JP4417913B2 - 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
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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- JP4417913B2 JP4417913B2 JP2005517892A JP2005517892A JP4417913B2 JP 4417913 B2 JP4417913 B2 JP 4417913B2 JP 2005517892 A JP2005517892 A JP 2005517892A JP 2005517892 A JP2005517892 A JP 2005517892A JP 4417913 B2 JP4417913 B2 JP 4417913B2
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- 230000003287 optical effect Effects 0.000 title claims description 43
- 238000005477 sputtering target Methods 0.000 title claims description 28
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000000463 material Substances 0.000 claims description 30
- 239000010409 thin film Substances 0.000 claims description 15
- 229910006404 SnO 2 Inorganic materials 0.000 claims description 11
- 239000002131 composite material Substances 0.000 claims description 3
- 239000010410 layer Substances 0.000 description 34
- 239000010408 film Substances 0.000 description 26
- 238000004544 sputter deposition Methods 0.000 description 24
- 239000000843 powder Substances 0.000 description 12
- 229910004298 SiO 2 Inorganic materials 0.000 description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 11
- 239000011241 protective layer Substances 0.000 description 11
- 229910052717 sulfur Inorganic materials 0.000 description 11
- 239000011593 sulfur Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
- 230000006866 deterioration Effects 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000009792 diffusion process Methods 0.000 description 8
- 238000002834 transmittance Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 230000001681 protective effect Effects 0.000 description 6
- 229910001316 Ag alloy Inorganic materials 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 238000011109 contamination Methods 0.000 description 3
- 238000000151 deposition Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000001552 radio frequency sputter deposition Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000002310 reflectometry Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 241001025261 Neoraja caerulea Species 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
- C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/547—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on sulfides or selenides or tellurides
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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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。
また、大容量化、高速記録化のため高反射率で高熱伝導特性を有する純AgまたはAg合金が反射層材に使用されるようになったが、このような反射層も保護層材であるZnS−SiO2と接するように配置されている。
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。
また、ZnS−SiO2等のセラミックスターゲットは、バルク抵抗値が高いため、直流スパッタリング装置により成膜することができず、通常高周波スパッタリング(RF)装置が使用されている。
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。
以上のようなことから、ZnSの使用すなわち硫黄成分を含有しない透明導電材料が提案されている(特許文献1、特許文献2参照)。
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。
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、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Ta2O5、Y2O3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。
また、本発明のスパッタリングターゲットは、相対密度が90%以上とすることが可能である。密度の向上は、スパッタ膜の均一性を高め、またスパッタリング時のパーティクルの発生を抑制できる効果を有する。
本発明は、このようにIn2O3とZnOとSnO2の酸化物で構成されるSnO2を主成分とする材料とすることにより、導電性を保有させることができ、これによって、直流スパッタ(DCスパッタ)によって薄膜を形成することも、選択される材料によって可能となる。
また、光学特性を調整することにより、保護膜自体の膜厚を薄くすることも可能となるため、生産性向上、基板加熱防止効果をさらに発揮できる。
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、SnO2粉、Ta2O5粉、Y2O3粉、及び4N相当で平均粒径5μm以下のZnO粉を準備し、表1及び表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、1300°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+A)、Zn/(In+Zn+Sn+A)、Sn/(In+Zn+Sn+A)、 A/(In+Zn+Sn+A))を表1及び表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、表1及び表2に示す。
スパッタ膜の透過率は、95〜98%(633nm)に達し、屈折率は2.0〜2.2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(1.0〜1.3)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、選択される成分組成によっては、DCスパッタも可能であった。
表1及び表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、特に比較例5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。この結果を、同様に表1及び表2に示す。
本発明の組成比から逸脱する比較例の成分・組成、例えば比較例1については、Sn酸化物含有量が多く、またTa酸化物含有量が少ないために、成膜速度は速いが、透過率:82%屈折率2.3及び非晶質性:2.0と悪い結果となった。
比較例3については、In酸化物量が多く、Y酸化物量が少ないために、透過率が89と悪く、非晶質性も3.1と悪い結果となった。
比較例4については、ZnOが多く、逆にSnO2が少ないために、非晶質性が劣り、成膜速度が0.4Å/secと著しく悪い結果となった。
また、特に比較例5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。
さらに、非晶質性が安定化するとともにターゲットに導電性が付与され、相対密度を90%以上の高密度化によって、材料によっては安定したDCスパッタを可能とする。そして、このDCスパッタリングの特徴である、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、Ta、Yの何れか1種又は2種の元素の酸化物を添加した材料から成り、Ta、Yの何れか1種又は2種の元素をAとしたとき、それぞれの元素比がIn/(In+Zn+Sn+A)=0.005〜0.41、Zn/(In+Zn+Sn+A)=0.03〜0.45、Sn/(In+Zn+Sn+A)=0.13〜0.82、A/(In+Zn+Sn+A)=0.08〜0.66、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形成用スパッタリングターゲット。
- Ta、Yの何れか1種又は2種の元素をAとしたとき、(Sn+A)/(In+Zn+Sn+A)=0.45〜0.92、で構成される酸化物であることを特徴とする請求項1記載の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を形成す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ことを特徴とする光情報記録媒体の製造方法。
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CN101460651B (zh) * | 2006-06-08 | 2011-04-06 | 旭硝子株式会社 | 透明导电膜及其制造方法以及用于其制造的溅射靶材 |
US7452488B2 (en) * | 2006-10-31 | 2008-11-18 | H.C. Starck Inc. | Tin oxide-based sputtering target, low resistivity, transparent conductive film, method for producing such film and composition for use therein |
JP5437919B2 (ja) * | 2010-06-04 | 2014-03-12 | 三井金属鉱業株式会社 | Itoスパッタリングターゲットおよびその製造方法 |
US9214519B2 (en) | 2011-05-10 | 2015-12-15 | Idemitsu Kosan Co., Ltd. | In2O3—SnO2—ZnO sputtering target |
JP5965338B2 (ja) | 2012-07-17 | 2016-08-03 | 出光興産株式会社 | スパッタリングターゲット、酸化物半導体薄膜及びそれらの製造方法 |
JP6284710B2 (ja) | 2012-10-18 | 2018-02-28 | 出光興産株式会社 | スパッタリングターゲット、酸化物半導体薄膜及びそれらの製造方法 |
JP6059513B2 (ja) | 2012-11-14 | 2017-01-11 | 出光興産株式会社 | スパッタリングターゲット、酸化物半導体薄膜及びそれらの製造方法 |
CN112110721B (zh) * | 2020-09-21 | 2022-07-01 | 先导薄膜材料(广东)有限公司 | 氧化铟锡钽靶材的制备方法 |
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US6042752A (en) * | 1997-02-21 | 2000-03-28 | Asahi Glass Company Ltd. | Transparent conductive film, sputtering target and transparent conductive film-bonded substrate |
US6534183B1 (en) * | 1998-08-31 | 2003-03-18 | Idemitsu Kosan Co., Ltd. | Target for transparent electroconductive film, transparent electroconductive material, transparent electroconductive glass, and transparent electroconductive film |
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US6833058B1 (en) * | 2000-10-24 | 2004-12-21 | Honeywell International Inc. | Titanium-based and zirconium-based mixed materials and sputtering targets |
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US7635440B2 (en) * | 2003-03-04 | 2009-12-22 | Nippon Mining & Metals Co., Ltd. | Sputtering target, thin film for optical information recording medium and process for producing the same |
JP4793773B2 (ja) * | 2003-03-04 | 2011-10-12 | Jx日鉱日石金属株式会社 | スパッタリングターゲットの製造方法 |
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