JP5180034B2 - 窒化アルミニウム焼結体、その製法及びそれを用いた静電チャック - Google Patents
窒化アルミニウム焼結体、その製法及びそれを用いた静電チャック Download PDFInfo
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Description
(a)窒化アルミニウムと、窒化アルミニウム100重量部に対して2〜10重量部の酸化ユウロピウムと、酸化ユウロピウムに対してモル比で2〜10の酸化アルミニウムと、酸化アルミニウムに対してモル比で0.05〜1.2の酸化チタンとを含み、サマリウム化合物を含まない混合粉末を調製する工程と、
(b)前記混合粉末を用いて成形体を作製する工程と、
(c)該成形体を焼成するにあたり、(1)真空又は不活性雰囲気下でホットプレス焼成を行うか、(2)真空又は不活性雰囲気下でホットプレス焼成を行ったあと焼成温度よりも高い温度でアニール処理を行う工程と、
を含むものである。
(1)調合粉末の調製
窒化アルミニウム粉末、酸化ユウロピウム粉末、酸化アルミニウム粉末及び酸化チタン粉末をそれぞれ100重量部、3.0重量部、8.7重量部、0.4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、ナイロン製玉石を用いて4時間湿式混合した。なお、酸化アルミニウムに対する酸化チタンのモル比は0.05、酸化ユウロピウムに対する酸化アルミニウムのモル比は10.0であった。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。さらに、得られた調合粉末を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、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。
(3)焼成
焼成はホットプレス法を用いた。プレス圧力は200kgf/cm2とし、ホットプレス焼成温度は1920℃とし、その温度での保持時間は4時間とした。焼成雰囲気は、室温から1000℃までは真空とし、1000℃からホットプレス焼成温度に至るまでの間及びそのホットプレス焼成温度で保持する間は、1.5kgf/cm2の窒素ガスを導入した。このようにして、実施例1の窒化アルミニウム焼結体を得た。
・Eu、Ti含有量
誘導結合プラズマ(ICP)発光スペクトル分析により定量した。
・O含有量
不活性ガス融解赤外線吸収法により定量した。
・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。
・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、主電極径20mm、ガード電極内径30mm、ガード電極外径40mm、印加電極径40mmとなるよう各電極を銀で形成した。印加電圧は500V/mmとし、電圧印加後1分時の電流を読みとり、体積抵抗率を算出した。
・活性化エネルギー(Ea)
アレニウスプロットから活性化エネルギーEaを求めた。具体的には、室温から300℃において、少なくとも2点以上、好ましくは4点程度(例えば、室温、100℃、200℃、300℃の4点)の各温度での体積抵抗率ρを測定し、その逆数(電気伝導度σ)の自然対数lnσを縦軸に、1/T(Tは絶対温度)を横軸にプロットした。それらの各点について、下記式に基づき最小二乗法を用いて傾き(Ea/k)を求め、活性化エネルギーEaを求めた。
lnσ=A−(Ea/kT)
但し、σ:電気伝導率、k:ボルツマン定数,T:絶対温度、A:定数
・熱伝導率
レーザフラッシュ法により測定した。
・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°
実施例1に準じて、表1の組成及び焼成条件により実施例2〜13,比較例1〜10の窒化アルミニウム焼結体を作製し、実施例1と同様にして上述した項目の測定を行った。その結果を表1に示す。
表1から明らかなように、実施例1〜13の窒化アルミニウム焼結体は、室温体積抵抗率が1×1012Ω・cm以下で且つ活性化エネルギー(Ea)が0.5eV以下であった。特に、実施例11〜13の窒化アルミニウム焼結体は、室温体積抵抗率が1×1011Ω・cm以下で且つ活性化エネルギー(Ea)が0.4eV以下と良好な結果であった。実施例6と実施例11は、同じ組成の焼結体であるが、前者は通常のホットプレス焼成を行ったもの、後者はホットプレス焼成とアニール処理を行ったものである。それぞれのSEM写真を図1に示す。図1から明らかなように、実施例6でも粒界相が連続しているが、実施例11の方が粒界相が更に増加している。なお、SEM写真において、薄い灰色の細かい粒は窒化チタン、真っ白に輝いて見える部分がEuAl2O4(少ない)、灰色の連続相が導電性のEuAl12O19である。但し、EuAl2O4は構成元素がEu、Al、Oからなり、XRDによるピーク位置がSrAl2O4と略一致する結晶相を表している。
Claims (5)
- (a)窒化アルミニウムと、窒化アルミニウム100重量部に対して2〜10重量部の酸化ユウロピウムと、酸化ユウロピウムに対してモル比で2〜10の酸化アルミニウムと、酸化アルミニウムに対してモル比で0.05〜1.2の酸化チタンとを含み、サマリウム化合物を含まない混合粉末を調製する工程と、
(b)前記混合粉末を用いて成形体を作製する工程と、
(c)該成形体を焼成するにあたり、(1)真空又は不活性雰囲気下、1900〜1950℃でホットプレス焼成を行うか、(2)真空又は不活性雰囲気下、1800〜1890℃でホットプレス焼成を行ったあと1900〜1920℃でアニール処理を行う工程と、
を含む窒化アルミニウム焼結体の製法。 - 前記工程(a)では、前記混合粉末を調製するにあたり、窒化アルミニウム100重量部に対して3〜5重量部の酸化ユウロピウムを使用する、
請求項1に記載の窒化アルミニウム焼結体の製法。 - 請求項1又は2に記載の窒化アルミニウム焼結体の製法により製造された窒化アルミニウム焼結体であって、
窒化アルミニウムを主成分とし、EuAl12O19と一致するピークを有する連続化した粒界相を有すると共にTiNと一致するピークを有する結晶相を有するが、Smを含む結晶相を有しない焼結体からなり、500V/mmにおける室温体積抵抗率が1×1012Ω・cm以下で且つ室温から300℃までの体積抵抗率の変化から求められる活性化エネルギー(Ea)が0.5eV以下である、
窒化アルミニウム焼結体。 - 窒化アルミニウムを主成分とし、EuAl12O19と一致するピークを有する連続化した粒界相を有すると共にTiNと一致するピークを有する結晶相を有するが、Smを含む結晶相を有しない焼結体からなり、500V/mmにおける室温体積抵抗率が1×1012Ω・cm以下で且つ室温から300℃までの体積抵抗率の変化から求められる活性化エネルギー(Ea)が0.5eV以下である、
窒化アルミニウム焼結体。 - 請求項3又は4に記載の窒化アルミニウム焼結体を用いて作製された静電チャック。
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TW098138747A TWI433826B (zh) | 2008-11-21 | 2009-11-13 | Aluminum nitride sintered body and its preparation method, and an electrostatic chuck using the same method |
EP09252626.8A EP2189431B1 (en) | 2008-11-21 | 2009-11-16 | Aluminum nitride sintered product, method for producing the same and electrostatic chuck including the same |
US12/618,901 US8022001B2 (en) | 2008-11-21 | 2009-11-16 | Aluminum nitride sintered product, method for producing the same, and electrostatic chuck including the same |
CN2009102244048A CN101734924B (zh) | 2008-11-21 | 2009-11-19 | 氮化铝烧结体、其制造方法和使用其的静电卡盘 |
KR1020090112635A KR101413250B1 (ko) | 2008-11-21 | 2009-11-20 | 질화알루미늄 소결체, 그 제법 및 그것을 이용한 정전 척 |
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