JPWO2013114967A1 - 酸化亜鉛スパッタリングターゲット及びその製造方法 - Google Patents
酸化亜鉛スパッタリングターゲット及びその製造方法 Download PDFInfo
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Abstract
Description
体積基準D50平均粒径が0.1〜1.0μmの板状酸化亜鉛粉末を用意する工程と、
前記板状酸化亜鉛粉末を、せん断力を用いた手法により配向させて配向成形体を得る工程と、
前記配向成形体を1000〜1400℃の焼成温度で焼成して、酸化亜鉛結晶粒子を配向して含んでなる酸化亜鉛焼結体を得る工程と
を含んでなる、酸化亜鉛スパッタリングターゲットの製造方法が提供される。
本発明による酸化亜鉛スパッタリングターゲットは、酸化亜鉛結晶粒子を含んで構成される酸化亜鉛焼結体からなり、スパッタ面における(100)配向度が50%以上、好ましくは75%以上、より好ましくは90%以上である。このように、酸化亜鉛結晶の(100)面をスパッタ面に沿って配向させることで、スパッタリング時におけるターゲットの割れやクラックの発生を効果的に抑制して、酸化亜鉛透明導電膜を高い生産性で製造することが可能となる。
上述したような本発明による酸化亜鉛スパッタリングターゲットは、以下のようにして製造することができる。
酸化亜鉛の原料粉末を以下の方法により作製した。硝酸亜鉛六水和物(関東化学株式会社製)を用いて、濃度0.1MのZn(NO3)2水溶液を作製した。また、水酸化ナトリウム(シグマアルドリッチ社製)を用いて、濃度0.1MのNaOH水溶液を作製した。NaOH水溶液に対し、Zn(NO3)2水溶液を体積比1:1で混合し、攪拌しながら80℃で6時間保持して、沈殿物を得た。沈殿物をイオン交換水で3回洗浄した後、乾燥することで、板状の酸化亜鉛一次粒子が凝集した球状の二次粒子を得た。図1に得られた二次粒子の電子顕微鏡画像を示す。続いて、直径2mmのZrO2製ボールを用い、エタノールを溶媒として、ボールミル粉砕処理を3時間行うことにより、図1に示される酸化亜鉛二次粒子を体積基準D50平均粒径0.6μmの板状一次粒子へと粉砕した。図2に得られた板状一次粒子の電子顕微鏡画像を示す。
スラリー粘度が45000cPとなるように分散媒の量を少なくしたこと以外は、例1と同様にしてターゲットの作製及びスパッタリングを行った。その結果、配向度は0.97に向上した。図3に酸化亜鉛焼結体断面の研磨及びエッチング後のSEM画像を示す。
図3に示されるように板状であった原料粉末の酸化亜鉛粒子が等方性の結晶粒子構造に成長したことが分かる。図4に酸化亜鉛焼結体のXRDプロファイルを示す。図4に示されるように、(100)面における回折強度ピークが突出して高く、(100)面が高度に配向されていることが分かる。5個全てのターゲットにおいて割れは発生しなかった。
焼成温度を1200℃としたこと以外は例2と同様にして、ターゲットの作製及びスパッタリングを行った。全てのターゲットで割れは発生しなかった。
焼成温度を1350℃としたこと以外は例2と同様にして、ターゲットの作製及びスパッタリングを行った。全てのターゲットで割れは発生しなかった。
例1の組成に加え、平均粒径0.4μmのα−Al2O3を2重量部添加した。その他の作製条件は例2と同様。全てのターゲットで割れは発生しなかった。なお、粒径の測定において、ZnAl2O4相と推定される、微粒(内接する円の直径が500nm以下のもの)は除いた。
市販の酸化亜鉛粉末(正同化学製、酸化亜鉛1種、体積基準D50平均粒径0.6μm)を円盤状に一軸プレス成形した後、2tf/cm2で静水圧プレスした。1300℃×5hrで焼成した結果、配向度0.02の焼結体を得た。例1と同様のスパッタリングを行った結果、全てのターゲットで割れが発生した。
例1で作製したスラリーを用い、厚さ4μmのシート状成形体を作製した。積層は行わず、650℃で20時間脱脂した後、1300℃で5時間焼成し、酸化亜鉛シート状焼結体を作製した。得られた酸化亜鉛シート状焼結体を乳鉢で粗粉砕後、ボールミルにて体積基準D50平均粒径20μmまで粉砕し、板状酸化亜鉛粉末を作製した。得られた板状酸化亜鉛粉末と例6で用いた市販の酸化亜鉛粉末を重量比1:1で混合した後、200kgf/cm2の圧力で一軸プレス成形した。得られたプレス成形体を1350℃で5時間焼成し、焼結体を作製した。得られた焼結体をターゲットとして例1と同様のスパッタリングを行った結果、5個中1個のターゲットに割れが発生した。
Claims (12)
- 酸化亜鉛結晶粒子を含んで構成される酸化亜鉛焼結体からなり、スパッタ面における(100)配向度が50%以上である、酸化亜鉛スパッタリングターゲット。
- 前記配向度が75%以上である、請求項1に記載の酸化亜鉛スパッタリングターゲット。
- 前記スパッタ面に垂直な方向の断面における前記結晶粒子のアスペクト比が2.0以下である、請求項1又は2に記載の酸化亜鉛スパッタリングターゲット。
- 前記アスペクト比が1.5以下である、請求項3に記載の酸化亜鉛スパッタリングターゲット。
- 前記酸化亜鉛結晶粒子の平均粒径が1〜50μmである、請求項1〜4のいずれか一項に記載の酸化亜鉛スパッタリングターゲット。
- 酸化亜鉛スパッタリングターゲットの製造方法であって、
体積基準D50平均粒径が0.1〜1.0μmの板状酸化亜鉛粉末を用意する工程と、
前記板状酸化亜鉛粉末を、せん断力を用いた手法により配向させて配向成形体を得る工程と、
前記配向成形体を1000〜1400℃の焼成温度で焼成して、酸化亜鉛結晶粒子を配向して含んでなる酸化亜鉛焼結体を得る工程と
を含んでなる、酸化亜鉛スパッタリングターゲットの製造方法。 - 前記せん断力を用いた手法が、テープ成形、押出し成形、及びドクターブレード法からなる群から選択される少なくとも一種である、請求項6に記載の方法。
- 前記せん断力を用いた手法が、前記板状亜鉛粉末をスラリー化し、得られたスラリーを吐出口に通して前記配向成形体をシート状に得ることにより行われる、請求項6又は7に記載の方法。
- 前記焼成に先立ち、前記シート状の配向成形体を複数枚用意して、該複数枚のシート状配向成形体を積層させて前駆積層体を得て、該前駆積層体にプレス成形を施す工程をさらに含んでなる、請求項8に記載の方法。
- 前記板状酸化亜鉛粉末を用意する工程が、亜鉛塩水溶液にアルカリ水溶液を加えて60〜95℃で2〜10時間攪拌することにより沈殿物を析出させ、該沈殿物を洗浄、乾燥及び粉砕することを含む、請求項6〜9のいずれか一項に記載の方法。
- 前記粉砕が、ボールミルを用いて1〜10時間行われる、請求項10に記載の方法。
- 請求項1〜5のいずれか一項に記載のスパッタリングターゲット又は請求項6〜11のいずれか一項に記載の方法により得られたスパッタリングターゲットを用いたスパッタリングによって得られた、酸化亜鉛透明導電膜。
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