JP5887625B1 - 円筒型スパッタリングターゲット、円筒型焼結体、円筒型成形体及びそれらの製造方法 - Google Patents
円筒型スパッタリングターゲット、円筒型焼結体、円筒型成形体及びそれらの製造方法 Download PDFInfo
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- JP5887625B1 JP5887625B1 JP2015067552A JP2015067552A JP5887625B1 JP 5887625 B1 JP5887625 B1 JP 5887625B1 JP 2015067552 A JP2015067552 A JP 2015067552A JP 2015067552 A JP2015067552 A JP 2015067552A JP 5887625 B1 JP5887625 B1 JP 5887625B1
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Abstract
Description
図1乃至4を用いて、本発明の実施形態に係る円筒型スパッタリングターゲット及び円筒型焼結体の構成を説明する。まず、図1及び2を用いて円筒型スパッタリングターゲットの概要について説明する。
図1は、本発明の実施形態に係る円筒型スパッタリングターゲットを構成する円筒型焼結体の一例を示す斜視図である。図1に示すように、円筒型スパッタリングターゲット100は、中空構造の複数の円筒型焼結体110を有する。上記複数の円筒型焼結体110は一定のスペースを介して互いに隣接して配置される。ここで、図1においては、説明の便宜上、隣接する円筒型焼結体110のスペースを大きくして図示した。
次に、本発明に係る円筒型スパッタリングターゲットの円筒型焼結体の製造方法について、図3を用いて詳細に説明する。図3は、本発明の実施形態に係る円筒型焼結体の製造方法を示すプロセスフローである。図3では、酸化インジウムスズ(ITO:Indium Tin Oxide)焼結体の製造方法を例示するが、焼結体の材料はITOに限定されず、IGZOなどのその他の酸化金属焼結体にも使用することができる。
実施例1では、円筒型ITOターゲット材(円筒型焼結体)を製造する方法について説明する。まず、原料粉末としてBET(Brunauer, Emmet and Teller’s equation)比表面積が4.0〜6.0m2/gの4Nの酸化インジウムとBET比表面積が4.0〜5.7m2/g以下の4Nの酸化スズとを準備した。ここで、BET比表面積とは、BET法で求めた表面積を表すのもである。BET法とは、窒素、アルゴン、クリプトン、酸化炭素などの気体分子を固体粒子に吸着させ、吸着した気体分子の量から固体粒子の比表面積を測定する気体吸着法である。ここでは、酸化インジウムが90質量%、酸化スズが10質量%となるように原料を秤量した。次にこれらの原料粉末を湿式のボールミルで粉砕し混合した。ここで粉砕メディアとしてジルコニアボールを使用した。混合されたスラリーはスプレードライヤによって急速乾燥造粒した。
・円筒外径(直径)=190mm
・円筒内径(直径)=159mm
・円筒軸方向長さ=280mm
・成形体密度=4.00g/cm3
・成形体の相対密度=55.9%
なお、円筒型成形体の相対密度は、円筒型成形体の寸法及び重量から算出している。
・昇温速度=300℃/時間
・高温保持温度=1560℃
・高温保持時間=20hr
・焼結時雰囲気=酸素雰囲気
・焼結時圧力=大気圧
・円筒外径(直径)=157mm
・円筒内径(直径)=131mm
・円筒軸方向長さ=230mm
・焼結体密度=7.131g/cm3
・焼結体の相対密度=99.7%
つまり、円筒型成形体は焼結工程による収縮率は80%であった。また、実施例1の複数の円筒型焼結体間の相対密度の差は0.03%であった。なお、円筒型焼結体の相対密度の評価方法はアルキメデス法を用いて密度を測定した。
・材質=Ti
・円筒外径(直径)=133mm
・円筒軸方向長さ=300mm
上記の方法で作製した円筒型スパッタリングターゲットを用いて、以下の条件で放電試験を行った。具体的には、ターゲット使用率、ノジュール発生の有無及び発生頻度評価、異常放電発生の有無及び発生頻度評価、ターゲット表面の割れ評価を行った。これらの評価は目視検査によって行った。
・アルゴンガス流量=300sccm
・チャンバ圧力=0.5Pa
・パワー密度=4.0W/cm2
・成膜温度=200℃(又は「室温」)
比較例1では、400MPaの圧力でCIPによる成形を行った。比較例1における円筒型成形体の密度は4.40g/cm3であり、成形体の相対密度は61.5%であった。上記の円筒型成形体を実施例1と同様の工程で焼結することで得られた円筒型焼結体の密度は7.107g/cm3であり、焼結体の相対密度は99.4%であった。上記の円筒型焼結体を使用した円筒型スパッタリングターゲットを使用して、上記の放電試験を行ったところ、ターゲット使用率が65%のときにノジュールおよびアーキングの発生が確認された。
比較例2では、300MPaの圧力でCIPによる成形を行った。比較例2における円筒型成形体の密度は4.30g/cm3であり、成形体の相対密度は60.1%であった。上記の円筒型成形体を実施例1と同様の工程で焼結することで得られた円筒型焼結体の密度は7.107g/cm3であり、焼結体の相対密度は99.4%であった。上記の円筒型焼結体を使用した円筒型スパッタリングターゲットを使用して、上記の放電試験を行ったところ、ターゲット使用率が65%のときにノジュールおよびアーキングの発生が確認された。
比較例3では、78.5MPaの圧力でCIPによる成形を行った。比較例3における円筒型成形体の密度は3.79g/cm3であり、成形体の相対密度は53.1%であった。上記の円筒型成形体を実施例1と同様の工程で焼結することで得られた円筒型焼結体の密度は7.121g/cm3であり、焼結体の相対密度は99.6%であった。 上記の円筒型焼結体を使用した円筒型スパッタリングターゲットを使用して、上記の放電試験を行ったところ、ターゲット使用率が65%のときにノジュールおよびアーキングの発生が確認された。
110:円筒型焼結体
120:スペース
130:円筒基材
140:ろう材
Claims (7)
- スペースを介して隣接する複数のITO又はIGZOの円筒型焼結体を有する円筒型スパッタリングターゲットにおいて、
前記円筒型焼結体の相対密度が99.7%以上99.9%以下であり、
前記隣接する複数の前記円筒型焼結体間の相対密度の差が0.1%以下であることを特徴とする円筒型スパッタリングターゲット。 - 相対密度が54.5%以上58.0%以下の円筒型成形体を焼結することで前記円筒型焼結体を形成することを特徴とする請求項1の円筒型スパッタリングターゲットの製造方法。
- 前記円筒型成形体は100MPa以上200MPa以下の冷間静水圧加圧で形成されることを特徴とする請求項2に記載の円筒型スパッタリングターゲットの製造方法。
- 円筒型スパッタリングターゲットに用いるITO又はIGZOの円筒型焼結体の製造方法であって、
相対密度が54.5%以上58.0%以下の円筒型成形体を焼結することで、相対密度が99.7%以上99.9%以下の前記円筒型焼結体を形成することを特徴とする円筒型焼結体の製造方法。 - 前記円筒型成形体は100MPa以上200MPa以下の冷間静水圧加圧で形成されることを特徴とする請求項4に記載の円筒型焼結体の製造方法。
- 円筒型スパッタリングターゲットに用いる円筒型焼結体を形成するためのITO又はIGZOの円筒型成形体であって、相対密度が54.5%以上58.0%以下であることを特徴とする円筒型成形体。
- 前記円筒型成形体は100MPa以上200MPa以下の冷間静水圧加圧で形成されることを特徴とする請求項6に記載の円筒型成形体の製造方法。
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