JP5265710B2 - Bi−Ge−O系焼結体スパッタリングターゲット及びその製造方法並びに光記録媒体 - Google Patents
Bi−Ge−O系焼結体スパッタリングターゲット及びその製造方法並びに光記録媒体 Download PDFInfo
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- 230000003287 optical effect Effects 0.000 title claims description 29
- 238000005477 sputtering target Methods 0.000 title claims description 26
- 238000004519 manufacturing process Methods 0.000 title claims description 21
- 239000000843 powder Substances 0.000 claims description 37
- 239000002245 particle Substances 0.000 claims description 27
- 230000035939 shock Effects 0.000 claims description 23
- 238000004544 sputter deposition Methods 0.000 claims description 20
- 229910052797 bismuth Inorganic materials 0.000 claims description 14
- 229910052732 germanium Inorganic materials 0.000 claims description 13
- 239000012071 phase Substances 0.000 claims description 11
- 239000007858 starting material Substances 0.000 claims description 11
- 229910015902 Bi 2 O 3 Inorganic materials 0.000 claims description 9
- 238000005452 bending Methods 0.000 claims description 9
- 238000007731 hot pressing Methods 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- 229910005793 GeO 2 Inorganic materials 0.000 claims description 8
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000013078 crystal Substances 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 238000003746 solid phase reaction Methods 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 4
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 4
- 238000005245 sintering Methods 0.000 claims description 3
- 239000010408 film Substances 0.000 description 11
- 239000000203 mixture Substances 0.000 description 9
- 239000010409 thin film Substances 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 229910000416 bismuth oxide Inorganic materials 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 3
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005856 abnormality Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- PVADDRMAFCOOPC-UHFFFAOYSA-N oxogermanium Chemical compound [Ge]=O PVADDRMAFCOOPC-UHFFFAOYSA-N 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000007723 die pressing method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
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- 239000011812 mixed powder Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 239000013077 target material Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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Description
光ディスクは高密度化への要求に対応する為、多層化による高密度化が行われている。青色LDを用いる光ディスクにおいても同様に、高密度記録用の光記録媒体の開発が行われている。
1)ビスマス(Bi)、ゲルマニウム(Ge)、酸素(O)からなる焼結体ターゲットであって、BiとGeの原子数比が、0.57<(Bi/(Bi+Ge))<0.75であり、結晶相としてBi12GeO20、Bi4Ge3O12の2相から構成されることを特徴とするBi−Ge−O系焼結体スパッタリングターゲット
2)Bi12GeO20とBi4Ge3O12のモル比が、(Bi12GeO20/Bi4Ge3O12)<0.56であることを特徴とする上記1)記載のBi−Ge−O系焼結体スパッタリングターゲット
3)ターゲット焼結体中のBi12GeO20の最大粒径が3μm以下であることを特徴とする上記1)又は2)記載のBi−Ge−O系焼結体スパッタリングターゲット
4)ターゲットに200°C、30分の加熱後、水中急冷による熱衝撃を与えた場合の、該熱衝撃前後の平均曲げ強度低下率が50%以下であることを特徴とする上記1)〜3)のいずれか一項に記載の焼結体スパッタリングターゲット
5)上記1)〜4)のいずれか一項に記載のターゲットを用いてスパッタリングすることにより成膜した光記録媒体、を提供する。
6)GeO2粉14.3mol%及びBi2O3粉85.7mol%を混合後、固相反応させて得たBi12GeO20粉と、GeO2粉60.0mol%及びBi2O3粉40.0mol%を混合後、固相反応させて得たBi4Ge3O12粉末とを出発原料とし、ホットプレスすることにより、焼結体を作製することを特徴とするBi−Ge−O系焼結体スパッタリングターゲットの製造方法
7)Bi12GeO20粉とBi4Ge3O12粉末とを出発原料とし、BiとGeの原子数比が、0.57<(Bi/(Bi+Ge))<0.75となるように混合した後、600〜840°C、加圧力0〜400kg/cm2でホットプレスすることにより、焼結体を作製することを特徴とする上記6)記載のBi−Ge−O系焼結体スパッタリングターゲットの製造方法
8)平均粒径を1μm以下に微粉砕したBi12GeO20粉を使用することを特徴とする上記6)又は7)記載のBi−Ge−O系焼結体スパッタリングターゲットの製造方法、を提供する。
ところが、Bi12GeO20とBi4Ge3O12は熱膨張係数差が大きいため、熱衝撃に極めて弱くなり、高パワーでのスパッタリング成膜時に割れが発生するという問題が発生する。因みに、Bi12GeO20の熱膨張係数は1.39×10−5で、Bi4Ge3O12の熱膨張係数は6.00×10−6である。
また、Bi2O3とGeO2を出発原料とし、Bi12GeO20とBi4Ge3O12が共存する状態で微粉砕を行うと、Bi4Ge3O12が選択的に微粉砕されてしまい、分散系のBi12GeO20が粉砕されにくいことが判明した。
そこで、Bi12GeO20とBi4Ge3O12を出発原料とし、あらかじめBi12GeO20を微粉砕することで、耐熱衝撃性の向上を実現した。
また、割れや亀裂が原因となるパーティクルの発生が著しく減少し、安定した高品質の薄膜の作製が可能となり、記録ビットのエラー発生のない、そして高記録密度が達成できる光記録媒体の製造が可能となるという効果が得られた。
Bi12GeO20とBi4Ge3O12のモル比を(Bi12GeO20/Bi4Ge3O12)<0.56とすることが、耐熱衝撃性を向上させる上で有効である。
さらに、ターゲット焼結体中のBi12GeO20の粒径を微細化する場合に、最大粒径が3ミクロン以下、好ましくは平均粒径が1μm以下とすることがさらに有効である。上記のターゲットは、200°C、30分の加熱後、水中急冷による熱衝撃を与えた場合の、該熱衝撃前後の平均曲げ強度低下率が50%以下を達成することが可能となった。
本発明は、上記のターゲットを用いてスパッタリングすることにより成膜した光記録媒体を包含するものである。
この場合にも、平均粒径が1μm以下に微粉砕したBi12GeO20粉を使用することが有効である。
純度3N(99.9%)の酸化ビスマスと酸化ゲルマニウムの粉末を出発原料とし、予めBi12GeO20粉とBi4Ge3O12粉末を準備し、これらをそれぞれ、BiとGeの原子数比が、0.67となるように、Bi12GeO20粉16.67mol%とBi4Ge3O12粉83.33mol%を調合した後、混合し、さらに混合後の粉末をカーボン製ダイスに充填し、温度700°C、圧力250kg/cm2の条件でホットプレスを行った。
この焼結体の、X線回折測定により、Bi12GeO20、Bi4Ge3O12の2相構造であることを確認した。
次に、この焼結体の走査型電子顕微鏡観察写真を図1に示す。これにより、Bi4Ge3O12が母材(写真の灰色部分)となり、Bi12GeO20が分散系(写真の白色部分)であることを確認した。またBi12GeO20の最大粒径が3μm以下であり、平均粒径が1μm以下であることを確認した。
この結果、本願発明の実施例は、ターゲットの割れの発生がなく、生産効率を上げることができ、かつ安定して高品質の薄膜の作製が可能であり、記録ビットのエラー発生のない光記録媒体を得ることができるという優れた効果を有する良好なターゲットであった。
純度3N(99.9%)の酸化ビスマスと酸化ゲルマニウムの粉末を出発原料とし、これらをそれぞれ、BiとGeの原子数比が、0.67となるように、GeO2粉50.0mol%、Bi2O3粉50.0mol%を調合した後、混合し、さらに混合後の粉末をカーボン製ダイスに充填し、温度730°C、圧力250kg/cm2の条件でホットプレスを行った。
この焼結体のX線回折測定により、ターゲットの結晶相がBi12GeO20、Bi4Ge3O12の2相構造であることを確認した。
次に、この焼結体の走査型電子顕微鏡観察写真を図2に示す。これにより、Bi4Ge3O12が母材(写真の灰色部分)となり、Bi12GeO20が分散系(写真の白色部分)であることを確認した。またBi12GeO20の最大粒径が8μm以下、平均粒径が4μm以下であることを確認した。
次に、このターゲットを用いて、ガラス基板上に1kWで約1時間プレスパッタした後、2kWで10sスパッタ、5s停止を10回繰り返し、このスパッタサイクルの作業後、チャンバーを開放して目視により、ターゲットの異常を観察したところ、ターゲットに割れが発生していた。また、実施例に較べて、パーティクルの発生が著しく増加した。これはスパッタリング中のターゲットの割れが原因と考えられる。
Claims (8)
- ビスマス(Bi)、ゲルマニウム(Ge)、酸素(O)からなる焼結体ターゲットであって、BiとGeの原子数比が、0.57<(Bi/(Bi+Ge))<0.75であり、結晶相としてBi12GeO20、Bi4Ge3O12の2相から構成されることを特徴とするBi−Ge−O系焼結体スパッタリングターゲット。
- Bi12GeO20とBi4Ge3O12のモル比が、(Bi12GeO20/Bi4Ge3O12)<0.56であることを特徴とする請求項1記載のBi−Ge−O系焼結体スパッタリングターゲット。
- ターゲット焼結体中のBi12GeO20の最大粒径が3μm以下であることを特徴とする請求項1又は2記載のBi−Ge−O系焼結体スパッタリングターゲット。
- ターゲットに200°C、30分の加熱後、水中急冷による熱衝撃を与えた場合の、該熱衝撃前後の平均曲げ強度低下率が50%以下であることを特徴とする請求項1〜3のいずれか一項に記載の焼結体スパッタリングターゲット。
- 請求項1〜4のいずれか一項に記載のターゲットを用いてスパッタリングすることにより成膜した光記録媒体。
- GeO2粉14.3mol%及びBi2O3粉85.7mol%を混合後、固相反応させて得たBi12GeO20粉と、GeO2粉60.0mol%及びBi2O3粉40.0mol%を混合後、固相反応させて得たBi4Ge3O12粉末とを出発原料とし、ホットプレスすることにより、焼結体を作製することを特徴とするBi−Ge−O系焼結体スパッタリングターゲットの製造方法。
- Bi12GeO20粉とBi4Ge3O12粉末とを出発原料とし、BiとGeの原子数比が、0.57<(Bi/(Bi+Ge))<0.75となるように混合した後、600〜840°C、加圧力0〜400kg/cm2でホットプレスすることにより、焼結体を作製することを特徴とする請求項6記載のBi−Ge−O系焼結体スパッタリングターゲットの製造方法。
- 平均粒径が1μm以下に微粉砕したBi12GeO20粉を使用することを特徴とする請求項6又は7記載のBi−Ge−O系焼結体スパッタリングターゲットの製造方法。
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