JP2010077012A - 酸化アルミニウム焼結体及びその製法 - Google Patents
酸化アルミニウム焼結体及びその製法 Download PDFInfo
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Abstract
【解決手段】本発明の酸化アルミニウム焼結体は、主成分である酸化アルミニウムの粒子同士の間に希土類元素とフッ素とを含む相が層状に存在するもの、又は、主成分である酸化アルミニウムの粒子同士の稜に沿って希土類元素とフッ素とを含む相が存在するものである。この酸化アルミニウム焼結体は、SEM画像を見たときに、酸化アルミニウムの粒子同士の間に希土類元素とフッ素元素とを含む相が局所的に点となって存在するのではなく、線分をなすように存在している。また、本発明の酸化アルミニウム焼結体は、室温において2kV/mmの電圧を印加して1分経過後の電流値から算出した体積抵抗率を1×1013〜1×1016Ω・cmの範囲に容易に調整することができる。
【選択図】図1
Description
原料粉末として、純度99.99%以上、平均粒径0.6μmの市販の酸化アルミニウム(Al2O3)粉末、純度99.9%以上、平均粒径10μm以下の市販のフッ化イッテルビウム(YbF3)粉末をそれぞれ、100重量部、1.25重量部の割合で秤量し、イソプロピルアルコールを溶媒とし、ナイロン製のポット、直径5mmのアルミナ玉石を用いて4時間湿式混合した。なお、原料粉末の平均粒径はレーザ回折法による。混合後、スラリーをバットに取り出し、窒素気流中110℃で16時間乾燥した。その後30メッシュの篩に通し、調合粉末とした。得られた調合粉末を、200kgf/cm2の圧力で一軸加圧成形し、直径50mm、厚さ20mm程度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。焼成はホットプレス法を用いた。焼成時のプレス圧力は100kgf/cm2、雰囲気は、室温から1600℃までは真空とし、その後、1600℃で焼成を終了するまでは1.5kgf/cm2の窒素ガスを導入した。なお、焼成は、焼成温度で2時間保持することにより終了した。このようにして、実施例1の酸化アルミニウム焼結体を得た。
(1)開気孔率、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)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。試験片形状は直径50mm×厚さ0.5〜1mmとし、主電極の直径20mm、ガード電極の内径30mm、ガード電極の外径40mm、印加電極の直径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。
(3)結晶相
回転対陰極型X線回折装置(理学電機製のRINT)により同定した。測定条件はCuK α、50kV、300mA 、2θ=10−70°とした。
(4)希土類含有量
誘導結合プラズマ(ICP)発光スペクトル分析により求めた。
(5)フッ素含有量
熱加水分解分離−イオンクロマトグラフ法により求めた(JIS R9301−3−11)。
(6)マグネシウム含有量
誘導結合プラズマ(ICP)発光スペクトル分析により求めた。
(7)強度
JIS R1601に準じて、四点曲げ試験法により測定した。
(8)アルミナ粒径
アルミナ粒径の測定は、曲げ試験後の試料破面を電子顕微鏡により観察し、線分法により算出した平均粒径に1.5を乗じたものとした。
実施例1に準じて、表1及び表2の組成及び焼成条件により実施例2〜21,比較例1〜9の酸化アルミニウム焼結体を作製し、実施例1と同様にして(1)〜(8)の項目の測定を行った。その結果を表1及び表2に示す。なお、焼成温度が1700℃の場合の焼成時の雰囲気は、室温から1600℃までは真空とし、その後、1600℃から1700℃に昇温するまでの間及び1700℃で焼成を終了するまでの間は1.5kgf/cm2の窒素ガスを導入した。また、比較例9では大気中で焼成したため、特に雰囲気制御は行っていない。
たことを示す。また、Yb3Al5O12はYb3Al5O12でピーク位置を同定したことを示すものであり、フッ素を一部含有している可能性がある。また、他の希土類−アルミニウム酸化物においても同様にフッ素を含有する可能性がある。一方、比較例5,6では、酸化アルミニウムの多面体粒子同士の間に白色の相が点在している。この白色の相は、X線回折及び化学分析によって実質的にフッ素元素を含む相ではないことがわかっている。このように、実施例の酸化アルミニウム焼結体は、比較例の酸化アルミニウム焼結体に比べて、微構造が明らかに異なることがわかる。
図5は、横軸に酸化アルミニウム100重量部に対するフッ化イッテルビウムの添加量(重量部)を取り、縦軸に室温体積抵抗率(前出の(2)参照)を取ったグラフである。フッ化イッテルビウムの添加量がゼロのプロット(2つ)が比較例であり、それ以外のプロットが実施例であるが、ここでは比較例や実施例のナンバリングは省略した。各酸化アルミニウム焼結体は実施例1に準じて作製した。図5から明らかなように、主原料の酸化アルミニウムにフッ化イッテルビウムを添加した混合物を真空又は窒素ガス雰囲気下でホットプレス焼成することによって得られた酸化アルミニウム焼結体は、室温体積抵抗率が1×1014〜1×1016Ω・cmの範囲に入ることがわかる。
Claims (13)
- 主成分である酸化アルミニウムの粒子同士の間に希土類元素とフッ素とを含む相が層状に存在する、
酸化アルミニウム焼結体。 - 主成分である酸化アルミニウムの粒子同士の稜に沿って希土類元素とフッ素とを含む相が存在する、
酸化アルミニウム焼結体。 - 室温において2kV/mmの電圧を印加して1分経過後の電流値から算出した体積抵抗率が1×1013〜1×1016Ω・cm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。 - 前記希土類元素がイットリウム、ランタン及びイッテルビウムからなる群より選ばれた少なくとも1種以上である、
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。 - 前記希土類元素の含有量は焼結体全体に対して0.1〜20重量%であり、前記フッ素の含有量は焼結体全体に対して0.05〜5重量%である、
請求項1〜4のいずれか1項に記載の酸化アルミニウム焼結体。 - 前記希土類元素とフッ素とを含む相にはマグネシウムが含まれており、該マグネシウムの含有量は焼結体全体に対して0.1重量%以上である、
請求項1〜5のいずれか1項に記載の酸化アルミニウム焼結体。 - 前記希土類元素とフッ素とを含む相にはマグネシウムが含まれており、該マグネシウムの焼結体含有量の前記希土類元素の焼結体含有量に対する重量比は0.1〜0.33である、
請求項1〜6のいずれか1項に記載の酸化アルミニウム焼結体。 - 前記酸化アルミニウムの粒径は7μm以下である、
請求項1〜7のいずれか1項に記載の酸化アルミニウム焼結体。 - 静電チャックに用いられる、
請求項1〜8のいずれか1項に記載の酸化アルミニウム焼結体。 - 主原料の酸化アルミニウムに希土類元素のフッ素化合物を添加した混合物を真空又は不活性雰囲気下でホットプレス焼成することによって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。 - 前記酸化アルミニウム100重量部に対して前記希土類元素のフッ素化合物を0.5〜10重量部の範囲で添加する、
請求項10に記載の酸化アルミニウム焼結体の製法。 - 前記混合物として、前記酸化アルミニウム100重量部に対して酸化マグネシウムを0.3重量部以上添加したものを使用する、
請求項10又は11に記載の酸化アルミニウム焼結体の製法。 - 前記混合物として、前記希土類元素のフッ化物に対する酸化マグネシウムの重量比が0.1〜0.4となるように酸化マグネシウムを添加したものを使用する、
請求項12に記載の酸化アルミニウム焼結体の製法。
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JP2012178552A (ja) * | 2011-02-04 | 2012-09-13 | Sumitomo Osaka Cement Co Ltd | 静電チャック部材 |
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JPWO2016121286A1 (ja) * | 2015-01-29 | 2017-11-09 | 京セラ株式会社 | 試料保持具 |
JP2019114685A (ja) * | 2017-12-25 | 2019-07-11 | 日本特殊陶業株式会社 | 静電チャック |
JP2021521653A (ja) * | 2018-11-08 | 2021-08-26 | ケーエスエム・コンポーネント・カンパニー・リミテッド | 静電チャック及びその製造方法 |
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JP5872998B2 (ja) * | 2012-04-26 | 2016-03-01 | 日本特殊陶業株式会社 | アルミナ焼結体、それを備える部材、および半導体製造装置 |
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