JP4376868B2 - 光情報記録媒体薄膜製造用スパッタリングターゲット並びに光情報記録媒体及びその製造方法 - Google Patents
光情報記録媒体薄膜製造用スパッタリングターゲット並びに光情報記録媒体及びその製造方法 Download PDFInfo
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Description
しかし、今日Blue-Rayに代表される書き換え型DVDは、さらに書き換え回数の増加、大容量化、高速記録化が強く求められている。
光情報記録媒体の書き換え回数等が劣化する原因の一つとして、保護層ZnS−SiO2に挟まれるように配置された記録層材への、ZnS−SiO2からの硫黄成分の拡散が挙げられる。
したがって、この場合も同様に、ZnS−SiO2からの硫黄成分の拡散により、純AgまたはAg合金反射層材も腐食劣化して、光情報記録媒体の反射率等の特性劣化を引き起こす要因となっていた。
上記のような問題を解決するため、保護層材に硫化物を含まない酸化物のみの材料へと置き換え、ZnS−SiO2と同等以上の光学特性、非晶質安定性を有する材料系を見出すことが急務となっていた。
ところが、この高周波スパッタリング(RF)装置は、装置自体が高価であるばかりでなく、スパッタリング効率が悪く、電力消費量が大きく、制御が複雑であり、成膜速度も遅いという多くの欠点がある。
また、成膜速度を上げるため、高電力を加えた場合、基板温度が上昇し、ポリカーボネート製基板の変形を生ずるという問題がある。
しかし、特許文献1は、光学特性及び非晶質性が劣る領域を含む問題があり、また特許文献2は、十分な成膜速度が得られず、非晶質性に劣る領域を含むという問題があった。また、特許文献3は、同様に透明導電膜に関する発明で、光情報記録媒体用薄膜を製造する課題を有しておらず、したがって、したがって光情報記録媒体用薄膜としての要件も満たしていません。
上記の課題を解決するために、本発明者らは鋭意研究を行った結果、従来の保護層材ZnS−SiO2を、下記に提示する硫化物を含まない酸化物のみの材料へと置き換え、かつZnS−SiO2と同等の光学特性及び非晶質安定性を確保し、さらに高速成膜が可能であり、光情報記録媒体の特性改善、生産性向上が可能であるとの知見を得た。
また、本材料系を使用することにより、光情報記録媒体の特性改善、生産性の大幅な向上が可能となるという優れた効果を有する。
この材料は、光学特性及び膜の非晶質性が安定しており、相変化型光記録媒体の保護層材に適しており、高周波スパッタリングによるスパッタ成膜速度も速いことが判った。
本材料系にさらにSiO2、B2O3を適量添加することにより、より非晶質性が安定し、透過率を向上させることが出来るため、書換え速度の速い相変化記録媒体や青色レーザー系の相変化記録媒体用保護層材に適する。
これにより、非晶質安定性及び光学特性(屈折率、透過率)を改善することができる。上記数値範囲を逸脱するものは、上記特性に劣る傾向がある。
上記に述べるスパッタリングターゲットを使用して、少なくとも薄膜として光情報記録媒体構造の一部を形成する光情報記録媒体を提供することができる。さらに、上記スパッタリングターゲットを使用して、少なくとも薄膜として光情報記録媒体の構造の一部を形成し、且つ記録層又は反射層と隣接して配置されている光情報記録媒体を作製することができる。
本発明のスパッタリングターゲットの密度向上は、空孔を減少させ結晶粒を微細化し、ターゲットのスパッタ面を均一かつ平滑にすることができるので、スパッタリング時のパーティクルやノジュールを低減させ、さらにターゲットライフも長くすることができるという著しい効果を有し、品質のばらつきが少なく量産性を向上させることができる。
4N相当で5μm以下のIn2O3粉、ZnO粉、SiO2粉、及び4N相当で平均粒径5μm以下のSnO2粉を準備し、表1に示す組成となるように調合して、湿式混合し、乾燥後、1100°Cで仮焼した。
さらに、この仮焼粉を平均粒径1μm相当まで湿式微粉砕した後、バインダーを添加してスプレードライヤーで造粒した。この造粒粉を冷間で加圧成形し、酸素雰囲気、1200°Cで常圧焼結し、この焼結材を機械加工でターゲット形状に仕上げた。このターゲットの構成成分、組成比(In/(In+Zn+Sn+Si)、Zn/(In+Zn+Sn+Si)、Sn/(In+Zn+Sn+Si)、Si/(In+Zn+Sn+Si))を表1に示す。
成膜サンプルの透過率(波長633nm)%、屈折率(波長633nm)、非晶質性(成膜サンプルのアニール処理(600°C×30min、Ar雰囲気)を施した、XRD(Cu−Kα、40kV、30mA)による測定における2θ=20−60°の範囲の未成膜ガラス基板に対する最大ピーク強度で表した)、さらにスパッタ方式及び成膜速度(Å/sec)の測定した結果等を、まとめて表1に示す。
スパッタ膜の透過率は、92〜98%(633nm)に達し、屈折率は1.9〜2.2であり、また特定の結晶ピークは見られず、安定した非晶質性(1.0〜1.2)を有していた。
本実施例のターゲットは、ZnSを使用していないので、硫黄の拡散・汚染による光情報記録媒体の特性劣化は生じない。また、後述する比較例に比べて、成膜サンプルの透過率、屈折率、非晶質の安定性、ターゲット密度、成膜速度がいずれも良好な値を示した。
表1に示すように、本願発明の条件とは異なる原料粉の成分及び組成比の材料、特に比較例4においてはZnS原料粉を準備し、これを実施例と同様の条件で、ターゲットを作製し、かつこのターゲットを用いてスパッタ膜を形成した。一部の材料については、DC(直流)スパッタを実施した。
この結果を、同様に表1に示す。
比較例2はIn酸化物量が少なく、またSi酸化物量が多いために、高周波スパッタによっても、成膜速度が0.3Å/secと著しく悪い結果となった。
比較例3については、In酸化物量が多いために、非晶質性が4.2と悪い結果となった。
また、特に比較例4はZnSが多く含有されており、硫黄による汚染の危険のある材料であった。
4N相当で5μm以下のIn2O3粉、ZnO粉、B2O3粉、及び4N相当で平均粒径5μm以下のSnO2粉を準備し、表2に示す組成となるように調合して、湿式混合し、乾燥後、1100°Cで仮焼した。
さらに、この仮焼粉を実施例1−3と同様にしてターゲット形状に仕上げた。このターゲットの構成成分、組成比(In/(In+Zn+Sn+B)、Zn/(In+Zn+Sn+B)、Sn/(In+Zn+Sn+B)、B/(In+Zn+Sn+B))を表2に示す。
成膜サンプルの透過率(波長633nm)%、屈折率(波長633nm)、非晶質性(成膜サンプルのアニール処理(600°C×30min、Ar雰囲気)を施した、XRD(Cu−Kα、40kV、30mA)による測定における2θ=20−60°の範囲の未成膜ガラス基板に対する最大ピーク強度で表した)、さらにスパッタ方式及び成膜速度(Å/sec)の測定した結果等を、まとめて表2に示す。
スパッタ膜の透過率は、93〜98%(633nm)に達し、屈折率は1.9〜2.1であり、また特定の結晶ピークは見られず、安定した非晶質性(1.0〜1.2)を有していた。
本実施例のターゲットは、ZnSを使用していないので、硫黄の拡散・汚染による光情報記録媒体の特性劣化は生じない。また、後述する比較例に比べて、成膜サンプルの透過率、屈折率、非晶質の安定性、ターゲット密度、成膜速度がいずれも良好な値を示した。
表2に示すように、本願発明の条件とは異なる原料粉の成分及び組成比の材料を準備し、これを実施例と同様の条件で、ターゲットを作製し、かつこのターゲットを用いてスパッタ膜を形成した。一部の材料については、DC(直流)スパッタを実施した。この結果を、同様に表2に示す。
比較例6はZn酸化物量及びSn酸化物量が少なく、またB酸化物量が多いために、高周波スパッタによっても、成膜速度が0.4Å/secと著しく悪い結果となった。
比較例7については、Zn酸化物量及びB酸化物量が少なく、Sn酸化物量が多いために、透過率:83%、屈折率2.4及び非晶質性:が3.1と悪い結果となった。
さらに、非晶質性が安定化するとともに、相対密度を90%以上の高密度化によって、安定したRFスパッタ成膜を可能とする。そして、スパッタの制御性を容易にし、成膜速度を上げ、スパッタリング効率を向上させることができるという著しい効果がある。さらにまた、成膜の際にスパッタ時に発生するパーティクル(発塵)やノジュールを低減し、品質のばらつきが少なく量産性を向上させることができ、光ディスク保護膜をもつ光記録媒体を低コストで安定して製造できるという著しい効果がある。
Claims (7)
- SnO2を主成分とするIn2O3-ZnO-SnO2系複合酸化物に、SiO2を添加した材料から成り、それぞれの元素比がIn/(In+Zn+Sn+Si)=0.01〜0.43、Zn/(In+Zn+Sn+Si)=0.02〜0.47、Sn/(In+Zn+Sn+Si)=0.19〜0.82、Si/(In+Zn+Sn+Si)=0.04〜0.50、(Sn+Si)/(In+Zn+Sn+Si)=0.45〜0.90、で構成される酸化物であることを特徴とする光情報記録媒体薄膜製造用スパッタリングターゲット。
- SnO2を主成分とするIn2O3-ZnO-SnO2系複合酸化物に、B2O3を添加した材料から成り、それぞれの元素比がIn/(In+Zn+Sn+B)=0.01〜0.41、Zn/(In+Zn+Sn+B)=0.02〜0.45、Sn/(In+Zn+Sn+B)=0.13〜0.81、B/(In+Zn+Sn+B)=0.09〜0.66、(Sn+B)/(In+Zn+Sn+B)=0.45〜0.90、で構成される酸化物であることを特徴とする光情報記録媒体薄膜製造用スパッタリングターゲット。
- 相対密度が90%以上であることを特徴とする請求項1又は2記載の光情報記録媒体薄膜製造用スパッタリングターゲット。
- 請求項1〜3のいずれか一項に記載のスパッタリングターゲットを使用して、少なくとも薄膜として光情報記録媒体構造の一部が形成されていることを特徴とする光情報記録媒体。
- 請求項1〜3のいずれか一項に記載のスパッタリングターゲットを使用して、少なくとも薄膜として光情報記録媒体の構造の一部が形成されており、且つ記録層又は反射層と隣接して配置されていることを特徴とする光情報記録媒体。
- 請求項1〜3のいずれかに記載のスパッタリングターゲットを使用して、少なくとも薄膜として光情報記録媒体構造の一部を形成することを特徴とする光情報記録媒体の製造方法。
- 請求項1〜3のいずれか一項に記載のスパッタリングターゲットを使用して、少なくとも薄膜として光情報記録媒体構造の一部を形成することを特徴とする光情報記録媒体。
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JP2008097791A (ja) | 2006-09-11 | 2008-04-24 | Ricoh Co Ltd | 多層相変化型光記録媒体 |
JP4535080B2 (ja) | 2007-03-23 | 2010-09-01 | ソニー株式会社 | 光記録媒体およびその製造方法 |
JP5440388B2 (ja) * | 2010-05-26 | 2014-03-12 | 三菱マテリアル株式会社 | 酸化物スパッタリングターゲットおよび光記録媒体用酸化物膜 |
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KR20140027238A (ko) * | 2011-05-10 | 2014-03-06 | 이데미쓰 고산 가부시키가이샤 | In₂O₃-SnO₂-ZnO계 스퍼터링 타겟 |
CN102351528B (zh) * | 2011-09-28 | 2013-07-10 | 华南理工大学 | 硼化镧掺杂的氧化物半导体材料及其应用 |
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