に記載の酸化アルミニウム焼結体の製法。
- 前記混合粉末中の窒化アルミニウム粉末とユウロピウム化合物粉末の酸化ユウロピウム換算とのモル比は1.7〜2.6である、請求項4又は5に記載の酸化アルミニウム焼結体の製法。
- 前記所定形状の成形体は厚さが20mm以上の板状成形体である、請求項4〜6のいずれか1項に記載の酸化アルミニウム焼結体の製法。
- 請求項1〜3のいずれか1項に記載の酸化アルミニウム焼結体を加工してなる、半導体製造装置部材。
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WO2017057273A1 (ja) * | 2015-09-30 | 2017-04-06 | 日本碍子株式会社 | 静電チャック |
JP6546538B2 (ja) * | 2016-01-29 | 2019-07-17 | 日本特殊陶業株式会社 | 窒化アルミニウム焼結体及びその製造方法 |
KR101965895B1 (ko) | 2018-11-08 | 2019-04-04 | 주식회사 케이에스엠컴포넌트 | 정전 척 및 그 제조 방법 |
JP7312712B2 (ja) * | 2020-02-07 | 2023-07-21 | 新光電気工業株式会社 | セラミックス基板、静電チャック、静電チャックの製造方法 |
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JPS5978972A (ja) * | 1982-10-25 | 1984-05-08 | 株式会社豊田中央研究所 | アルミナ質焼結体の製造方法 |
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JPH0829975B2 (ja) * | 1993-12-24 | 1996-03-27 | 工業技術院長 | アルミナ基セラミックス焼結体 |
JPH1067560A (ja) * | 1996-03-18 | 1998-03-10 | Fuji Electric Co Ltd | 高熱伝導率セラミックスおよびその製造方法 |
JP2000272958A (ja) * | 1998-11-24 | 2000-10-03 | Ngk Spark Plug Co Ltd | スパークプラグ用絶縁体、その製造方法及びそれを用いたスパークプラグ |
JP4827110B2 (ja) * | 1999-04-26 | 2011-11-30 | 日本特殊陶業株式会社 | 高耐電圧性アルミナ基焼結体 |
JP2001322867A (ja) * | 2000-05-09 | 2001-11-20 | Matsushita Electric Ind Co Ltd | 透光性焼結体と、これを用いた発光管及び放電灯 |
JP4008230B2 (ja) | 2001-11-14 | 2007-11-14 | 住友大阪セメント株式会社 | 静電チャックの製造方法 |
JP2004022585A (ja) | 2002-06-12 | 2004-01-22 | Ngk Spark Plug Co Ltd | 静電チャック |
JP4424659B2 (ja) * | 2003-02-28 | 2010-03-03 | 日本碍子株式会社 | 窒化アルミニウム質材料および半導体製造装置用部材 |
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2009
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JP2016086080A (ja) * | 2014-10-27 | 2016-05-19 | 住友大阪セメント株式会社 | 静電チャック装置およびその製造方法 |
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