JP2020090690A - 窒化物半導体光電極の製造方法 - Google Patents
窒化物半導体光電極の製造方法 Download PDFInfo
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- JP2020090690A JP2020090690A JP2018226249A JP2018226249A JP2020090690A JP 2020090690 A JP2020090690 A JP 2020090690A JP 2018226249 A JP2018226249 A JP 2018226249A JP 2018226249 A JP2018226249 A JP 2018226249A JP 2020090690 A JP2020090690 A JP 2020090690A
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- Prior art keywords
- nitride semiconductor
- heat treatment
- gallium nitride
- layer
- electrode
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- 239000004065 semiconductor Substances 0.000 title claims abstract description 91
- 150000004767 nitrides Chemical class 0.000 title claims abstract description 66
- 238000000034 method Methods 0.000 title claims abstract description 46
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- 229910002601 GaN Inorganic materials 0.000 claims abstract description 36
- JMASRVWKEDWRBT-UHFFFAOYSA-N Gallium nitride Chemical compound [Ga]#N JMASRVWKEDWRBT-UHFFFAOYSA-N 0.000 claims abstract description 35
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 35
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000001301 oxygen Substances 0.000 claims abstract description 34
- 229910052738 indium Inorganic materials 0.000 claims abstract description 21
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- 229910052759 nickel Inorganic materials 0.000 claims abstract description 17
- 229910000480 nickel oxide Inorganic materials 0.000 claims description 30
- 238000004519 manufacturing process Methods 0.000 claims description 21
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- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- TXEYQDLBPFQVAA-UHFFFAOYSA-N tetrafluoromethane Chemical compound FC(F)(F)F TXEYQDLBPFQVAA-UHFFFAOYSA-N 0.000 description 1
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- IBEFSUTVZWZJEL-UHFFFAOYSA-N trimethylindium Chemical compound C[In](C)C IBEFSUTVZWZJEL-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
還元反応:4H+ + 4e- → 2H2 (2)
具体的には、図3に示すように、酸化槽110は水溶液111と酸化電極112を具備している。酸化電極112は水溶液111に接している。水溶液111は例えば、水酸化ナトリウム水溶液、水酸化カリウム水溶液、塩酸である。酸化電極112は窒化物半導体や酸化チタン、アモルファスシリコンである。還元槽120は水溶液121と還元電極122を具備している。還元電極122は水溶液121に接している。水溶液121は例えば、炭酸水素カリウム水溶液、炭酸水素ナトリウム水溶液、塩化カリウム水溶液、塩化ナトリウム水溶液である。還元電極122は金属や金属化合物であり、例えば、ニッケル、鉄、金、白金、銀、銅、インジウム、チタンである。酸化槽110と還元槽120の間には、プロトン膜130が挟まれており、酸化槽110で生成したプロトンがプロトン膜130を介し、還元槽120へ拡散していく。プロトン膜130は例えば、ナフィオン(登録商標)であり、炭素−フッ素からなる疎水性テフロン骨格とスルホン酸基を持つパーフルオロ側鎖から構成されるパーフルオロカーボン材料である。酸化電極112と還元電極122は導線132で電気的に接続されており、酸化電極112から還元電極122へ電子の移動がなされている。光源140は例えば、キセノンランプ、水銀ランプ、ハロゲンランプ、疑似太陽光源、太陽光又はこれらの組み合わせである。酸化電極112を構成する材料が吸収可能な波長の光が照射される。例えば、窒化ガリウムで構成される電極では、吸収可能な波長は365nm以下の波長である。
本発明は、窒化物半導体薄膜で生成した電荷を酸素発生用助触媒に受け渡す際の価電子帯に生じる障壁を低減するため、酸素発生用助触媒を酸素雰囲気中で熱処理することにより、酸素過剰の酸化物材料とすることで、p型半導体とし、酸素発生用助触媒の価電子帯が窒化物半導体薄膜の価電子帯よりも高い準位に位置する界面を持つ窒化物半導体光電極を用いることで、光エネルギー変換効率の向上を図る。
(窒化物半導体光電極の作製)
図1に、実施例1における窒化物半導体光電極の製造工程を示す。
図2は、実施例1における窒化物半導体光電極の構成を示す断面図である。実施例1における窒化物半導体光電極は、図2に示すように、絶縁性または導電性の基板(サファイア基板)1と、基板1上に配置されたn型窒化ガリウム(n−GaN)層2と、n型窒化ガリウム層2上に配置された窒化インジウムガリウム(InGaN)層3と、窒化インジウムガリウム層3上に配置された酸素過剰の酸化ニッケル(NiO)層4とを備える。
次に、実施例1における酸化還元反応試験について説明する。ここでも、水の分解装置の構成図(図3)を用いるが、既に説明した点については詳しい説明を省略する。
実施例2では、実施例1の熱処理工程(第4工程)を200℃、30分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例3では、実施例1の熱処理工程を200℃、1時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例4では、実施例1の熱処理工程を200℃、2時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例5では、実施例1の熱処理工程を200℃、3時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例6では、実施例1の熱処理工程を200℃、4時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例7では、実施例1の熱処理工程を250℃、15分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例8では、実施例1の熱処理工程を250℃、30分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例9では、実施例1の熱処理工程を250℃、1時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例10では、実施例1の熱処理工程を250℃、2時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例11では、実施例1の熱処理工程を250℃、3時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例12では、実施例1の熱処理工程を250℃、4時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例13では、実施例1の熱処理工程を300℃、15分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例14では、実施例1の熱処理工程を300℃、30分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例15では、実施例1の熱処理工程を300℃、1時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例16では、実施例1の熱処理工程を300℃、2時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例17では、実施例1の熱処理工程を300℃、3時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例18では、実施例1の熱処理工程を300℃、4時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例19では、実施例1の熱処理工程を400℃、15分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例20では、実施例1の熱処理工程を400℃、30分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例21では、実施例1の熱処理工程を400℃、1時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例22では、実施例1の熱処理工程を400℃、2時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例23では、実施例1の熱処理工程を400℃、3時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例24では、実施例1の熱処理工程を400℃、4時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例25では、実施例1の熱処理工程を500℃、15分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例26では、実施例1の熱処理工程を500℃、30分間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例27では、実施例1の熱処理工程を500℃、1時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例28では、実施例1の熱処理工程を500℃、2時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例29では、実施例1の熱処理工程を500℃、3時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例30では、実施例1の熱処理工程を500℃、4時間とした窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例1では、実施例8の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例2では、実施例9の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例3では、実施例10の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例4では、実施例14の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例5では、実施例15の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例6では、実施例16の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例7では、実施例20の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例8では、実施例21の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
比較対象事例9では、実施例22の熱処理工程を空気雰囲気として窒化物半導体電極を作製した。その他の点においては実施例1と同様である。
実施例および比較対象例における、光照射から10時間後の酸素・水素ガスの生成量を表1に示す。各ガスの生成量は、半導体光電極の表面積で規格化して示した。どの例でも光照射時に、酸素と水素が生成されていることがわかった。
上記では幾つかの実施例について記載したが、開示の一部をなす論述および図面は例示的なものであり、限定するものであると理解すべきではない。この開示から当業者には様々な代替実施例および運用技術が明らかとなろう。
以上説明したように、本発明の実施例における窒化物半導体光電極の製造方法は、絶縁性または導電性の基板1上にn型窒化ガリウム層2を形成する第1工程と、n型窒化ガリウム層2上に窒化インジウムガリウム層3を形成する第2工程と、窒化インジウムガリウム層3上にニッケル層4を形成する第3工程と、酸素雰囲気中においてニッケル層4を熱処理する第4工程とを含む。このように、窒化インジウムガリウム半導体薄膜上にニッケルを形成した後、酸素雰囲気で熱処理し、酸素過剰の酸化ニッケルを形成した窒化物半導体光電極を製造することで、光吸収率の高い半導体薄膜に対して、正孔が移動できない障壁を生成しない酸素発生用の助触媒を形成し、光エネルギー変換効率の向上を図ることが可能となる。
2…n型窒化ガリウム層
3…窒化インジウムガリウム層
4…酸化ニッケル層(ニッケル層)
110…酸化槽
111…水溶液
112…酸化電極
120…還元槽
121…水溶液
122…還元電極
130…プロトン膜
132…導線
140…光源
Claims (5)
- 絶縁性または導電性の基板上にn型窒化ガリウム層を形成する第1工程と、
前記n型窒化ガリウム層上に窒化インジウムガリウム層を形成する第2工程と、
前記窒化インジウムガリウム層上にニッケル層を形成する第3工程と、
酸素雰囲気中において前記ニッケル層を熱処理する第4工程と
を含むことを特徴とする窒化物半導体光電極の製造方法。 - 前記第1工程および前記第2工程では、有機金属気相成長法(MOCVD)を用いることを特徴とする請求項1に記載の窒化物半導体光電極の製造方法。
- 前記第3工程では、電子ビーム(EB)蒸着法を用いることを特徴とする請求項1または2に記載の窒化物半導体光電極の製造方法。
- 前記第4工程は、250℃以上400℃以下の温度であり、保持時間が30分以上2時間以下で行われることを特徴とする請求項1から3のいずれか1項に記載の窒化物半導体光電極の製造方法。
- 前記第4工程後の前記ニッケル層は、酸素過剰の酸化ニッケル層となり、p型の半導体としての特性を示すことを特徴とする請求項1から4のいずれか1項に記載の窒化物半導体光電極の製造方法。
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