JP4892142B2 - Method for growing high quality iii- Nitride thin films by metalorganic chemical vapor deposition - Google Patents

Method for growing high quality iii- Nitride thin films by metalorganic chemical vapor deposition Download PDF

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JP4892142B2
JP4892142B2 JP2001186499A JP2001186499A JP4892142B2 JP 4892142 B2 JP4892142 B2 JP 4892142B2 JP 2001186499 A JP2001186499 A JP 2001186499A JP 2001186499 A JP2001186499 A JP 2001186499A JP 4892142 B2 JP4892142 B2 JP 4892142B2
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nitride
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JP2003012398A (en )
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玉 鉉 南
哲 守 孫
炯 洙 朴
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サムソン エルイーディー カンパニーリミテッド.
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【0001】 [0001]
【発明の属する技術分野】 BACKGROUND OF THE INVENTION
本発明はIII−族窒化物系化合物(BN、AlN、GaN、InNを含む化合物)半導体薄膜の成長方法に係り、より詳細には薄膜成長段階を二元化させることによって薄膜の特性を向上させうるMOCVD法(MOCVD;MetalOrganic Chemical Vapor Deposition)による高品位III−族窒化物系化合物薄膜の成長方法に関する。 The present invention relates to a method for growing a semiconductor thin film (a compound containing a BN, AlN, GaN, InN) III- Nitride-based compound, to improve the characteristics of the thin film by two yuan the film growth step is more sell MOCVD method; about growing method (MOCVD MetalOrganic Chemical Vapor deposition) high grade III- nitride-based compound thin film by.
【0002】 [0002]
【従来の技術】 BACKGROUND OF THE INVENTION
図1は、従来のMOCVD法により成長したGaN薄膜の垂直断面図である。 Figure 1 is a vertical sectional view of a GaN film grown by a conventional MOCVD method. 前記GaN薄膜は示したように、まずサファイア基板1上にMOCVD法により400〜600℃でAlGaNバッファ層2を成長させ、その上に再び900〜1100℃でGaN層3を成長させる。 The GaN thin film as shown, first by MOCVD on the sapphire substrate 1 is grown AlGaN buffer layer 2 at 400 to 600 ° C., a GaN layer 3 is grown on again 900 to 1100 ° C. As.
【0003】 [0003]
このようにMOCVD法で成長したIII−族窒化物薄膜の特性は色々な実験変数により変化するが、特に成長過程で反応器圧力の変化によって初期成長機構に大きい差が生じる現象を見つけた。 This property of III- Nitride films grown by the MOCVD method so as to vary with different experimental variables, found a phenomenon that a large difference in the initial growth mechanism is caused by a change in reactor pressure, especially in the growth process.
【0004】 [0004]
また、窒化物系化合物半導体素子を製造する場合に一番基本的な特性は結晶性であって、研究者ごとに各自の反応器、実験条件に合うように最適化して使用している。 Also, most basic properties in the production of nitride-based compound semiconductor device is a crystalline, their reactor per researchers have used optimized to suit experimental conditions. ところが研究過程で多重量子ウェル、p−GaN、AlGaNなどの成長に有利な低い反応器圧力条件で結晶性が落ちる問題点が見つかった。 However multiple quantum wells in the research process, p-GaN, crystalline problems are found to fall in an advantageous low reactor pressure conditions for the growth of such AlGaN.
【0005】 [0005]
【発明が解決しようとする課題】 [Problems that the Invention is to Solve
本発明は前記のような問題点を改善するために創案したものであって、MOCVD法でIII−族窒化物薄膜を成長させる時に、反応器内の圧力を変化させる多段成長法を用いて薄膜の結晶性及び表面形状が向上するMOCVD法による高品位III−族窒化物薄膜の成長方法を提供するのにその目的がある。 The present invention was invented to solve the problems as described above, when growing III- Nitride films by MOCVD using a multi-stage growth method for changing the pressure in the reactor thin it is an object for the crystallinity and the surface shape to provide a high quality III- nitride method of growing a thin film by MOCVD to improve.
【0006】 [0006]
【課題を解決するための手段】 In order to solve the problems]
前記のような目的を達成するために本発明に係るMOCVD法による高品位III−族窒化物薄膜の成長方法は、基板上にMOCVD法を用いるIII−族窒化物薄膜の成長方法において、前記基板上にIII−族窒化物バッファ層を形成する段階と、前記III−族窒化物バッファ層上に反応器内部の圧力を所定値以上に高めて第1のIII−族窒化物薄膜を形成する段階と、前記第1のIII−族窒化物薄膜上に、前記反応器内部の圧力を前記第1のIII−族窒化物薄膜成長時の圧力より所定値以下に低めて第2のIII−族窒化物薄膜を形成する段階とを含むことを特徴とする。 High grade III- Nitride method of growing a thin film by MOCVD method according to the present invention in order to accomplish the above objects, in the growth method of III- Nitride films using MOCVD method on a substrate, said substrate forming forming a III- nitride buffer layer above the first III- nitride films by increasing the reactor pressure inside than a predetermined value in the III- nitride buffer layer If the the first III- nitride thin film, a second III- group nitride reduced the reactor pressure inside to a predetermined value or less than the pressure at the first III- nitride films grown characterized in that it comprises a step of forming an object thin film.
【0007】 [0007]
本発明において、前記基板はサファイア基板、シリコン基板またはGaAs基板であり、前記窒化物バッファ層はAl x Ga 1-x N(0≦x≦1)またはIn x Ga 1-x N(0≦x≦1)より形成され、前記第1及び第2のIII−族窒化物薄膜はGaN系窒化物より形成され、前記第1のIII−族窒化物薄膜は150〜400Torrの圧力範囲内で成長させ、前記第2のIII−族窒化物薄膜は50〜150Torrの圧力範囲内で成長させることが望ましい。 In the present invention, the substrate is a sapphire substrate, a silicon substrate or a GaAs substrate, the nitride buffer layer is Al x Ga 1-x N ( 0 ≦ x ≦ 1) or In x Ga 1-x N ( 0 ≦ x ≦ 1) is formed from the first and second III- nitride films formed from GaN-based nitride, the first III- nitride films grown in a pressure range of 150~400Torr the second III- nitride film is preferably grown in the pressure range of 50~150Torr.
【0008】 [0008]
【発明の実施の形態】 DETAILED DESCRIPTION OF THE INVENTION
以下、図面を参照して本発明に係るMOCVD法による高品位III−族窒化物薄膜の成長方法を詳細に説明する。 Hereinafter will be described a method of growing high quality III- Nitride Films by MOCVD method according to the present invention with reference to the drawings.
【0009】 [0009]
図2は、本発明に係るMOCVD法により成長したIII−族窒化物薄膜の垂直断面図である。 Figure 2 is a vertical sectional view of the grown III- Nitride films by MOCVD method according to the present invention. 本発明に係るMOCVD法により成長したIII−族窒化物薄膜は、1段階目の圧力が2段階目の圧力より高い2段階成長法を用いて、薄膜の結晶性及び表面形状が向上する特徴を有する。 III- Nitride films grown by MOCVD method according to the present invention, the characteristic pressure of the first stage is used two step growth method higher than the pressure in the second stage, thereby improving the crystallinity and the surface shape of the film a. すなわち、成長したIII−族窒化物薄膜の結晶性が落ちて表面形状が滑らかでない問題を改善するために、1段目では反応器圧力を高めて薄膜の結晶性を向上させ、2段階目では反応器圧力を低めて気相反応が少なくて勾配の大きい界面が得られ、厚さの均一性に優れた素子構造を成長させうる。 That is, in order to improve the problems crystallinity of the grown III- Nitride thin film surface shape falls not smooth, increasing the reactor pressure to improve the crystallinity of the thin film in the first stage, the second stage reactor with a small gas-phase reaction reduced pressure large surface gradient obtained may be grown excellent device structure the uniformity of the thickness. また、その成長方法自体は原料消耗側面でも優れた材料節減効果を有する。 Also, the growth method itself has an excellent material savings in raw material exhaustion side.
【0010】 [0010]
このようなIII−族窒化物半導体薄膜を具体的に製造する方法は次の通りである。 Method of manufacturing such a III- Nitride semiconductor thin film specifically is as follows.
【0011】 [0011]
本発明に係るMOCVD法による高品位III−族窒化物薄膜の成長方法では密着空間シャワーヘッド型反応器を用いる。 The high-grade III- Nitride films growth method by MOCVD according to the present invention using the trivial topology showerhead reactor.
【0012】 [0012]
まず、サファイアよりなる基板11上に400〜600℃の低温で20〜30nm厚さのAlGaN緩衝膜12を成長させた後、反応器内の温度を1000℃程度に高め、結晶成長圧力を150〜400Torrに変更して0.5μm以上の厚さを有する第1のIII−族窒化物薄膜13を成長させる(第1段階)。 First, after growing the 20~30nm thick AlGaN buffer layer 12 at a low temperature of the substrate 11 on the 400 to 600 ° C. of sapphire, increasing the temperature in the reactor to about 1000 ° C., 150 to the crystal growth pressure change to 400Torr growing first III- nitride film 13 having a thickness of more than 0.5 [mu] m (first step).
【0013】 [0013]
次に、III−族窒化物薄膜13の成長後に反応器内の温度を1000℃程度に維持したまま原料気体の供給を中断し、反応器圧力を50〜150Torrに低めて第2のIII−族窒化物薄膜14を形成する(第2段階)。 Next, III- family the temperature in the reactor after the growth of the nitride film 13 interrupts the supply of the material gas while maintaining at about 1000 ° C., a second III- families by lowering the reactor pressure to 50~150Torr forming a nitride thin film 14 (second step). ここで、前記AlGaN緩衝膜12はAl x Ga 1-x N(0≦x≦1)の含量比を有する。 Here, the AlGaN buffer layer 12 having a content ratio of Al x Ga 1-x N ( 0 ≦ x ≦ 1).
【0014】 [0014]
このように第1段階で反応器内の圧力が増加すれば、AlGaN緩衝膜12の分解が促進されて核生成層の全体的な粒子サイズが大きくなり、その密度は減少する。 In this way the pressure in the reactor in the first stage is increased, the overall particle size of the decomposition is promoted nucleation layer of AlGaN buffer layer 12 is increased, the density decreases. 粒子サイズが大きくなれば界面に形成される欠陥密度が急減する。 Defect density drops sharply particle size is formed at the interface the larger. また、反応器圧力が増加し、移送(キャリア)気体として使われる水素の解離が促進されて、III−族元素の表面移動度が増加し、このために粒子成長が促進される。 Also, the reactor pressure was increased, the transfer (carriers) are accelerated dissociation of the hydrogen to be used as a gas, increases the surface mobility of III- group element, particle growth is promoted for this. このような成長機構の変化によって、図3に示したように、成長圧力の増加によって双晶(double crystal)回折パターンの半価幅が減少し、これは欠陥密度の減少を意味する。 By a change in such growth mechanisms, as shown in FIG. 3, the half width of twin (double crystal) diffraction pattern is reduced by an increase in growth pressure, which means a reduction in defect density. しかし、粒子間の合体が起きつつ粒子界面に微細孔が形成される可能性が高まり、これは素子製造時に漏れ電流の原因となって素子破壊を促進する役割をする。 However, the more likely that the fine pores in the particle interface with happening coalescence between particles are formed, which serves to facilitate the device destruction causing current leakage during device manufacture. 結論的に、III−族窒化物薄膜の成長時に反応器内部の圧力が高まれば垂直方向への成長が速くなり、外部的微細孔またはピットが多く生じる代わりに内部的結晶欠陥は減る。 In conclusion, III-if the family inside the reactor pressure during growth of the nitride thin film Takamare faster growth in the vertical direction, internally crystal defects instead caused many external micropores or pits is reduced.
【0015】 [0015]
一方、第2段階でIII−族窒化物薄膜の成長時に反応器内部の圧力が低くなれば垂直方向への成長が遅くなり、相対的に側面への成長が速くなって外部的微細孔が少なく生じる代わりに内部的結晶欠陥は多くなる。 On the other hand, if pressure inside the reactor during the growth of III- Nitride films in the second stage is low slows down the growth in the vertical direction, less externally micropores grow to relatively sides faster internally crystal defects instead occurring increases.
【0016】 [0016]
図4A及び図4Bは、実際のGaN薄膜で観察される微細孔の様相を示している。 4A and 4B show the appearance of micropores observed in actual GaN film. すなわち、図4Aに示したように、200torrの高圧力で第1段階でのみ成長したGaN表面では微細孔が観察される一方、図4Bに示したように、200torrで1次成長させた後、100torrで2次成長させたGaN表面では微細孔がほとんど観察されなかった。 That is, as shown in FIG. 4A, while the micropores are observed in only grown GaN surface in the first stage at a high pressure of 200 torr, as shown in Figure 4B, after primarily grown in 200 torr, at the secondary the grown GaN surface was observed mostly micropores 100 torr.
【0017】 [0017]
このような実験の結果に基づいて本発明の成長法では、第1段階の高圧成長で外部的微細孔は多いが内部的欠陥が少ない窒化物結晶を成長させ、このような微細孔を第2段階で反応器圧力を低める低圧成長で埋め立てることによって素子構造成長に適した良質のGaN薄膜を確保できる。 The growth method results Based on the present invention in such experiments, external micropores at high pressure growth of the first stage often is grown internal defects is small nitride crystal, such micropores second the GaN thin film of good quality suitable for device structure grown by landfill at low pressure growth to lower the reactor pressure stages can be ensured.
【0018】 [0018]
【発明の効果】 【Effect of the invention】
以上、説明したように、本発明に係るMOCVD法による高品位III−族窒化物薄膜の成長方法は、反応器内部の圧力が高まれば垂直方向への成長が速くなり、外部的微細孔が多く生じる代わりに内部的結晶欠陥は減り、一方、反応器内部の圧力が低くなれば垂直方向への成長が遅くなり、相対的に側面への成長が速くなって、外部的微細孔が少なく生じる代わりに内部的結晶欠陥は多くなる実験結果に基づいて、まず高圧で内部的に欠陥が少ないIII−族窒化物結晶を成長させた後、相対的に多くなった微細孔を低圧成長で充填することによって、高品質のIII−族窒化物薄膜の素子を得られる長所を有する。 As described above, the growth method of high-grade III- Nitride Films by MOCVD method according to the present invention, the reactor if the pressure inside Takamare faster growth in the vertical direction, many external micropores reduced internally crystal defects instead of occurring, whereas, instead of reactor growth internal pressure to become if vertically lower slower and faster growth of the relatively aspects, occur less externally micropores internally crystal defects based on a number becomes experiments, firstly after growing internally few defects III- nitride crystals at high pressure, to fill the relatively large since micropores low growth by having the advantage obtained an element of high quality III- nitride films. すなわち、高圧成長工程と低圧成長工程から各工程の変数の長所だけをとることによって薄膜特性の向上が得られる。 That is, improvement in the film properties can be obtained by taking only the advantages of variables for each process from the high-pressure growth process and the low pressure growth process.
【図面の簡単な説明】 BRIEF DESCRIPTION OF THE DRAWINGS
【図1】従来のMOCVD法により成長したGaN薄膜の垂直断面図。 [1] vertical sectional view of a GaN film grown by a conventional MOCVD method.
【図2】本発明に係るMOCVD法により成長したGaN薄膜の垂直断面図。 Vertical cross-sectional view of a GaN thin film grown by the MOCVD method according to the invention; FIG.
【図3】図2のGaN薄膜のX線(10−12面)半値幅変化を示すグラフ。 [3] X-ray (10-12 surface) of the GaN thin film of Figure 2 a graph showing the half-width changes.
【図4】図4Aは200Torr圧力で1段階のみで成長させたGaN薄膜のSEM(Scanning Electron Microscope)写真であり、図4Bは200Torrで1次成長させた後100Torr圧力で2次成長させたGaN薄膜のSEM写真。 4A is a SEM (Scanning Electron Microscope) photograph of the GaN films grown only in one stage at 200 Torr pressure, Figure 4B were secondary grown 100Torr pressure After primary grown in 200 Torr GaN thin film SEM photograph of.
【符号の説明】 DESCRIPTION OF SYMBOLS
1…サファイア基板2…AlGaNバッファ層3…GaN薄膜11…サファイア基板12…AlGaNバッファ層13…第1GaN薄膜14…第2GaN薄膜 1 ... sapphire substrate 2 ... AlGaN buffer layer 3 ... GaN thin film 11 ... sapphire substrate 12 ... AlGaN buffer layer 13 ... first 1GaN film 14 ... second 2GaN film

Claims (7)

  1. 基板上にMOCVD法を用いるIII−族窒化物薄膜の成長方法において、 In III- Nitride growth method of a thin film using an MOCVD method on a substrate,
    前記基板上にIII−族窒化物バッファ層を形成する段階と、 Forming a III- Nitride buffer layer on the substrate,
    前記III−族窒化物バッファ層上に反応器内部の圧力を前記III−族窒化物バッファ層を形成した圧力よりも増加させて、第1のIII−族窒化物薄膜を形成する段階と、 On the III- Nitride buffer layer, the reactor internal pressure is increased than the pressure forming the III- Nitride buffer layer, forming a first III- Nitride films,
    前記第1のIII−族窒化物薄膜上に、前記反応器内部の圧力を前記第1のIII−族窒化物薄膜成長時の圧力より所定値以下に低めて第2のIII−族窒化物薄膜を形成する段階とを含むことを特徴とするMOCVD法による高品位III−族窒化物薄膜の成長方法。 Wherein the first III- Nitride thin film, the pressure inside the reactor to said first III- Nitride film growth during the second and lower than a predetermined value than the pressure of the III- Nitride films high grade III- nitride method of growing a thin film by MOCVD, characterized in that it comprises a step of forming a.
  2. 前記基板はサファイア基板、シリコン基板またはGaAs基板であることを特徴とする請求項1に記載の有機金属気相化学蒸着法による高品位III−族窒化物薄膜の成長方法。 The substrate high grade III- Nitride growth process of a thin film by metalorganic chemical vapor deposition method according to claim 1, wherein the sapphire substrate, a silicon substrate or a GaAs substrate.
  3. 前記窒化物バッファ層はAl x Ga 1-x N(0≦x≦1)またはIn x Ga 1-x N(0≦x≦1)より形成されることを特徴とする請求項1に記載のMOCVD法による高品位III−族窒化物薄膜の成長方法。 According to claim 1 wherein the nitride buffer layer is characterized in that it is formed from Al x Ga 1-x N ( 0 ≦ x ≦ 1) or In x Ga 1-x N ( 0 ≦ x ≦ 1) high grade III- nitride method of growing a thin film by MOCVD.
  4. 前記第1及び第2のIII−族窒化物薄膜はGaN系窒化物より形成されることを特徴とする請求項1に記載のMOCVD法による高品位III−族窒化物薄膜の成長方法。 It said first and second III- Nitride films high grade III- Nitride method of growing a thin film by MOCVD method according to claim 1, characterized in that it is formed from GaN-based nitride.
  5. 前記第1のIII−族窒化物薄膜は150〜400Torrの圧力範囲内で成長され、前記第2のIII−族窒化物薄膜は50〜150Torrの圧力範囲内で成長させることを特徴とする請求項1に記載のMOCVD法による高品位III−族窒化物薄膜の成長方法。 Claim wherein the first III- Nitride films grown at a pressure range of 150~400Torr, the second III- Nitride films, characterized in that grown in the pressure range of 50~150Torr high grade III- nitride method of growing a thin film by MOCVD method described in 1.
  6. 前記第1のIII−族窒化物薄膜を形成する段階は、前記圧力の上昇により前記バッファ層の分解が促進されることを特徴とする請求項1から5のいずれか一項に記載のMOCVD法による高品位III−族窒化物薄膜の成長方法。 Said first III- Nitride forming a thin film, MOCVD method according to any one of claims 1 5, characterized in that decomposition of the buffer layer by increasing the pressure is promoted high grade III- nitride method of growing a thin film by.
  7. 前記第1のIII−族窒化物薄膜と、前記第2のIII−族窒化物薄膜とは、共にGaNである請求項4に記載の高品位III−族窒化物薄膜の成長方法。 It said first III- group and a nitride film, said a second III- Nitride films, high-grade III- Nitride growth method of a thin film according to claim 4 are both GaN.
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US7855386B2 (en) 2004-04-27 2010-12-21 Showa Denko K.K. N-type group III nitride semiconductor layered structure
JP4432827B2 (en) 2005-04-26 2010-03-17 住友電気工業株式会社 Iii nitride semiconductor device and an epitaxial substrate
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JP4877144B2 (en) * 2007-08-10 2012-02-15 三菱化学株式会社 Method for manufacturing an epitaxial wafer
CN101847673A (en) * 2009-03-27 2010-09-29 大连美明外延片科技有限公司 GaN-based LED epitaxial wafer and growing method thereof
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CN103413872B (en) * 2013-08-13 2016-02-24 湘能华磊光电股份有限公司 Led epitaxial growth method and led chip obtained by this method

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