JP2006176389A - 高配向ダイヤモンド膜及びその製造方法並びに高配向ダイヤモンド膜を備えた電子デバイス - Google Patents
高配向ダイヤモンド膜及びその製造方法並びに高配向ダイヤモンド膜を備えた電子デバイス Download PDFInfo
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- 239000010432 diamond Substances 0.000 title claims abstract description 287
- 229910003460 diamond Inorganic materials 0.000 title claims abstract description 286
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 15
- 239000013078 crystal Substances 0.000 claims abstract description 108
- 239000007789 gas Substances 0.000 claims abstract description 62
- 239000000758 substrate Substances 0.000 claims abstract description 49
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000001301 oxygen Substances 0.000 claims abstract description 9
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 9
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000010410 layer Substances 0.000 claims description 160
- 239000002245 particle Substances 0.000 claims description 21
- 125000004432 carbon atom Chemical group C* 0.000 claims description 14
- 125000004430 oxygen atom Chemical group O* 0.000 claims description 12
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 9
- 229910001882 dioxygen Inorganic materials 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 8
- 239000002344 surface layer Substances 0.000 claims description 5
- 125000004429 atom Chemical group 0.000 claims description 3
- 238000004050 hot filament vapor deposition Methods 0.000 claims description 3
- 238000007740 vapor deposition Methods 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 18
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 7
- 239000001257 hydrogen Substances 0.000 abstract description 7
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 5
- 238000000151 deposition Methods 0.000 abstract description 3
- 238000005268 plasma chemical vapour deposition Methods 0.000 abstract description 2
- 239000008246 gaseous mixture Substances 0.000 abstract 2
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 10
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- 239000010703 silicon Substances 0.000 description 10
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- 239000012535 impurity Substances 0.000 description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 229910052741 iridium Inorganic materials 0.000 description 2
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 229910052763 palladium Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 229910052594 sapphire Inorganic materials 0.000 description 2
- 239000010980 sapphire Substances 0.000 description 2
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 2
- 238000004581 coalescence Methods 0.000 description 1
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- 238000001748 luminescence spectrum Methods 0.000 description 1
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Abstract
【解決手段】 原料ガスとしてメタン及び水素の混合ガスを使用して、CVD法により、基板3上にダイヤモンド結晶を{111}セクタ成長させてダイヤモンド層1を形成する。次に、原料ガスとしてメタン、水素及び酸素の混合ガスを使用し、プラズマCVD法により、ダイヤモンド層1上にダイヤモンド結晶を{100}セクタ成長させてダイヤモンド層2を形成する。このとき、原料ガスの圧力を133hPa以上とし、原料ガスの組成を([C]−[O])/[CH3+H2+O2]が−0.2×10−2以上で且つ[O]/[C]が1.2以下になるようにし、更に、基板温度を750℃を超え1000℃未満とする。
【選択図】 図1
Description
前記第2のダイヤモンド層の表面における平均結晶粒径をDa(μm)、前記第2のダイヤモンド層と前記第1のダイヤモンド層との界面、又は前記界面が前記第2のダイヤモンド層の表面に平行でない場合は前記第1のダイヤモンド層内における前記界面に最も近く且つ前記第2のダイヤモンド層の表面に平行の断面における前記第1のダイヤモンド層の平均結晶粒径をDb(μm)とし、
前記第2のダイヤモンド層の表面から、前記第1のダイヤモンド層と前記第2のダイヤモンド層の界面までの距離をL(μm)としたとき、下記数式1により求められる粒径拡大率M(%)が50%以上であることを特徴とする。
前記第2のダイヤモンド層を形成する工程において、
前記原料ガスのガス圧を133hPa以上とし、
前記原料ガスの組成を炭素原子の量(モル)と酸素原子の量(モル)との差を全ガス分子の量(モル)で割った値が−0.2×10−2以上で
且つ酸素原子の量(モル)と炭素原子の量(モル)との比(O/C)が1.2以下になるようにし、
基板温度を750℃を超え1000℃未満とすることを特徴とする。
先ず、本発明の第1試験の結果について説明する。表面が(100)面により構成されているシリコン基板をマイクロ波CVD装置に入れ、メタンが2体積%で水素が98体積%である混合ガスを、圧力が33hPa、流量が300標準cm3/分(sccm)の条件で流しながら、基板温度を650℃にして15分間マイクロ波を照射した。このとき、マイクロ波入力パワーは略1kWであったが、基板温度を650℃に維持できるように、マイクロ波の入力パワーを微調整した。また、これと同時に、シリコン基板に、電流量は10mA/cm2になるようにして、負のバイアス電圧を印加した。これにより、シリコン基板の表面にダイヤモンド配向核を形成した。
次に、本発明の第2試験の結果について説明する。前述の第1試験結果と同様の方法及び条件で、シリコン基板上に、ダイヤモンド結晶を{111}セクタ成長させた後、このダイヤモンド層上に上記表1に示す実施例6と同じ条件でダイヤモンド結晶を{100}セクタ成長させ、更にその上に上記表1に示す実施例7と同じ条件でダイヤモンド結晶を{100}セクタ成長させ、その粒径の変化を確認した。図6は本試験の高配向ダイヤモンド膜を示すSEM(Scanning Electron Microscope:走査型電子顕微鏡)写真である(倍率350倍)。その結果、図6に示すように、シリコン基板13上に形成された1層目のダイヤモンド層11の粒径r11の平均値は約3μmであったが、2層目のダイヤモンド層12は膜厚が8μmの段階で粒径r12が8μmに拡大し(粒径拡大率約60%)、表面が平坦になった。更に、同じ条件で25μm成膜したが、粒径の拡大は鈍化した。更に、ダイヤモンド層12の上に、条件を変えて3層目のダイヤモンド層を形成したところ、再び粒径が拡大し始め、膜厚が約40μmになるまでの間に平均結晶粒径が35μmになった(粒径拡大率68%)。その後、粒径の拡大は鈍化し、最終的には、平均結晶粒径が35μmで、表面が平坦で且つ表面に非配向結晶が存在しない高配向ダイヤモンド膜が得られた。
次に、本発明の第3試験の結果について説明する。表1に示す実施例8のダイヤモンド膜について、断面観察及びカソードルミネッセンス測定を行った。図7(a)は実施例8のダイヤモンド膜の断面を示すSEM写真(倍率225倍)であり、図7(b)はそのカソードルミネッセンス像(倍率225倍)である。また、図8は横軸に波長をとり、縦軸に強度をとって、実施例8のダイヤモンド膜のカソードルミネッセンススペクトルを示す図である。図7(a)に示すように、実施例8のダイヤモンド膜は、粒径が略一定であるダイヤモンド層21上に、成長するに従い粒径が大きくなっているダイヤモンド層22が形成されていた。なお、図7(a)においては、上層のダイヤモンド層22が更に2層に分かれているように見えるが、これは観察時のチャージアップによるものであり、膜の性質が異なっているわけではない。
3;基板
4;配向結晶
5;非配向結晶
6;プラズマ
7;ダイヤモンド配向核
13;シリコン基板
Claims (12)
- {111}セクタ成長により形成された第1のダイヤモンド層と、前記第1のダイヤモンド層上に{100}セクタ成長により形成され前記第1のダイヤモンド層から遠ざかるに従い結晶粒径が大きくなる第2のダイヤモンド層と、を有し、
前記第2のダイヤモンド層の表面における平均結晶粒径をDa(μm)、前記第2のダイヤモンド層と前記第1のダイヤモンド層との界面、又は前記界面が前記第2のダイヤモンド層の表面に平行でない場合は前記第1のダイヤモンド層内における前記界面に最も近く且つ前記第2のダイヤモンド層の表面に平行の断面における前記第1のダイヤモンド層の平均結晶粒径をDb(μm)とし、
前記第2のダイヤモンド層の表面から、前記第1のダイヤモンド層と前記第2のダイヤモンド層の界面までの距離をL(μm)としたとき、下記数式により求められる粒径拡大率M(%)が50%以上であることを特徴とする高配向ダイヤモンド膜。
- 前記第1のダイヤモンド層における前記第2のダイヤモンド層側の面を含む表層部は、相互に隣接する結晶粒子のオイラー角{α,β,γ}の差{Δα,Δβ,Δγ}が、|Δα|≦1°、|Δβ|≦1°、|Δγ|≦1°であることを特徴とする請求項1に記載の高配向ダイヤモンド膜。
- 前記第2のダイヤモンド層の表面における平均結晶粒径が30μm以上であることを特徴とする請求項1又は2に記載の高配向ダイヤモンド膜。
- 前記第2のダイヤモンド層の表面における平均結晶粒径が100μm以上であることを特徴とする請求項3に記載の高配向ダイヤモンド膜。
- 前記第2のダイヤモンド層の表面は、(100)面により形成されていることを特徴とする請求項1乃至4のいずれか1項に記載の高配向ダイヤモンド膜。
- 化学気相成長法により基板上にダイヤモンド結晶を{111}セクタ成長させて第1のダイヤモンド層を形成する工程と、炭素原子を含有するガスと酸素ガスとを含む混合原料ガスを使用し、化学気相成長法により前記第1のダイヤモンド層上にダイヤモンド結晶を{100}セクタ成長させて第2のダイヤモンド層を形成する工程と、を有し、
前記第2のダイヤモンド層を形成する工程において、
前記原料ガスのガス圧を133hPa以上とし、
前記原料ガスの組成を炭素原子の量(モル)と酸素原子の量(モル)との差を全ガス分子の量(モル)で割った値が−0.2×10−2以上で
且つ酸素原子の量(モル)と炭素原子の量(モル)との比(O/C)が1.2以下になるようにし、
基板温度を750℃を超え1000℃未満とすることを特徴とする高配向ダイヤモンド膜の製造方法。 - 前記第2のダイヤモンド層を形成する工程において、前記原料ガスにおける炭素原子の量(モル)と酸素原子の量(モル)との差を全ガス分子の量(モル)で割った値が1.0×10−2以上、又は前記原料ガスにおける酸素原子の量(モル)と炭素原子の量(モル)との比(O/C)が0.5以下である場合に、前記基板温度を750℃を超え900℃以下とすることを特徴とする請求項6に記載の高配向ダイヤモンド膜の製造方法。
- 前記第2のダイヤモンド層をプラズマ気相成長法又は熱フィラメント気相成長法により形成することを特徴とする請求項6又は7に記載の高配向ダイヤモンド膜の製造方法。
- 前記第1のダイヤモンド層を形成する工程において、前記基板の表面にダイヤモンド配向核を形成した後に、酸素ガスを含まない混合原料ガスを使用し、化学気相成長法により前記基板上にダイヤモンド結晶を{111}セクタ成長させることを特徴とする請求項6乃至8のいずれか1項に記載の高配向ダイヤモンド膜の製造方法。
- 前記第2のダイヤモンド層を形成する工程において、徐々に又は段階的に前記酸素ガスの割合を増加させてダイヤモンド結晶を{100}セクタ成長させることにより第2のダイヤモンド層を形成することを特徴とする請求項6乃至9のいずれか1項に記載の高配向ダイヤモンド膜の製造方法。
- 請求項1乃至5のいずれか1項に記載の高配向ダイヤモンド膜を有することを特徴とする電子デバイス。
- トランジスタとして使用されることを特徴とする請求項11に記載の電子デバイス。
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DE602005022397D1 (de) | 2010-09-02 |
EP1662021A2 (en) | 2006-05-31 |
EP1662021B1 (en) | 2010-07-21 |
US20060112874A1 (en) | 2006-06-01 |
CN1804116A (zh) | 2006-07-19 |
JP4646752B2 (ja) | 2011-03-09 |
KR20060059820A (ko) | 2006-06-02 |
TW200630501A (en) | 2006-09-01 |
CN1804116B (zh) | 2010-06-16 |
EP1662021A3 (en) | 2006-06-07 |
KR100736281B1 (ko) | 2007-07-06 |
US7311977B2 (en) | 2007-12-25 |
TWI303670B (en) | 2008-12-01 |
ATE474941T1 (de) | 2010-08-15 |
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