WO2009119159A1 - Substrat pour dispositif optique et procédé de fabrication du substrat - Google Patents

Substrat pour dispositif optique et procédé de fabrication du substrat Download PDF

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Publication number
WO2009119159A1
WO2009119159A1 PCT/JP2009/051871 JP2009051871W WO2009119159A1 WO 2009119159 A1 WO2009119159 A1 WO 2009119159A1 JP 2009051871 W JP2009051871 W JP 2009051871W WO 2009119159 A1 WO2009119159 A1 WO 2009119159A1
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Prior art keywords
buffer layer
layer
substrate
substrate member
optical device
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PCT/JP2009/051871
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English (en)
Japanese (ja)
Inventor
名西　▲やす▼之
荒木　努
高橋　功次
大平　重男
悟仁 鈴木
Original Assignee
日本軽金属株式会社
学校法人立命館
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Publication of WO2009119159A1 publication Critical patent/WO2009119159A1/fr

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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
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • 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
    • C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
    • C30B23/02—Epitaxial-layer growth
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02367—Substrates
    • H01L21/0237—Materials
    • H01L21/0242—Crystalline insulating materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02436—Intermediate layers between substrates and deposited layers
    • H01L21/02439—Materials
    • H01L21/02455—Group 13/15 materials
    • H01L21/02458—Nitrides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02436—Intermediate layers between substrates and deposited layers
    • H01L21/02494—Structure
    • H01L21/02496—Layer structure
    • H01L21/02502—Layer structure consisting of two layers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02521—Materials
    • H01L21/02538—Group 13/15 materials
    • H01L21/0254—Nitrides
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02656—Special treatments
    • H01L21/02658—Pretreatments
    • H01L21/02661—In-situ cleaning

Definitions

  • the present invention relates to an optical device substrate and a method for manufacturing the same, and more particularly, to an optical device substrate having a gallium oxide single crystal substrate member and having a gallium nitride layer grown at a predetermined growth temperature as a surface layer. About.
  • Gallium nitride (GaN) -based nitride semiconductor layers are applied as materials for optical devices, and blue LEDs, green LEDs, white LEDs, blue-violet LEDs, etc. are already on the market.
  • a substrate member for such an optical device sapphire and SiC are used. If the substrate member is conductive, electrodes can be drawn out from the back surface of the substrate member to form a vertical device structure, allowing a larger current to flow than the horizontal structure, which can improve luminous efficiency. It is. Further, if the substrate member is transparent with respect to the emission wavelength, light can be extracted from both surfaces of the substrate member, and the light extraction efficiency can be improved. For this reason, a conductive and transparent substrate member is desired. However, sapphire in practical use is transparent but not conductive. On the other hand, SiC is conductive but opaque.
  • gallium oxide (Ga 2 O 3 ) has been attracting attention as a substrate member for growing a GaN-based nitride semiconductor layer because it has the property of being conductive and transparent.
  • Ga 2 O 3 gallium oxide
  • the present inventors have proposed a method of forming a GaN layer on the surface of the Ga 2 O 3 substrate member by nitriding, and then lattice matching with the GaN layer to be grown thereafter (Patent Document 1 and Patent Document 1 below) 2).
  • Patent Document 1 and Patent Document 1 below JP 2007-137727 A JP 2007-137728 A
  • the present invention has been made to solve such a conventional problem, and has a gallium nitride layer having excellent surface flatness and crystal quality while using a gallium oxide substrate member. And an object of the present invention is to provide a manufacturing method thereof.
  • an optical device substrate includes a gallium oxide single crystal substrate member and has a gallium nitride layer grown at a predetermined growth temperature as a surface layer.
  • a second buffer layer made of hexagonal gallium nitride, and a hexagonal gallium nitride layer grown on the surface of the second buffer layer at the predetermined growth temperature is a gallium oxide single crystal substrate member and has a gallium nitride layer grown at a predetermined growth temperature as a surface layer.
  • a method for manufacturing an optical device substrate according to the present invention includes a gallium nitride single crystal substrate member and a method for manufacturing an optical device substrate having a gallium nitride layer grown at a predetermined growth temperature as a surface layer.
  • a first buffer layer made of hexagonal gallium nitride is formed on the surface of the gallium oxide single crystal substrate member by nitriding the gallium oxide single crystal substrate member, and a predetermined amount is formed on the surface of the first buffer layer.
  • FIG. 2 is a diagram showing RHEED patterns on the surface of a Ga 2 O 3 substrate member before and after nitriding in Example 1.
  • FIG. 6 is a diagram showing an RHEED pattern on the surface of a second buffer layer in Example 1.
  • FIG. 2 is a diagram showing an RHEED pattern and an SEM image on the surface of a GaN layer in Example 1.
  • FIG. 3 is a diagram showing a cross-sectional TEM image of the optical device substrate according to Example 1.
  • FIG. 3 is a diagram showing an X-ray rocking curve of a GaN layer in Example 1.
  • FIG. 6 is a diagram illustrating a manufacturing process of an optical device substrate according to Comparative Example 1.
  • FIG. 6 is a diagram showing an RHEED pattern and an SEM image on the surface of a GaN layer in Comparative Example 1.
  • FIG. 10 is a diagram showing a cross-sectional TEM image of an optical device substrate according to Comparative Example 2.
  • FIG. 1 shows a cross-sectional structure of an optical device substrate according to an embodiment of the present invention.
  • a first buffer layer 2 made of hexagonal gallium nitride (GaN) formed by nitriding is disposed on the surface portion of the gallium oxide (Ga 2 O 3 ) single crystal substrate member 1.
  • a second buffer layer 3 made of hexagonal GaN grown at a temperature lower than a predetermined growth temperature is disposed on the surface of the first buffer layer 2, and further, a predetermined buffer layer is formed on the surface of the second buffer layer 3.
  • a hexagonal GaN layer 4 grown at a temperature of 5 mm is disposed.
  • Si silicon
  • HF hydrogen
  • GaAs gallium arsenide
  • the Ga 2 O 3 substrate member 1 subjected to such pretreatment is set in a vacuum vessel, and thermal cleaning is performed.
  • Thermal cleaning is a method in which the Ga 2 O 3 substrate member 1 is heated and cleaned, and the temperature is 750 ° C. to 850 ° C., preferably 800 ° C., and the heating time is 10 minutes to 60 minutes.
  • the Ga 2 O 3 substrate member 1 is nitrided. Nitrogen plasma is used for the nitriding treatment, but radio frequency (RF) plasma is used as a plasma excitation method. In this case, an excited plasma is generated by applying a high-frequency magnetic field to molecular nitrogen (N 2 ).
  • RF radio frequency
  • the GaN layer is grown using the RF plasma excitation molecular beam epitaxy (MBE) method. In this case, continuous processing from nitriding to GaN layer growth can be performed in the same apparatus, and efficient processing becomes possible.
  • ECR electron cyclotron resonance
  • MBE RF plasma excitation molecular beam epitaxy
  • the nitriding treatment is performed with the Ga 2 O 3 substrate member 1 at a temperature of 300 to 400 ° C., a plasma power of 300 to 350 W, a nitrogen flow rate of 2 to 3 sccm, and a nitriding time of 60 to 100 minutes. If the nitridation time is shorter than 60 minutes, the formation of the nitride layer becomes insufficient, and cubic GaN is preferentially formed, and the formation of hexagonal GaN requires more than 60 minutes. Conversely, even if the nitriding time exceeds 100 minutes, the thickness of the nitrided layer becomes saturated and constant. For this reason, a nitriding time of 60 to 100 minutes is preferable. By such nitriding treatment, the first buffer layer 2 made of hexagonal GaN is formed.
  • the second buffer layer 3 made of hexagonal GaN is grown on the surface of the nitrided Ga 2 O 3 substrate member 1.
  • the temperature of the Ga 2 O 3 substrate member 1 is 480 to 520 ° C.
  • the plasma power is 250 to 350 W
  • the nitrogen flow rate is 1.5 to 2.5 sccm
  • the growth time is 5 to 15 minutes. If the growth time is less than 5 minutes, the growth of the GaN layer will be insufficient.On the other hand, if the layer thickness increases beyond 15 minutes, defects and dislocations will be induced by stress generation, which will affect the subsequent growth of the GaN layer. Therefore, it is preferable that the growth time is within this range.
  • a hexagonal GaN layer 4 is grown on the surface of the second buffer layer 3.
  • the GaN layer 4 is grown at a temperature of 650 to 750 ° C., a plasma power of 250 to 350 W, a nitrogen flow rate of 1.5 to 2.5 sccm, and a growth time of 50 to 90 minutes of the Ga 2 O 3 substrate member 1.
  • the second buffer layer 3 made of hexagonal GaN is further grown and formed.
  • various optical devices such as a light emitting element and a light receiving element, can be manufactured by using the board
  • this optical device substrate can be used as a template substrate, and a hexagonal GaN layer can be produced with good reproducibility on the GaN layer serving as the surface layer.
  • Example 1 First, a Ga 2 O 3 single crystal was grown by the floating zone (FZ) method. At this time, Ga 2 O 3 powder (purity 4N) was molded with a rubber tube and then sintered, and a single crystal was grown using this as a raw material rod. The single crystal growth conditions are a growth rate of 7.5 mm / h in a dry air atmosphere. The grown single crystal was cut into a thickness of 8 mm ⁇ 8 mm ⁇ 0.8 mm, and polished so that the (100) face became the surface, to a thickness of 0.4 mm.
  • FZ floating zone
  • This substrate member was introduced into an RF-MBE apparatus, heated to a temperature near 800 ° C., and then thermally cleaned by holding for 10 minutes. Thereafter, nitriding treatment was performed with nitrogen plasma excited by RF.
  • the nitriding conditions are a substrate member temperature of 300 ° C., an RF plasma power of 350 W, a nitrogen flow rate of 2.5 sccm, and a nitriding time of 90 minutes.
  • FIG. 3 shows the results of observation of reflection high-energy electron diffraction (RHEED) patterns on the surface of the Ga 2 O 3 substrate member before and after nitriding.
  • RHEED reflection high-energy electron diffraction
  • FIG. 4 shows an RHEED pattern when an electron beam is incident on the surface of the second buffer layer from the [11-20] direction or the [1-100] direction. A sharp streak pattern was observed similar to the surface of the Ga 2 O 3 substrate member after nitriding shown in FIG.
  • FIG. 5 shows a RHEED pattern and a surface SEM photograph of the GaN layer when an electron beam is incident on the surface of the formed GaN layer from the [11-20] orientation. RHEED is a streak-like pattern, and SEM photographs confirm that the surface has excellent flatness.
  • FIG. 6 shows a TEM cross section from the surface of the Ga 2 O 3 substrate member to the GaN layer in the optical device substrate thus manufactured. Further, when the crystallinity of the GaN layer produced in Example 1 was evaluated by an X-ray rocking curve, as shown in FIG. 7, the FWHM of GaN (002) was 22.0 arcmin with a single peak. It was.
  • Example 2 An optical device substrate was manufactured under the same conditions as in Example 1 above, except that the substrate member temperature when forming the GaN layer on the surface of the second buffer layer was set to 700 ° C. When the crystallinity of the produced GaN layer was evaluated by an X-ray rocking curve, the FWHM of the GaN (002) peak was 22.1 arcmin.
  • FIG. 8 shows a GaN layer was grown directly at a high temperature on the nitrided Ga 2 O 3 substrate member surface without forming a second buffer layer.
  • the growth temperature is set to 780 ° C. and 700 ° C. in the RF-MBE apparatus, and the growth time is 60 minutes. GaN growth for layer formation was performed.
  • FIG. 9 shows an RHEED pattern and a surface SEM photograph of the GaN layer when an electron beam is incident on the surface of the formed GaN layer from the [11-20] direction.
  • the growth temperature was 780 ° C., it was confirmed that peeling occurred in the GaN layer.
  • the GaN layer grown at a growth temperature of 700 ° C was able to suppress delamination, but the RHEED pattern was not a streak but a spot, and the surface flatness was found to be low from SEM photographs. did.
  • the FWHM of the GaN (002) peak measured by the X-ray rocking curve is 41.8 arcmin when the growth temperature is 780 ° C, and 83.0arcmin when the growth temperature is 700 ° C.
  • the GaN (002) peak in the GaN layers obtained in Examples 1 and 2 was 2 to 4 times larger than the FWHM. From this, it was found that the formation of the second buffer layer in the present invention is effective not only for the flatness of the GaN layer but also for improving the crystallinity.
  • FIG. 10 shows a cross-sectional TEM image of an optical device substrate described in the document EGVillora et al., Appl. Phys. Lett., 90 (2007) 234102.
  • a GaN layer having a thickness of about 400 nm is formed on the nitride layer on the surface of the Ga 2 O 3 substrate member indicated by a without forming the second buffer layer.
  • the GaN layer without the stacking fault itself is formed on the second buffer layer having a thickness of about 100 nm. That is, when the second buffer layer is not formed, GaN growth with a thickness of about 200 nm is necessary to eliminate stacking faults, whereas the thickness is formed on the nitride layer on the surface of the Ga 2 O 3 substrate member.
  • the second buffer layer By forming the second buffer layer by GaN growth of about 100 nm, a GaN layer free from stacking faults can be obtained. Therefore, it can be seen that the formation of the second buffer layer is effective from the viewpoint of production efficiency, manufacturing cost, and the like.
  • the second buffer layer made of gallium nitride is grown at a temperature lower than a predetermined growth temperature, and Since the gallium nitride layer is grown on the surface of the second buffer layer at a predetermined growth temperature, the light having a gallium nitride layer having excellent surface flatness and excellent crystal quality while using a gallium oxide substrate member A device substrate can be obtained.

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  • Condensed Matter Physics & Semiconductors (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Computer Hardware Design (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Power Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
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  • Physical Vapour Deposition (AREA)

Abstract

L'invention porte sur un substrat pour un dispositif optique possédant une couche de nitrure de gallium, qui présente une excellente planéité de surface même lorsqu'un élément substrat en oxyde de gallium est utilisé, et d'excellentes qualités cristallines. L'invention porte également sur un procédé de fabrication d'un tel substrat pour le dispositif optique. L'élément substrat en Ga2O3 sur lequel est effectué un nettoyage thermique est nitruré, une première couche tampon composée de GaN hexagonal est formée sur une surface de l'élément substrat en Ga2O3 et une seconde couche tampon composée de GaN hexagonal est amenée à croître sur la surface de la première couche tampon à une température de croissance de 480 à 520 °C. Ensuite, sur la surface de la seconde couche tampon, une couche de GaN hexagonal est amenée à croître en tant que couche de surface du substrat de dispositif optique à une température de croissance de 650 à 750 °C.
PCT/JP2009/051871 2008-03-25 2009-02-04 Substrat pour dispositif optique et procédé de fabrication du substrat WO2009119159A1 (fr)

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JP2008077902A JP2009227545A (ja) 2008-03-25 2008-03-25 光デバイス用基板及びその製造方法

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014084105A1 (fr) * 2012-11-28 2014-06-05 日本碍子株式会社 Substrat composite et élément fonctionnel
CN116190520A (zh) * 2023-05-05 2023-05-30 江西兆驰半导体有限公司 提高波长良率的led外延片及其制备方法、led芯片

Families Citing this family (3)

* Cited by examiner, † Cited by third party
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JP2013251439A (ja) * 2012-06-01 2013-12-12 Tamura Seisakusho Co Ltd 半導体積層構造体及び半導体素子
JP2015168594A (ja) * 2014-03-06 2015-09-28 日本電信電話株式会社 窒化物半導体の成長方法
JP2015017034A (ja) * 2014-06-25 2015-01-29 株式会社タムラ製作所 半導体積層構造体及び半導体素子

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006310765A (ja) * 2005-03-31 2006-11-09 Toyoda Gosei Co Ltd 低温成長バッファ層の形成方法、発光素子の製造方法、発光素子、および発光装置
JP2007134463A (ja) * 2005-11-09 2007-05-31 Koha Co Ltd 窒化物半導体成長基板及びその製造方法
JP2007137728A (ja) * 2005-11-18 2007-06-07 Nippon Light Metal Co Ltd 酸化ガリウム単結晶複合体の製造方法、及びこれを用いた窒化物半導体膜の製造方法

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2006310765A (ja) * 2005-03-31 2006-11-09 Toyoda Gosei Co Ltd 低温成長バッファ層の形成方法、発光素子の製造方法、発光素子、および発光装置
JP2007134463A (ja) * 2005-11-09 2007-05-31 Koha Co Ltd 窒化物半導体成長基板及びその製造方法
JP2007137728A (ja) * 2005-11-18 2007-06-07 Nippon Light Metal Co Ltd 酸化ガリウム単結晶複合体の製造方法、及びこれを用いた窒化物半導体膜の製造方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2014084105A1 (fr) * 2012-11-28 2014-06-05 日本碍子株式会社 Substrat composite et élément fonctionnel
CN116190520A (zh) * 2023-05-05 2023-05-30 江西兆驰半导体有限公司 提高波长良率的led外延片及其制备方法、led芯片

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