JP4494400B2 - スパッタリングターゲット及び光情報記録媒体 - Google Patents
スパッタリングターゲット及び光情報記録媒体 Download PDFInfo
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- JP4494400B2 JP4494400B2 JP2006514411A JP2006514411A JP4494400B2 JP 4494400 B2 JP4494400 B2 JP 4494400B2 JP 2006514411 A JP2006514411 A JP 2006514411A JP 2006514411 A JP2006514411 A JP 2006514411A JP 4494400 B2 JP4494400 B2 JP 4494400B2
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- 230000003287 optical effect Effects 0.000 title claims description 42
- 238000005477 sputtering target Methods 0.000 title claims description 27
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 21
- 239000010409 thin film Substances 0.000 claims description 14
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 12
- 239000010410 layer Substances 0.000 description 36
- 239000000463 material Substances 0.000 description 27
- 239000010408 film Substances 0.000 description 16
- 239000011241 protective layer Substances 0.000 description 13
- 238000005245 sintering Methods 0.000 description 13
- 230000000694 effects Effects 0.000 description 12
- 238000004544 sputter deposition Methods 0.000 description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 229910052717 sulfur Inorganic materials 0.000 description 10
- 239000011593 sulfur Substances 0.000 description 10
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000002834 transmittance Methods 0.000 description 9
- 238000009792 diffusion process Methods 0.000 description 8
- 239000000843 powder Substances 0.000 description 8
- 230000006866 deterioration Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 5
- 230000001681 protective effect Effects 0.000 description 5
- 229910001316 Ag alloy Inorganic materials 0.000 description 4
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 4
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000011109 contamination Methods 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
- 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
- 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
- 230000002542 deteriorative effect Effects 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000007496 glass forming Methods 0.000 description 1
- 238000007731 hot pressing 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
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 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
- 239000007921 spray Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
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- C03C17/245—Oxides by deposition from the vapour phase
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- C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
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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
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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
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
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- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
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- G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
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- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/26—Apparatus or processes specially adapted for the manufacture of record carriers
- G11B7/266—Sputtering or spin-coating layers
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
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- C03C2217/21—Oxides
- C03C2217/213—SiO2
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- C03C2217/00—Coatings on glass
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- C03C2217/214—Al2O3
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
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- C04B2235/6585—Oxygen containing atmosphere, e.g. with changing oxygen pressures at an oxygen percentage above that of air
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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。
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。
しかし、特許文献1〜3は、光学特性及び非晶質性が劣る領域を含む問題があった。
また、本材料系を使用することにより、繰返し書き換え特性等、光情報記録媒体の特性改善が可能となるという優れた効果を有する。特に、短波長側の透過率を向上させることができるため、青色レーザー系の相変化記録媒体用保護層材に適用できる。
Al2O3の添加は、焼結温度を低下させる効果を有する。焼結温度を下げることによって、密度を上げることができ、安定した製造が可能である。その効果を達成するためにAl2O3は10mol%以上とすることが望ましい。しかし、多量の添加は、非晶質性を悪くし、熱伝導率が大きくなり過ぎるので、Al2O3を40mol%以下とすることが望ましい。残部はY2O3であり、すなわちY2O3を10-60mol%とする。
これによって、スパッタリングターゲットの相対密度を95%以上とすることが可能となり、安定した高密度のスパッタリングターゲットを製造することができる。
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いる。成膜には、高周波スパッタリングを使用する。
本材料は、上記の通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。
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。
また、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すると共に、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。
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、この隣接する反射層への硫黄成分の拡散も無くなり、同様に反射層材が腐食劣化して、光情報記録媒体の反射率等の特性劣化を引き起こす原因が一掃されるという優れた効果を有する。
この場合、焼結前に酸化イットリウムを主成分とした酸化物粉末を、1000〜1400°Cで仮焼することが望ましい。この仮焼後、3μm以下に粉砕して焼結用の原料とする。
本発明において、特にAl2O3を添加することに大きな特徴を有する。上述したように、Al2O3を添加することによって焼結温度を低下させることができるという優れた効果を有する。
Y2O3−SiO2の2成分系では光学特性及び非晶質性等は良好であるが、場合によっては1700°C以上の高温に上げないと密度を十分に上げることができず、安定した製造が難しいという問題があった。本発明では焼結温度を1600°C以下に下げることが可能となり、高密度でかつ光学特性及び非晶質性等を満足することができるという著しい効果が得られた
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SiO2粉、Y2O3粉及びAl2O3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程度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(フロー)中、1200〜1600°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。
実施例1−4の焼結温度は、それぞれ1400°C、1550°C、1250°C、1400°Cとした。なお、焼結温度は上記の温度範囲にあれば、ほぼ同等に焼結することが可能であった。
成膜サンプルの透過率(波長405nm)%、屈折率(波長405nm)、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)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、95〜96%(405nm)に達し、屈折率は1.7〜1.9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(1.0〜1.5)を有していた。
また、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、焼結温度条件を1500〜1800°Cとし、他は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。比較例1−4の焼結温度は、それぞれ1650°C、1550°C、1750°C、1000°C(ホットプレスによる)とした。
この結果を、同様に表1に示す。
比較例2は、Y2O3とAl2O3が少なく、一方ではSiO2が多いために、バランスがとれておらず、屈折率が基準よりも低下した。
比較例3は、Y2O3が多すぎる一方で、SiO2が少ないために、バランスがとれておらず、密度が十分に上がらず、スパッタ特性が劣る結果となった。
比較例4は、屈折率が高く、密度も高いが、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。また、透過率も悪かった。
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、比較的低温での焼結が可能となり安定した製造が可能となった。また、これにより相対密度を95%以上の高密度化が達成でき、安定したRFスパッタ成膜を可能となった。そして、スパッタの制御性を容易にし、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得られ、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製造できる。
Claims (4)
- Y2O3:10-60mol%、Al2O3:10-40mol%及びSiO2:30-80mol%から成ることを特徴とするスパッタリングターゲット。
- 相対密度が95%以上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。
- 請求項1又は2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又は2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。
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