JP5493861B2 - Iii族窒化物結晶基板の製造方法 - Google Patents
Iii族窒化物結晶基板の製造方法 Download PDFInfo
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- JP5493861B2 JP5493861B2 JP2009536920A JP2009536920A JP5493861B2 JP 5493861 B2 JP5493861 B2 JP 5493861B2 JP 2009536920 A JP2009536920 A JP 2009536920A JP 2009536920 A JP2009536920 A JP 2009536920A JP 5493861 B2 JP5493861 B2 JP 5493861B2
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- group iii
- iii nitride
- nitride crystal
- crystal substrate
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- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/40—AIIIBV compounds wherein A is B, Al, Ga, In or Tl and B is N, P, As, Sb or Bi
- C30B29/403—AIII-nitrides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y20/00—Nanooptics, e.g. quantum optics or photonic crystals
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
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- C30B29/406—Gallium nitride
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
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- C30B9/00—Single-crystal growth from melt solutions using molten solvents
- C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
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- H01S5/22—Structure or shape of the semiconductor body to guide the optical wave ; Confining structures perpendicular to the optical axis, e.g. index or gain guiding, stripe geometry, broad area lasers, gain tailoring, transverse or lateral reflectors, special cladding structures, MQW barrier reflection layers having a ridge or stripe structure
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Description
アルカリ金属とアルカリ土類金属との少なくともいずれか一方を含むフラックスを用いた成長法によりIII族窒化物結晶を形成する結晶形成工程と、
前記III族窒化物結晶をスライスしてIII族窒化物結晶基板を作成するスライス工程と、
前記結晶形成工程の際の結晶内部への入り込みにより前記III族窒化物結晶基板の内部に入り込んでいるフラックスを気化させて前記III族窒化物結晶基板の外部へ排出させることが可能な最低温度以上、かつ前記III族窒化物結晶基板の表面を分解させない最高温度以下で、前記III族窒化物結晶基板を熱処理する熱処理工程と、
を有する。
図1、図2を参照して、本発明の実施の形態1のIII族窒化物結晶基板の製造方法を説明する。
次に、本発明の実施の形態2のIII族窒化物結晶基板の製造方法について、図3を参照して説明する。
上述の実施の形態1、2では、アルカリ金属をフラックスとして用いるフラックス溶液成長法が使用された。これに対し、実施の形態3として、アモノサーマル法を用いたIII族窒化物結晶基板の製造方法においても、本発明の特徴である熱処理工程を適用することができる。
図1、図2に示される方法によってIII族窒化物結晶基板であるGaN基板を製造するプロセスを、一例として説明する。
実施例1に比べて、熱処理温度を、フラックスが気化する最低温度よりも低温の800℃に変更する。そして、それ以外の工程は実施例1と同じとして、GaN基板を作製する。その評価結果は、後述する。
図3を参照して、実施例2のIII族窒化物結晶基板の製造方法について、GaN基板を例に説明する。
実施例2に比べて、熱処理温度を、III族窒化物結晶基板の表面で分解が生じる限界よりも高温の1300℃に変更する。そして、それ以外の工程は実施例2と同じとして、GaN基板を作製する。
この温度条件で製造したGaN基板のGa面の表面粗さRaを測定したところ、Ra=0.6nmで「○」であった。また、熱処理後のマクロ欠陥面積比率は、0.03%で「○」であった。
800℃での熱処理後の表面粗さはRa=0.5nm,マクロ欠陥面積比率0.003%とともに良好であり、両者ともに「○」であった。
実施例1において1000℃の熱処理を行ったところ、Ga面の表面粗さRaは増えて1.3nmであった(「○」)。熱処理後のマクロ欠陥面積比率は、0.01%となり(「○」)、電子顕微鏡を用いて倍率1000倍で観察すると、Gaが表面に析出したバルーン状(液滴状)の欠陥や、ピット状の欠陥が認められた。その後、GaN基板上にエピタキシャル成長を行ったところ、表面粗さRaはエピタキシャル膜の成長前と同じRa=1.3nmであり「○」であった。またマクロ欠陥の増加は認められず、0.01%のままであり「○」であった。
1100℃の熱処理を行ったところ、GaN基板のGa面の表面粗さRaは1.5nmであった(「○」)。熱処理直後のマクロ欠陥面積比率は、0.15%で、「○」であり、バルーン状の欠陥よりもピット状の欠陥が優勢になっていた。その後、GaN基板上にエピタキシャル膜の成長を行ったところ、表面粗さRa及びマクロ欠陥の増加は認められなかった(いずれも「○」)。したがって、実施例1において熱処理温度を1100℃とすることにより、フラックス成分であるナトリウム(Na)を有効に除去できることを確認した。
1200℃で熱処理したところ、GaN基板のGa面の表面粗さRaは8.3nmとなり(「△」)、マクロ欠陥面積比率は1.3%となった(「△」)。Raが5nmを超えるとエピタキシャル膜の成長時に悪影響を及ぼすので、実施の形態2の処方により、熱処理工程の後に、研磨量が1μm以下となるように、「平坦化処理」を行った。この平坦化処理工程には、平均直径50nmのダイヤモンドスラリを用いた鏡面研磨を適用した。研磨後に、ダミー基板を剥がし、接着に用いたワックスを除去するために、ソルベントナフサ(登録商標)洗浄と、アセトン洗浄と、イソプロピルアルコール洗浄とから構成される洗浄工程(第1の洗浄工程15と同じ処理)を行った。その後、GaN基板の研磨による加工変質層を除去するために、塩素系プラズマドライエッチング処理を行った。さらに、GaN基板をバッファフッ酸溶液に10分間浸漬し、純水による流水洗浄を10分間行い、窒素乾燥後に120℃の硫酸過水溶液に10分間浸漬し、さらに流水純水洗浄する第2の洗浄工程を行い、窒素乾燥した。
1300℃の熱処理により、GaN表面粗さRaは、22.3nmまで劣化した(「×」)。マクロ欠陥面積比率も10.3%となり(「×」)、バルーン状のマクロ欠陥が増えた。これは、1300℃の熱処理によりGaN基板の窒素が脱離することでGaN結晶表面が分解し、GaN結晶のGaが液滴状態で付着したためである。この場合、平坦化処理工程の前に、熱処理に際に生じたバルーン状のGaの除去を行う必要がある。しかし、この状態で平坦化処理工程を行っても、工程が極めて複雑になり、生産性が低下する。
上記実施例1、2で得られたIII族窒化物結晶基板を用いて、半導体装置として、半導体レーザダイオードを作製した。図6を参照して説明する。図6は、本発明の実施例3の半導体レーザダイオード90の構造を示す断面図である。
Claims (13)
- アルカリ金属とアルカリ土類金属との少なくともいずれか一方を含むフラックスを用いた成長法によりIII族窒化物結晶を形成する結晶形成工程と、
前記III族窒化物結晶をスライスしてIII族窒化物結晶基板を作成するスライス工程と、
前記結晶形成工程の際の結晶内部への入り込みにより前記III族窒化物結晶基板の内部に入り込んでいるフラックスを気化させて前記III族窒化物結晶基板の外部へ排出させることが可能な最低温度以上、かつ前記III族窒化物結晶基板の表面を分解させない最高温度以下で、前記III族窒化物結晶基板を熱処理する熱処理工程と、
を有することを特徴とするIII族窒化物結晶基板の製造方法。 - 前記最低温度とは、前記フラックスが気化する温度である請求項1記載のIII族窒化物結晶基板の製造方法。
- 前記熱処理工程は、窒素を含むガス中で行われ、前記ガスの流速が毎分0.1mから10mである請求項1又は2に記載のIII族窒化物結晶基板の製造方法。
- III族窒化物結晶基板を洗浄することによって、熱処理工程によりIII族窒化物結晶基板の外部に排出されて前記基板に付着しているフラックスを除去する除去工程を、さらに有す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III族窒化物結晶基板の製造方法。
- 熱処理工程の後に、III族窒化物結晶基板の表面を平坦にする平坦化処理工程を、さらに有す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III族窒化物結晶基板の製造方法。
- 平坦化処理工程が、研磨、ドライエッチング処理、湿式エッチング処理の何れか一つあるいは二つ以上を組み合わせた処理工程であって、III族窒化物結晶基板の表面を、中心線平均表面粗さが0.1nm〜5nmとなるように平坦化させる工程であることを特徴とする請求項5記載のIII族窒化物結晶基板の製造方法。
- スライス工程において、III族窒化物結晶基板の厚みが200μm〜800μmとなるようにIII族窒化物結晶をスライスす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III族窒化物結晶基板の製造方法。
- ナトリウムを含むフラックスを用い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III族窒化物結晶基板の製造方法。
- 熱処理工程において、883℃以上1200℃以下で熱処理を行うことを特徴とする請求項8記載のIII族窒化物結晶基板の製造方法。
- 結晶形成工程において超臨界状態のアンモニアと鉱化剤とを含むフラックスを用い、熱処理工程において、III族窒化物結晶基板の内部に入り込んでいるアンモニアと鉱化剤とを前記III族窒化物結晶基板の外部へ排出させることを特徴とする請求項1記載のIII族窒化物結晶基板の製造方法。
- III族窒化物が窒素とガリウムを含む化合物であることを特徴とする請求項1記載のIII族窒化物結晶基板の製造方法。
- 熱処理工程の後に、マクロ欠陥量を光学的に検査する検査工程を有することを特徴とする請求項1記載のIII族窒化物結晶基板の製造方法。
- III族窒化物結晶基板の主表面側から検査した欠陥部分と正常部分との面積比率をマクロ欠陥量とすることを特徴とする請求項12記載のIII族窒化物結晶基板の製造方法。
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US20100213576A1 (en) | 2010-08-26 |
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JPWO2009047894A1 (ja) | 2011-02-17 |
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