JPWO2010095681A1 - 光吸収材料及びそれを用いた光電変換素子 - Google Patents
光吸収材料及びそれを用いた光電変換素子 Download PDFInfo
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 57
- 239000011358 absorbing material Substances 0.000 title claims abstract description 29
- 239000004065 semiconductor Substances 0.000 claims abstract description 76
- 150000001875 compounds Chemical class 0.000 claims abstract description 71
- 230000031700 light absorption Effects 0.000 claims abstract description 55
- 229910052723 transition metal Inorganic materials 0.000 claims abstract description 54
- 150000003624 transition metals Chemical class 0.000 claims abstract description 49
- 239000012535 impurity Substances 0.000 claims abstract description 47
- 239000002019 doping agent Substances 0.000 claims description 38
- 239000000463 material Substances 0.000 claims description 20
- 229910052748 manganese Inorganic materials 0.000 claims description 12
- 229910052804 chromium Inorganic materials 0.000 claims description 10
- 229910052720 vanadium Inorganic materials 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 9
- 229910052742 iron Inorganic materials 0.000 claims description 9
- 229910052759 nickel Inorganic materials 0.000 claims description 9
- 229910052706 scandium Inorganic materials 0.000 claims description 9
- 229910052719 titanium Inorganic materials 0.000 claims description 9
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 5
- 238000006467 substitution reaction Methods 0.000 claims description 4
- 239000010408 film Substances 0.000 description 57
- 239000000758 substrate Substances 0.000 description 36
- 238000000034 method Methods 0.000 description 32
- 238000010521 absorption reaction Methods 0.000 description 27
- 238000004544 sputter deposition Methods 0.000 description 21
- 238000000862 absorption spectrum Methods 0.000 description 18
- 229910052594 sapphire Inorganic materials 0.000 description 17
- 239000010980 sapphire Substances 0.000 description 17
- 238000001451 molecular beam epitaxy Methods 0.000 description 14
- 239000007789 gas Substances 0.000 description 12
- 239000013078 crystal Substances 0.000 description 11
- 238000005259 measurement Methods 0.000 description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
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- 230000005284 excitation Effects 0.000 description 5
- 239000001257 hydrogen Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 230000007423 decrease Effects 0.000 description 4
- 239000007769 metal material Substances 0.000 description 4
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 4
- 230000005855 radiation Effects 0.000 description 4
- 229910052710 silicon Inorganic materials 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 229910052984 zinc sulfide Inorganic materials 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 229910021529 ammonia Inorganic materials 0.000 description 3
- 125000005842 heteroatom Chemical group 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000002096 quantum dot Substances 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 229910002601 GaN Inorganic materials 0.000 description 2
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 2
- 230000005355 Hall effect Effects 0.000 description 2
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 description 2
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- 229910045601 alloy Inorganic materials 0.000 description 2
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- 229910000530 Gallium indium arsenide Inorganic materials 0.000 description 1
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 125000004429 atom Chemical group 0.000 description 1
- 238000000089 atomic force micrograph Methods 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
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- 238000002156 mixing Methods 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
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- 238000005001 rutherford backscattering spectroscopy Methods 0.000 description 1
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- 230000008685 targeting Effects 0.000 description 1
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- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 231100000701 toxic element Toxicity 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
すなわち、本発明の光吸収材料は、Gaの一部が少なくとも1種の3d遷移金属で一定以上量置換されたGaN系化合物半導体からなり、価電子帯と伝導帯の間に1以上の不純物バンドを有し、波長領域1500nm以下、300nm以上の全波長領域における光吸収係数が1000cm−1以上であることを特徴とする。本発明の光吸収材料は、光電変換材料として好適に用いることができる。
2 n−GaN層
3 p−GaMnN層
4,5 電極
11 単結晶サファイア基板
12 p−GaN層
13 GaMnN層
14 n−GaN層
15,16 電極
20 基板ホルダー
21 基板
22 真空槽
23 液体窒素シュラウド
24 第1の蒸着源
25 第2の蒸着源
26 ガス導入ノズル
27 RHEEDスクリーン
28 ガス源
29 ヒータ
本発明の一の光吸収材料は、Gaの一部が少なくとも1種の3d遷移金属で置換されたGaN系化合物半導体からなり、価電子帯と伝導帯の間に1以上の不純物バンドを有し、波長領域1500nm以下、300nm以上の全波長領域における光吸収係数が1000cm−1以上であることを特徴とするものである。
実施例1.
(Ga1−xMnxN膜の作製)
図5に示すMBE装置を用いてGa1−xMnxN膜を作製した。この装置は、真空槽22を有し、その底壁側にはガス源28からアンモニアガスを導入するガス導入ノズル26と、第1の蒸着源24及び第2の蒸着源25とが配置されている。真空槽22の天井側にはヒータ29が配置されている。第1、第2の蒸着源内には、それぞれGaを主成分とする第1の金属材料と、Mnを主成分とする第2の金属材料が配置されている。21は基板であり(サファイア、シリコン、石英、GaNなどが使用できるがここではサファイア基板を用いる)、20は基板ホルダーである。電子線は基板表面に照射され、RHEEDスクリーン27に到達する。また、23は、冷却用の液体窒素シュラウドである。
薄膜X線回折装置(日本フィリップス製、X’part)を用いて、MBE法で作製したGaMnN膜のX線回折パターンの測定を行った。結果を図6に示す。ウルツ鉱型GaNと同様に34.5度付近に反射ピークを観測し、ウルツ鉱型であることがわかった。
光吸収スペクトルは、紫外可視分光光度計(島津製作所製、UV−3600及びSOLID Spec−3700)を用いて測定した。
図7中に示した白色光源(波長400〜750nm)を用い、Ga1−xMnxN膜の光導電性を測定した。Ga1−xMnxN膜に蒸着した一対のNi/Au電極に電圧を印加し、光照射下で電流測定をおこなった。図8は、光源の出力と電流値との関係を示すグラフである。図面中、暗時とは、白色光を照射しない状態である。また、光出力をその最大出力の25%から100%へと段階的に増加させて測定した。光源の出力が増加するとともに電流値も増加し、光強度と発生する電流との間に相関が認められた。GaNのバンドギャップは、365nmに相当し、この白色光源ではGaNは励起されないことから、この電流はGa1−xMnxNの不純物バンドの生成によるものである。
Ga1−xMnxN膜の再結合時間の測定は、時間分解光電流測定法を用いて測定した。測定方法は、Ga1−xMnxN膜に一対のNi電極を形成し、電流計を接続し、一定時間光照射した後の電流の時間変化を測定し、電流が光照射前の値に戻るまでの時間を測定し、本発明ではこの値を再結合時間と定義した。その結果、200秒であった。
(Ga1−xMnxN膜の作製)
成膜時のMnセル温度を調整することによりMn供給量を制御した以外は、実施例1と同様の方法により、Ga1−xMnxN膜を作製した。膜厚は0.4μm、xは0.05であった。
実施例1と同様の方法により、光導電性を測定した。結果を図9に示す。照射光の強度と共に、電流値が増加していることがわかる。白色光源の波長は400〜750nmであるので、GaNの価電子帯から伝導帯への直接遷移(365nm)は起きない。この電流値の増加は、400〜750nmの光をGa1−xMnxNの不純物バンドが吸収して、キャリアが生成したことによるものである。
(Ga1−x−zMnxMgzN膜の作製)
作製時にGa、Mnと同時にMgを供給した以外は、実施例2と同様の方法によりGa1−x−zMnxMgzN膜を作製した。膜厚は0.4μm、xは0.05、zは0.02であった。
図10は、光源の出力と電流値との関係を示すグラフである。その結果、光照射時に電流値が増加した。GaNのバンドギャップは、365nmに相当し、この白色光源ではGaNは励起されないことから、この電流はGa1−x−zMnxMgzNの不純物バンドによるものである。
(Ga1−xMnxN:Hy膜の作製)
Ga1−xMnxN膜を作製する際、基板温度を600℃程度の低い値に設定し、アンモニアの分解を一部抑制することで水素を残留させた以外は実施例1と同様の方法によりGa1−xMnxN:Hy膜を作製した。また、700℃以上の高い基板温度で作製し、水素が残留しなかったGa1−xMnxN膜については、水素雰囲気中でホットフィラメント法により水素分子を熱分解し、Ga1−xMnxN膜に照射することで、Ga1−xMnxN:Hyを作製した。膜厚は0.3μm、xは0.06、yは0.03であった。
光吸収スペクトルを図11に示す。Ga1−xMnxN:Hy膜は、400〜1000nmの波長域で7000cm−1以上であり、300〜1500nmの波長域で1000cm−1以上の吸収係数を有していた。また、紫外及び赤外領域でもGaNよりも大きな吸収を有する。不純物バンドによる吸収は1500〜700nm領域のブロードなピーク構造および700〜400nm領域の連続吸収構造に認められた。
(Ga1−xMnxN膜の作製)
表面粗さの異なる3種のGa1−xMnxN膜を以下の方法により作製した。
作製方法は、Ga1−xMnxN膜成長開始時に核発生密度を制御し、3次元成長を促進させた。あるいは、成長中のアンモニア供給量を低くし、3次元成長を促進させる方法を用いることもできる。
表面粗さは、デジタルインスツルメンツ社製の原子間力顕微鏡(AFM)を用い、AFM像の高さ線分析により測定した。表面粗さの異なる試料は、以下の方法により作製した。Ga1−xMnxN膜成長開始時の温度を変え、核発生密度を制御し、さらに成長中の温度を制御し3次元成長を促進させる方法である。図13の(a)、(b)、(c)はそれぞれ試料1から3のAFM写真と表面粗さの測定結果を示す。表面平均粗さは、試料1で0.2nm、試料2で0.6nm、試料3で1.0nmであった。
図14は、光源の出力と電流値との関係を示すグラフである。表面が平滑な試料1と比較して、表面平均粗さが粗い試料2および試料3で大きな光電流が発生した。これにより、表面平均粗さを大きくすることにより、変換効率をさらに向上させることが可能である。
(pin素子作製)
基板としてはサファイア、シリコン、石英、GaNなどが使用できるが、ここでは単結晶サファイア基板11上に予め形成したp−GaN層12を基板として採用し、図15の試料を作成した。基板上にはGaMnN層13とその上にn−GaN層14をMBEで製膜した。Mnの置換量は製膜時のMn供給量から推定して、xは約0.08である。製膜工法は、まずp―GaN層12の一部を金属マスクで覆い、GaMnN層13を製膜し、次にn−GaN層14を製膜した。製膜後、p−GaN層12とn−GaN層14表面の一部にInを電極15,16として形成した。
前記試料に対し、逐次的に紫外光のみ、紫外光と可視光、可視光のみの光線を照射したときに観察された光電流の変化を図16に示す。光が照射されない状態ではIn電極間に電流は流れないが、紫外光を照射すると電流が発生し、この電流は可視光を重畳して照射すると増大した。その後、紫外光の照射を止めて可視光のみを照射すると、紫外光のみ照射した場合よりも電流値は低下するが、引き続き電流が発生し続けた。
(スパッタ法による作製)
次に、スパッタ法によってGaN系化合物半導体を作製した。高周波スパッタ装置の真空槽内に基板として単結晶サファイア上に形成したp-GaN、あるいはn-GaNを設置し、これと対向してGaNターゲットを設置する。ターゲット上にはGaと置換する3d遷移金属のチップを設置した。添加量の調整は、ここではチップの個数を変化させて行った。基板を設置するホルダーの裏面には基板加熱用ヒータが設置されている。チャンバ内を一旦排気した後、Ar−N2の混合ガスを導入し、基板を所定温度に加熱した後、高周波電力を印加してプラズマを誘起し、所定時間スパッタ製膜を行った。また、スパッタ製膜に先立って、基板およびターゲットをプラズマ中で清浄化してもよい。
主なスパッタ製膜条件を下記に示す。
RFパワー:200W
基板温度 :300℃
Ar:N2混合比:2:1
製膜速度 :11nm/min
得られたGa1―xTxN膜は、3d遷移金属添加の有無に関わらず、緻密で平坦性を有し、また欠陥の少ない膜であった。スパッタ法により作製したGaN系化合物半導体膜の組成分析をラザフォード後方散乱分光法により行い、Ga1-xTxNのxを求めた。
スパッタ法で製膜した薄膜の光吸収スペクトルを測定した。図17〜図20にGaNのGaを各種の3d遷移金属で置換した試料の光吸収スペクトルの測定結果を示す。図17は3d遷移金属がVで、x=0.056の試料の光吸収スペクトルであり、3.3eVより長波長側に吸収のテールを有し、1.5eV近傍にブロードな吸収ピーク持つ。波長300〜1500nmでの吸収係数は3000cm―1以上である。
(pn接合素子の作製)
スパッタ法により、次のようにしてpn接合素子を作製した。まず、単結晶サファイア上に予め形成したp−GaNを基板として用い、この上にGaMnN層を形成した。Mn量xは0.2である。形成したGaMnN層はファンデルパウ法によりn型の電気伝導性を有することが示された。スパッタ製膜方法は、基板表面の一部を金属マスクで覆い、基板上にスパッタ膜が製膜されない非製膜部を形成した。スパッタ製膜終了後、GaMnN層の表面の一部と、非製膜部にNiを下地としてAuを蒸着してそれぞれn層電極、p層電極を形成した。
前記のpn接合素子の両電極をポテンシオスタットに接続し、−3〜+3Vのバイアス電圧を印加しながら、両極間に流れる電流を測定した。測定においては、白色光を照射しない場合と照射した場合について行った。この素子に白色光を照射すると開放端電圧として約2.0Vという高い電圧が観察された。
Claims (14)
- Gaの一部が少なくとも1種の3d遷移金属で置換されたGaN系化合物半導体からなり、価電子帯と伝導帯の間に1以上の不純物バンドを有し、波長領域1500nm以下、300nm以上の全波長領域における光吸収係数が1000cm−1以上である光吸収材料。
- 前記3d遷移金属が、Sc、Ti、V、Cr、Mn、Fe、Co、Ni、またはCuである請求項1記載の光吸収材料。
- 上記3d遷移金属がMnであり、Mn置換量xをGa1−xMnxNで表したとき、xの範囲が0.02≦x≦0.3)である請求項1に記載の光吸収材料。
- Gaの一部が少なくとも1種の3d遷移金属で置換され、かつ、アクセプタードーパント及び/又はドナードーパントがドープされてなるGaN系化合物半導体からなり、価電子帯と伝導帯の間に1以上の不純物バンドを有し、波長領域1500nm以下、300nm以上の全波長領域における光吸収係数が1000cm−1以上である光吸収材料。
- 上記アクセプタードーパントがMgであり、一般式Ga1−x−zMnxMgzN(0.02≦x≦0.3、0<z≦0.125)で表される化合物半導体からなる、請求項4に記載の光吸収材料。
- 上記ドナードーパントが水素原子であり、一般式Ga1−xMnxN:Hy(0.02≦x≦0.3、0<y<x)で表される化合物半導体からなる請求項4に記載の光吸収材料。
- 上記アクセプタードーパントとドナードーパントがそれぞれMgとHであり、一般式Ga1−x−zMnxMgzN:Hy(0.02≦x≦0.3、0<z≦0.125、y>zの場合は0<y−z<x、y≦zの場合は0<y≦z)で表される化合物半導体からなる、請求項4に記載の光吸収材料。
- 複数の化合物半導体層により少なくとも1つのpn接合又はpin接合からなる光電変換層が形成されてなる光電変換素子であって、上記複数の化合物半導体層のうち少なくとも1層は、Gaの一部が少なくとも1種の3d遷移金属で置換されたGaN系化合物半導体からなり、価電子帯と伝導帯の間に1以上の不純物バンドを有し、波長領域1500nm以下、300nm以上の全波長領域における光吸収係数が1000cm−1以上である光吸収材料を用いてなる光電変換素子。
- 上記化合物半導体が、Ga1−xMnxN(0.02≦x≦0.3)である請求項8に記載の光電変換素子。
- 複数の化合物半導体層により少なくとも1つのpn接合又はpin接合からなる光電変換層が形成されてなる光電変換素子であって、上記複数の化合物半導体層のうち少なくとも1層は、Gaの一部が少なくとも1種の3d遷移金属で置換され、かつアクセプタードーパント及び/又はドナードーパントがドープされてなるGaN系化合物半導体からなり、価電子帯と伝導帯の間に1以上の不純物バンドを有し、波長領域1500nm以下、300nm以上の全波長領域における光吸収係数が1000cm−1以上である光吸収材料を用いてなる光電変換素子
- 上記化合物半導体が、アクセプタードーパントがMgであり、一般式Ga1−x−zMnxMgzN(0.02≦x≦0.3、0<z≦0.125)で表される請求項10に記載の光電変換素子。
- 上記化合物半導体が、ドナードーパントが水素原子であり、一般式Ga1−xMnxN:Hy(0.02≦x≦0.3、0<y<x)で表される請求項10に記載の光電変換素子。
- 上記化合物半導体が、アクセプタードーパントとドナードーパントがそれぞれMgとHであり、一般式Ga1−x−zMnxMgzN:Hy(0.02≦x≦0.3、0<z≦0.125、y>zの場合は0<y−z<x、y≦zの場合は0<y≦z)で表される化合物半導体からなる、請求項10に記載の光電変換素子。
- 上記GaN系化合物半導体の表面及び/又は界面に凹凸を設けてなる請求項8から13のいずれか一つに記載の光電変換素子。
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