WO2013141099A1 - Substrat autoporteur cristallin au nitrure de gallium, et procédé de fabrication de celui-ci - Google Patents

Substrat autoporteur cristallin au nitrure de gallium, et procédé de fabrication de celui-ci Download PDF

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WO2013141099A1
WO2013141099A1 PCT/JP2013/056940 JP2013056940W WO2013141099A1 WO 2013141099 A1 WO2013141099 A1 WO 2013141099A1 JP 2013056940 W JP2013056940 W JP 2013056940W WO 2013141099 A1 WO2013141099 A1 WO 2013141099A1
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base substrate
substrate
plane
gan crystal
sapphire
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Japanese (ja)
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大士 古家
正信 東
只友　一行
成仁 岡田
啓輔 山根
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国立大学法人山口大学
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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/01—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes on temporary substrates, e.g. substrates subsequently removed by etching
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
    • C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
    • C23C16/30—Deposition of compounds, mixtures or solid solutions, e.g. borides, carbides, nitrides
    • C23C16/301—AIII BV compounds, where A is Al, Ga, In or Tl and B is N, P, As, Sb or Bi
    • C23C16/303—Nitrides
    • 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
    • C30B25/186—Epitaxial-layer growth characterised by the substrate being specially pre-treated by, e.g. chemical or physical means
    • 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
    • C30B29/406—Gallium nitride
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    • 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
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    • H01L21/0243—Surface structure
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    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
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    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02367—Substrates
    • H01L21/02433—Crystal orientation
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    • 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
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    • 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
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    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/02636—Selective deposition, e.g. simultaneous growth of mono- and non-monocrystalline semiconductor materials
    • H01L21/02639—Preparation of substrate for selective deposition
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    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/02636—Selective deposition, e.g. simultaneous growth of mono- and non-monocrystalline semiconductor materials
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    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02656—Special treatments
    • H01L21/02664—Aftertreatments

Definitions

  • the present invention relates to a gallium nitride crystal free-standing substrate, and more specifically, a gallium nitride crystal free-standing substrate in which a gallium nitride (GaN) crystal layer having a small threading dislocation density (dark spot density) is stacked on a sapphire base substrate and separated from the stacked substrate. And a method for manufacturing the same.
  • GaN gallium nitride
  • a semiconductor light emitting device such as a light emitting diode (LED) or a semiconductor laser (LD)
  • multiple quantum devices in which a quantum well layer composed of an n-type GaN layer, an InGaN layer, and a barrier layer composed of a GaN layer are alternately stacked on a sapphire substrate.
  • a well layer Multiple Quantum Wells: MQWs
  • a p-type GaN layer are sequentially stacked are mass-produced.
  • a GaN crystal grows in the axial direction, and the surface is a c-plane ( ⁇ 0001 ⁇ plane).
  • a Ga atom surface containing only Ga atoms is slightly positively charged, while an N atom surface containing only N atoms is slightly negatively charged, resulting in a c-axis.
  • Spontaneous polarization occurs in the direction (layer thickness direction).
  • compressive strain or tensile strain is generated in the GaN crystal due to the difference in lattice constant between the two, and piezoelectric polarization (piezo polarization) in the c-axis direction in the GaN crystal. Occurs (Patent Documents 1 and 2).
  • the piezoelectric polarization generated by the compressive strain applied to the InGaN quantum well layer is superimposed on the InGaN quantum well layer, Therefore, a large internal polarization electric field is generated in the c-axis direction. Under the influence of this internal polarization electric field, the quantum confined Stark Effect (QCSE) is considered to cause problems such as peak emission wavelength shift due to decrease in luminous efficiency and increase in required injection current. It has been.
  • QCSE quantum confined Stark Effect
  • an InGaN layer is formed on an a-plane ( ⁇ 11-20 ⁇ plane) or m-plane ( ⁇ 1-100 ⁇ plane), which is a nonpolar plane of a GaN crystal. It has been studied to avoid the influence of an internal electric field in which spontaneous polarization and piezoelectric polarization are superimposed (Patent Documents 1 to 3). Further, an InGaN quantum well layer is formed on a plane called a semipolar plane inclined about 60 degrees in the a-axis or m-axis direction, for example, a semipolar ⁇ 11-22 ⁇ plane, thereby It has also been studied to avoid the influence of the internal electric field (Non-Patent Documents 1 and 2).
  • Crystal dislocations are generated from the interface between sapphire and GaN due to the difference in lattice constant between sapphire as the base substrate and GaN as the growth crystal.
  • homoepitaxial growth in which a GaN crystal layer is grown on a GaN crystal free-standing substrate is effective.
  • the base substrate and the growth layer are the same material, it is possible to suppress the occurrence of dislocation due to the difference in physical properties. For this reason, a GaN crystal free-standing substrate is required to perform homoepitaxial growth.
  • a GaN crystal free-standing substrate having a nonpolar plane and a semipolar plane as a main surface is useful for manufacturing a highly efficient semiconductor light emitting device.
  • GaN crystal free-standing substrates having a nonpolar plane and a semipolar plane as a main surface are not in circulation and are difficult to obtain.
  • As a method for producing a GaN crystal free-standing substrate having a nonpolar plane and a semipolar plane as a main surface there is a method of cutting a specific surface from a bulk GaN crystal as a main surface, but it is extremely expensive and has a large area. However, it is not accepted industrially.
  • the laser lift-off method is a method of irradiating a laser from the sapphire side of a laminated substrate in which a GaN crystal layer is laminated on a sapphire substrate, decomposing the GaN crystal layer at the sapphire interface with the laser, and separating the sapphire substrate and the GaN crystal layer.
  • damage due to laser irradiation may occur in the GaN crystal layer.
  • the chemical etching method is not suitable for separation of the sapphire substrate because sapphire is chemically stable and insoluble in an acid solution or an alkali solution.
  • Mechanical polishing is extremely difficult because sapphire is very hard, and there is a risk of damage to the GaN crystal layer during the polishing process. Insertion of a release layer during the crystal growth process has a problem that the quality of the GaN crystal to be grown may be deteriorated and the number of crystal growth steps increases.
  • Mainly non-polar or semipolar surfaces such as GaN free standing substrate with low threading dislocation density and high crystal quality a-plane or m-plane, or free-standing substrate with ⁇ 11-22 ⁇ plane as the main plane
  • An object of the present invention is to provide a GaN crystal free-standing substrate made of only GaN crystal as a surface, and a method for manufacturing the same.
  • the present inventors have advanced research on a method for producing a GaN crystal having a desired crystal plane starting from the side wall surface of the groove portion of the base substrate using a sapphire base substrate having a plurality of concave groove portions. I made a suggestion. As we continue this research, we confirmed that the GaN crystal grown from the side wall surface spontaneously peels from the underlying substrate due to the difference in thermal expansion coefficient between GaN and sapphire and the resulting thermal stress near the interface between the two. The present invention has been completed.
  • a gallium nitride crystal layer is formed by laterally crystal growth from the side wall using a sapphire base substrate having a plurality of grooves having side walls inclined with respect to the main surface of the base substrate, After the film thickness of the crystal layer is grown to 100 ⁇ m or more, the sapphire base substrate and the gallium nitride crystal layer are simultaneously cooled to separate the sapphire base substrate and the gallium nitride crystal layer.
  • a method of manufacturing a gallium crystal free-standing substrate is provided.
  • 1) The ratio of the total area of the side wall that is the starting point of crystal growth to the total surface area of the base substrate on the side on which the gallium nitride crystal layer is formed is 1 to 20%.
  • the side wall from which crystal growth starts is the c-plane of a sapphire single crystal.
  • the present invention also provides a gallium nitride crystal free-standing substrate having a dark spot density of less than 2 ⁇ 10 8 pieces / cm 2 and a surface having a nonpolar or semipolar plane orientation.
  • a GaN crystal free-standing substrate having a nonpolar or semipolar plane orientation with a dark spot density of less than 2 ⁇ 10 8 pieces / cm 2 can be produced at low cost with simple operation and deterioration of crystal quality. Can be offered without.
  • the substrate and the growth layer are the same because the materials of the base substrate and the growth layer are the same. Generation of dislocations can be suppressed, and a semiconductor light emitting device with high luminous efficiency can be manufactured.
  • the surface orientation of the surface of the GaN crystal layer is a nonpolar plane or a semipolar plane, the effect of a decrease in light emission efficiency due to the quantum confined Stark effect compared to a conventional gallium nitride crystal layer substrate having a c-plane as a main surface Is small.
  • FIG. 2 is a photograph showing a natural peeling state after cooling between the base substrate and the GaN crystal of Example 1.
  • FIG. It is a photograph which shows the natural peeling state after cooling with the base substrate of the comparative example 1, and a GaN crystal.
  • the self-supporting substrate manufacturing method of the present invention is characterized in that a base substrate made of sapphire having a plurality of grooves is used, and a GaN crystal having a specific thickness is grown on the substrate.
  • the base substrate is a substrate made of sapphire, and has a plurality of groove portions having side walls inclined with respect to the main surface of the substrate, and a part of the side walls serves as a crystal growth starting point.
  • the dark spot density is a physical property value that serves as an index for indicating the density of threading dislocations, which are dislocation defects in the crystal, and is measured using a scanning electron microscope / cathode luminescence (SEM / CL) apparatus.
  • the acceleration voltage during measurement is 5 kV, and the observation range is 20 ⁇ m ⁇ 20 ⁇ m.
  • the dark spot density is calculated from the total number of dark spots observed within the observation range.
  • an arbitrary plane orientation is selected according to the crystal plane of the target GaN crystal.
  • the main surface of the sapphire base substrate is ⁇ 10-12 ⁇ .
  • the main surface of the sapphire base substrate is ⁇ 11-23 ⁇ .
  • the ⁇ 10-10 ⁇ plane, the ⁇ 11-20 ⁇ plane, the ⁇ 20-21 ⁇ plane, and the like can be main.
  • This main surface may be a miscut surface inclined at a predetermined angle with respect to the crystal axis in order to obtain a desired GaN crystal.
  • the base substrate is usually a disc having a thickness of 0.3 to 3.0 mm and a diameter of 50 to 300 mm, but is not particularly limited thereto.
  • the main surface of the base substrate can be arbitrarily selected.
  • the base substrate needs to have a plurality of groove portions, and a part of the side walls of the groove portions can be a starting point of crystal growth.
  • the base substrate main surface is the ⁇ 10-12 ⁇ plane and the extending direction of the groove is the ⁇ 11-20 ⁇ plane, that is, the a-axis direction
  • the c-plane is formed on one side wall of the groove.
  • the base substrate principal surface is the ⁇ 11-23 ⁇ plane and the extending direction of the groove is the ⁇ 10-10 ⁇ plane, that is, the m-axis direction
  • a c-plane is formed on one side wall of the groove.
  • the present invention Is achieved.
  • the side wall preferably has a total area of 1 to 20% with respect to the total surface area of the base substrate on the side where the gallium nitride crystal layer is formed.
  • a plurality of grooves are provided in parallel on the main surface of the sapphire base substrate.
  • the opening width of the groove is not particularly limited, and is usually set in the range of 0.5 to 10 ⁇ m.
  • the interval between the groove portions that is, the interval between the adjacent groove portions and the groove portion on the base substrate main surface line is 1 to 100 ⁇ m.
  • the lateral width of the bottom surface of the groove that is, the distance (w) in the direction perpendicular to the extending direction of the groove is not particularly limited, and is generally 1 to 100,000 ⁇ m.
  • the number of grooves on the main surface can be arbitrarily set according to the desired area of the GaN crystal to be formed. About 10 to 500 may be provided.
  • FIG. 1 shows a typical base substrate.
  • the groove has side walls inclined at a predetermined angle with respect to the base substrate main surface, and as shown in FIG. 2, the cross-sectional shape narrows the groove width from the groove opening toward the groove bottom.
  • the taper is inclined outward.
  • the inclination angle means an angle ( ⁇ ) formed by the base substrate main surface and the extended surface of the groove side wall. The angle is determined in consideration of the surface orientation of the side wall surface formed corresponding to the surface orientation of the base substrate main surface.
  • this angle ( ⁇ ) is set to 58.4 degrees.
  • a GaN crystal is grown so that the c-axis of the GaN crystal is in the same direction as the c-axis of the sapphire base substrate to obtain a desired crystal.
  • the angle 58.4 degrees at this time is formed by the ⁇ 11-22 ⁇ plane that is the principal surface of the desired GaN crystal and the c-plane of the GaN crystal that is perpendicular to the c-axis of the GaN crystal that is the growth direction. The angle is determined from being 58.4 degrees.
  • the angle formed between the ⁇ 10-12 ⁇ plane, which is the main surface of the sapphire base substrate used, and the sapphire c-plane appearing on the side wall of the groove is 57.6 degrees
  • the angle ( ⁇ ) is 57.6 degrees
  • the surface of the GaN crystal layer grown thereon is inclined by about 0.8 degrees with respect to the main surface of the sapphire base substrate. Therefore, by using a miscut substrate in which the main surface of the substrate is a surface having an off-angle with respect to the sapphire ⁇ 10-12 ⁇ plane so as to cancel out this angle, the ⁇ 11-22 ⁇ plane of the GaN crystal becomes sapphire.
  • a GaN crystal layer grown so as to be parallel to the main surface of the base substrate can be obtained.
  • the surface orientation of the main surface of the sapphire base substrate is ⁇ 11-23 ⁇ and the surface orientation of the desired GaN crystal is the ⁇ 10-11 ⁇ plane
  • this angle is set to 62.0 degrees.
  • the main surface portion of the substrate has an off angle with respect to the sapphire ⁇ 11-23 ⁇ plane so as to cancel out the inclination angle between the base surface of the base substrate and the GaN crystal surface of about 0.8 degrees, which is caused by the same reason as described above.
  • the surface orientation of the main surface of the sapphire base substrate is ⁇ 11-20 ⁇ and the surface orientation of the desired GaN crystal is the ⁇ 10-10 ⁇ plane, or the surface orientation of the main surface of the sapphire base substrate is ⁇ 10-10] ⁇
  • this angle is set to 90 degrees, and the GaN crystal is separated from the c-axis of the sapphire base substrate and the c-axis of the GaN crystal from this side wall. Are grown in the same direction to obtain a desired crystal.
  • the angle ( ⁇ ) formed by the base substrate main surface and the groove side wall is By using a sapphire base substrate having a groove close to 90 degrees, the ⁇ 10-10 ⁇ plane of the GaN crystal is on the sapphire base substrate main surface on the sapphire base substrate having the ⁇ 11-20 ⁇ plane as the main surface.
  • a GaN crystal layer grown so as to be obtained can be obtained.
  • the angle of 90 degrees is the angle formed by the ⁇ 10-10 ⁇ plane that is the principal surface of the desired GaN crystal and the c-plane of the GaN crystal that is perpendicular to the c-axis of the GaN crystal that is the growth direction. , 90 degrees.
  • a GaN GaN substrate is formed on a sapphire base substrate having a ⁇ 10-10 ⁇ plane as a main surface. A GaN layer grown so that the ⁇ 11-20 ⁇ plane is parallel to the main surface of the sapphire base substrate can be obtained.
  • the plane orientation of the main surface of the sapphire base substrate is ⁇ 0001 ⁇ and the plane orientation of the desired GaN crystal is the ⁇ 10-10 ⁇ plane
  • this angle is set to 90 degrees and GaN is applied to the sapphire base from this side wall.
  • a desired crystal is obtained by growing so that the c-axis of the GaN crystal is in the same direction as the a-axis of the substrate.
  • the angle of 90 degrees is the angle formed by the ⁇ 10-10 ⁇ plane that is the principal surface of the desired GaN crystal and the c-plane of the GaN crystal that is perpendicular to the c-axis of the GaN crystal that is the growth direction. , 90 degrees.
  • the width (d) of the region where the GaN crystal is grown (hereinafter referred to as crystal growth region) on the side wall of the groove is not particularly limited, but is preferably 10 to 3000 nm in order to reduce the dark spot density. It is particularly preferable that the thickness be ⁇ 1000 nm.
  • the width (d) of the crystal growth region is defined between the side where the base substrate main surface and the side wall intersect and the side where the side wall and the groove bottom face intersect when all the side walls are crystal growth regions.
  • the shortest distance (interval) on the side wall As shown in FIG. 3, when a part of the side wall is masked and the crystal growth region is limited, the distance (d) is obtained by subtracting the width of the masking portion from the shortest distance (interval).
  • the GaN crystal grows ELO starting from the side wall of the base substrate, and finally, the base substrate is covered, and GaN crystal layers having various plane orientations having surfaces parallel to the main surface of the base substrate are formed.
  • it is essential to form a GaN crystal layer grown from the side wall as a starting point with a thickness of 100 ⁇ m or more on the base substrate.
  • the reason why this natural peeling occurs is mainly due to the difference in thermal expansion coefficient between sapphire and GaN of the base substrate. Due to the difference in thermal expansion coefficient between the sapphire base substrate and the GaN, thermal stress is applied to the interface between the sapphire and the GaN crystal layer in the cooling step after the GaN crystal growth, which becomes a driving force for causing natural separation.
  • the second reason is that sapphire and GaN crystal are chemically bonded on the side wall surface of sapphire, which is the crystal growth region, but are simply in contact with and stacked on the other surface and main surface of the groove.
  • the side wall of the sapphire base substrate to be used preferably has a total area of 1 to 20% with respect to the total surface area of the base substrate on the side where the GaN crystal layer is formed. That is, when the GaN crystal layer grows in the lateral direction and covers the entire surface of the underlying substrate, if the region that becomes the growth starting point of the GaN crystal is 1 to 20%, the bonding force between the sapphire and the GaN crystal layer is 1 / It is thought that it is reduced to 100 to 1/5. 6 and 7 show optical micrographs (cross section, surface Nomarski image) of the peeled surface of the GaN crystal after peeling.
  • the peeled surface shape of the GaN crystal layer peeled from sapphire is the same as the shape of the GaN crystal layer grown on the sapphire base substrate in which the groove portion shown in FIG. 1 and FIG. 2 is formed, It can be seen that peeling occurs at the interface between the sapphire base substrate and the GaN crystal layer.
  • the film thickness of the crystal layer needs to be 100 ⁇ m or more, and is preferably 300 ⁇ m or more, because the GaN crystal layer may be partially destroyed during natural peeling.
  • the groove portion having the sidewall having the predetermined inclination angle is formed by patterning a photoresist so that only a portion where the groove portion is to be formed becomes an open portion, the photoresist is used as an etching resist, and the sapphire base substrate is subjected to reactive ion etching (Reactive It can be formed by dry etching such as Ion Etching (RIE) or wet etching.
  • Reactive It can be formed by dry etching such as Ion Etching (RIE) or wet etching.
  • control means such as the width of the side wall, the width of the groove opening, the space between the grooves, and the width of the bottom surface, the photoresist coating amount, baking temperature, baking time, UV irradiation amount, UV, Examples include the shape of a photomask when irradiating.
  • the etching stage it can be controlled by the etching gas type, etching gas concentration, etching gas mixture ratio, antenna power, bias power, etching time, and the like. By combining these various conditions, a sapphire base substrate having a groove having a predetermined shape can be obtained.
  • the width of the side wall can be controlled by obtaining an etching rate, which is the rate at which sapphire is etched per unit time, and changing the etching time.
  • a base substrate having side walls of various plane orientations can be created by selecting the main surface of the sapphire base substrate and setting the direction in which the groove extends. Specifically, when the base substrate main surface is the ⁇ 10-12 ⁇ plane and the extending direction of the groove is the ⁇ 11-20 ⁇ plane orientation, that is, the a-axis direction, The c-plane is exposed. Alternatively, when the base substrate principal surface is the ⁇ 11-23 ⁇ plane and the extending direction of the groove is the ⁇ 10-10 ⁇ plane orientation, that is, the m-axis direction, the c-plane is formed on the side wall as the crystal growth plane. Exposed.
  • the c-plane is formed on the side wall which is the crystal growth plane.
  • the main surface of the base substrate is the ⁇ 10-10 ⁇ plane and the extending direction of the groove is the ⁇ 11-20 ⁇ plane orientation, that is, the a-axis direction
  • the c-plane is formed on the side wall as the crystal growth plane. Exposed.
  • the base substrate main surface is the ⁇ 0002 ⁇ plane and the extending direction of the groove is the ⁇ 10-10 ⁇ plane orientation, that is, the m-axis direction
  • the a-plane is exposed on the side wall that is the crystal growth plane.
  • the sapphire base substrate can be arbitrarily designed with respect to the surface orientation of its main surface and the surface orientation of the side wall that becomes the crystal growth starting surface.
  • the sidewalls having various plane orientations lateral growth starting from the c-plane sidewall is likely to occur preferentially and easily controlled. Therefore, it is a preferable aspect to form a side wall composed of the c-plane on at least a part of the side wall constituting the groove.
  • a SiO 2 film, a SiN x film, a TiO 2 is formed in a region other than the crystal growth region by a method such as vacuum deposition, sputtering, or CVD (Chemical Vapor Deposition).
  • a method such as vacuum deposition, sputtering, or CVD (Chemical Vapor Deposition). Examples of the method include masking by forming two films, ZrO 2 films, and the like.
  • the thickness of the masking layer is usually about 0.01 to 3 ⁇ m.
  • the GaN crystal layer is grown in the lateral direction by the ELO method using the base substrate as a starting point.
  • the plane orientation of the crystal surface of the obtained GaN crystal layer corresponds to the main surface of the sapphire base substrate, and is composed of ⁇ 11-22 ⁇ plane, ⁇ 10-11 ⁇ plane, ⁇ 20-21 ⁇ plane, and the like.
  • the growth method of the GaN crystal is not particularly limited, and metal organic vapor phase epitaxy (MOVPE), molecular beam epitaxy (MBE), hydride vapor phase epitaxy (Hydrid Vapor Phase Epitaxy). : HVPE) is adopted.
  • the HVPE method is preferably employed because the crystal growth rate is high.
  • the two-stage method in which the MOVPE method is adopted as the first-stage growth method to first produce high-quality crystals and then the crystals are grown at a high speed by the HVPE method is a particularly preferable method.
  • the growth method using HVPE method is demonstrated.
  • the technology relating to the base substrate having a groove described in WO2010 / 023846 proposed by the inventors of the present invention can be applied mutatis mutandis.
  • the HVPE method is a method in which GaN crystal is epitaxially grown on a base substrate by reacting gallium chloride with ammonia as a nitrogen source in a gas phase, and is a method known per se.
  • the HVPE apparatus used for crystal growth is mainly composed of a reaction tube, a heating system, a gas supply system, and a gas exhaust system.
  • the gas supply system can precisely control the gas supply amount by a mass flow controller.
  • a hot wall method is used in which a reaction tube made of quartz is covered with a resistance heating heater, and the reaction tube, a substrate and a susceptor installed therein, and a metal material are heated.
  • the source gas can be sufficiently heated and supplied to the substrate surface, and the saturated vapor pressure of the supplied source can be increased. As a result, a large amount of raw material can be supplied and high-speed growth can be realized.
  • the reaction tube is roughly divided into a metal raw material part and a substrate heating part.
  • Ga metal is placed in the metal raw material portion, and by supplying HCl gas at a high temperature, Ga metal reacts with HCl gas to generate GaCl.
  • the generated GaCl gas passes through a quartz pipe and is carried to the substrate heating unit.
  • a susceptor made of carbon or SiC is arranged perpendicular to the gas flow, and the susceptor has a rotation mechanism. Then, a sapphire base substrate or a laminated substrate in which a GaN crystal is grown on the sapphire base substrate is set on the susceptor, and the GaCl gas generated in the metal raw material part and the NH 3 gas react on the substrate.
  • the growth of the GaN crystal proceeds.
  • NH 3 gas as a nitrogen source and HCl gas for generating GaCl as a Ga source are used as source gases.
  • Cl 2 gas may be used instead of HCl gas.
  • Ga metal which is a Ga raw material is installed in the apparatus.
  • Carrier gases such as H 2 and N 2 are used in addition to the source gas NH 3 and HCl gas.
  • the growth temperature In order to control the growth so as to preferentially occur from the sidewall of the groove without causing growth from the main surface of the substrate, the growth temperature, It is necessary to optimize various conditions such as growth pressure, raw material gas supply amount, raw material gas supply ratio, carrier gas type, carrier gas amount, etc. The conditions may be determined by preliminary experiments.
  • the sapphire base substrate used in the present invention may be coated with a crystal growth inhibition layer made of SiO 2 except for a region for crystal growth, and the growth from the main surface of the substrate is also suppressed by the provision of the crystal growth inhibition layer.
  • the GaN crystal has a base substrate main surface, a groove sidewall exposed from the sapphire c surface, and the other groove sidewall.
  • crystal growth from it is necessary to optimize the above various growth conditions in order to control the growth so as to preferentially occur from the groove side wall where the sapphire c-plane is exposed.
  • the growth from the main surface of the base substrate can be suppressed by providing a crystal growth inhibiting layer.
  • the GaN crystal may grow from the base substrate main surface and the groove side wall.
  • the groove side walls on both sides have the same plane orientation, it is necessary to control so that the GaN crystal having the same plane orientation grows from either side and the crystal grows from either side wall of the trench.
  • the growth from the main surface of the base substrate may be suppressed. In order to suppress the growth from the main surface of the base substrate, it is effective to provide a crystal growth inhibiting layer, but control is possible only by optimizing the above various growth conditions.
  • a sapphire base substrate or a multilayer substrate in which a GaN crystal is stacked on a sapphire base substrate is set on a susceptor so that the main surface of the sapphire faces upward, and then the reaction tube is heated to a crystal growth temperature.
  • the heater can individually control the metal raw material part and the substrate heating part.
  • the metal raw material part is heated to 800 to 900 ° C.
  • the substrate heating part is heated to 900 ° C. to 1150 ° C.
  • the thermal decomposition of the GaN crystal occurs when the substrate heating part is 500 ° C.
  • H 2 gas and NH 3 gas are circulated for the purpose of preventing this. Further, after the reaction tube reaches the set temperature, the state is maintained for several minutes to perform thermal cleaning of the substrate surface. Next, by allowing HCl gas to flow through the Ga metal installed in the reaction tube at a flow rate of 0.1 to 2.0 L / min, the Ga metal and the HCl gas react to generate GaCl. Further, NH 3 is circulated at a flow rate of 1 to 40 L / min. At this time, the carrier gas is H 2 , N 2 , or a mixed gas thereof, and the flow rate is 1 to 100 L / min.
  • the GaN crystal grows on the sapphire base substrate or a laminated substrate in which the GaN crystal is laminated on the sapphire base substrate.
  • the flow of HCl gas is stopped.
  • the NH 3 gas is kept flowing until the substrate part temperature becomes 600 ° C. or lower.
  • the substrate After growing the GaN crystal, the substrate is cooled.
  • the cooling may be performed forcibly by supplying a low temperature gas or the like, or may be performed by natural cooling.
  • the temperature of the sapphire base substrate and the GaN crystal layer is lowered to 20 ° C. to 150 ° C. by cooling.
  • the cooling rate is, for example, 1 to 100 ° C./min.
  • the sapphire base substrate having a relatively large thermal expansion coefficient generates a thermal stress that tends to warp upward, and a compressive stress is applied to the GaN crystal layer.
  • the GaN crystal is grown only from the side wall of the sapphire base substrate having the groove shape, the region where the sapphire and GaN are chemically bonded is narrow and the bonding force is small. Natural exfoliation occurs at the interface between the sapphire base substrate and the GaN crystal layer only by thermal stress during cooling without applying mechanical stress.
  • the ratio of the total area of the side wall, which is the starting point of crystal growth is 1 to 20% with respect to the total surface area of the sapphire base substrate on the side where the GaN crystal layer is formed. Is preferable, more preferably 1 to 15%, and still more preferably 1 to 10%.
  • the ratio of the total area of the side wall which is the starting point of crystal growth to the total surface area of the sapphire base substrate on the side where the GaN crystal layer is formed can be changed by changing the groove depth of the groove shape formed on the sapphire base substrate, It is controlled by changing the forming interval.
  • a gallium nitride crystal free-standing substrate having a dark spot density of less than 2 ⁇ 10 8 pieces / cm 2 and a surface having a nonpolar or semipolar plane orientation is produced.
  • the obtained GaN crystal laminated free-standing substrate can be used as a substrate for various semiconductor light-emitting elements by performing surface polishing or the like, if necessary, or this free-standing substrate can be used as a base substrate for GaN crystal growth. You can also.
  • Example 1 [Production of sapphire base substrate] A resist was patterned in a stripe shape on a ⁇ 10-12 ⁇ plane sapphire substrate, and then dry etching was performed by reactive ion etching (RIE) to form a plurality of grooves on the sapphire substrate.
  • the groove portion was formed so that the groove opening width was 3 ⁇ m, the groove depth was 0.1 ⁇ m, and the width of the main surface portion of the substrate up to the adjacent groove portion was 3 ⁇ m.
  • the inclination angle of the side wall is about 60 degrees, and the side wall width (d) calculated from the groove depth and the inclination angle of the side wall is 0.115 ⁇ m. After dry etching, the resist was washed away to obtain a sapphire base substrate.
  • the sapphire base substrate has a substrate main surface, 8466 groove portions, a crystal growth region composed of c-plane side walls, and a groove bottom surface.
  • the total area of the c-plane side wall is approximately 1.89% based on the total area on the growth side of the sapphire base substrate.
  • the prepared sapphire base substrate is set in a MOVPE apparatus on a quartz tray so that the substrate surface faces upward, and then the substrate is heated to 1150 ° C. and the pressure in the reaction vessel is set to 100 kPa.
  • the substrate was thermally cleaned by circulating H 2 at 10 L / min as a carrier gas and maintaining this state for 10 minutes.
  • the temperature of the substrate is set to 460 ° C.
  • the pressure in the reaction vessel is set to 100 kPa
  • a carrier gas flowing through the reaction vessel is allowed to flow at a flow rate of 5 L / min of H 2 , while supplying a group V element supply source ( NH 3 ) and a group III element supply source (TMG) were deposited in a thickness of about 25 nm on the substrate at a supply rate of 5 L / min and 5.5 ⁇ mol / min, respectively.
  • the temperature of the substrate is set to 1075 ° C.
  • the pressure in the reaction vessel is set to 20 kPa
  • the carrier gas to be circulated in the reaction vessel is set to H 2 so that it is circulated at a flow rate of 5 L / min.
  • the GaN deposited on was recrystallized to selectively form GaN crystal nuclei in the crystal growth region on the side wall of the groove.
  • the temperature of the substrate is set to 1025 ° C.
  • the pressure in the reaction vessel is set to 20 kPa
  • the carrier gas to be circulated in the reaction vessel is set to H 2 while being circulated at a flow rate of 5 L / min.
  • a group V element supply source (NH 3 ) and a group III element supply source (TMG) were allowed to flow for 300 minutes so that the respective supply amounts were 2 L / min and 30 ⁇ mol / min, and GaN (undoped) was formed on the GaN crystal nucleus.
  • NH 3 group V element supply source
  • TMG group III element supply source
  • the GaN crystals grown from the respective side walls of the groove formed on the main surface of the base substrate meet when the crystals collide with each other and have a ⁇ 11-22 ⁇ plane as the main surface parallel to the main surface of the substrate.
  • a GaN crystal layer was formed to produce a GaN crystal multilayer substrate.
  • HCl gas was circulated through the Ga metal installed in the reaction tube at 0.8 L / min. Further, NH 3 gas was supplied at 8 L / min and carrier gas H 2 gas was supplied at 34 L / min to grow a GaN crystal for 360 minutes. The film thickness of the GaN crystal was 360 ⁇ m. Thereafter, the flow of HCl gas was stopped, the growth was terminated, and the substrate was cooled. Cooling was performed by natural cooling while circulating gas. During cooling, NH 3 gas was passed at 5 L / min and H 2 gas at 17.1 L / min until the substrate temperature was 600 ° C. or lower, and N 2 gas was passed at 37.7 L / min at 600 ° C. or lower.
  • FIG. 4 shows the GaN crystal after natural peeling.
  • the left side of the figure is the peeled sapphire base substrate, and the right side is the peeled surface of the peeled GaN crystal layer.
  • 6 and 7 show a cross section and a surface image of the GaN crystal peeling surface after separation of the base substrate, which are observed with a Nomarski differential interference microscope.
  • FIG. 8 shows a cross-sectional SEM image of the GaN crystal grown by ELO on the base substrate.
  • the crystal grows in a shape as shown in FIG. From FIG. 6, it is observed that the peeled surface of the GaN crystal layer maintains this shape, and it can be seen that the peeling occurred at the interface between the GaN crystal layer and the sapphire base substrate. Further, from the surface image of the peeled GaN crystal layer shown in FIG. 7, a striped shape is observed in the entire region, and peeling at the interface between the sapphire base substrate and the GaN crystal layer occurs not in a part but in the entire region. It can be confirmed.
  • the obtained crystal was a free-standing GaN crystal having a thickness of 360 ⁇ m having a ⁇ 11-22 ⁇ plane as a main surface.
  • Example 2 A GaN crystal was grown in the same manner as in Example 1 except that the side wall width (d) of the sapphire base substrate used was 1.15 ⁇ m. At this time, the total area of the c-plane side wall is approximately 16.1% based on the total area on the growth side of the sapphire base substrate. The GaN crystal taken out through the cooling process was spontaneously peeled off from the base substrate in the same manner as in Example 1 to form a self-supporting GaN crystal having a thickness of 360 ⁇ m.
  • the GaN crystal was formed in the same manner as in Example 1 except that the side wall width (d) of the sapphire base substrate used was 1.15 ⁇ m and the growth time of the GaN crystal in the HVPE apparatus was 15 minutes. Grown up. The GaN crystal taken out through the cooling process did not peel off the GaN crystal layer from the sapphire base substrate.
  • the grown GaN crystal is shown in FIG. From FIG. 5, it can be seen that a GaN crystal has grown on the sapphire base substrate and no cracks or the like have occurred.
  • the thickness of the GaN crystal layer is 27 ⁇ m, and since the thickness of the GaN crystal layer is thin, the stress applied to the GaN crystal layer is small, and it is considered that natural peeling did not occur.
  • Example 2 From the dark spot density evaluation results of Example 1 and Example 2, it can be recognized that a high-quality semipolar plane GaN crystal free-standing substrate with few dislocations can be obtained.

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Abstract

L'invention fournit un substrat autoporteur cristallin au nitrure de gallium et son procédé de fabrication, ledit substrat autoporteur étant caractéristique en ce que la densité de points sombres est inférieure à 2×108 unités/cm2, et sa surface possède une orientation planaire non-polaire ou semi-polaire. Le procédé de fabrication de substrat autoporteur cristallin au nitrure de gallium est caractéristique en ce qu'est mis en œuvre un substrat de base de saphir dans lequel est formée une pluralité de parties rainure possédant des parois latérales constituées d'une face (c) de monocristaux de saphir, ou similaire, inclinée par rapport à la face principale du substrat de base. Une couche cristalline de nitrure de gallium est formée par une croissance de cristaux dans une direction latérale prenant pour origine la paroi latérale, et sa croissance se poursuit pour atteindre une épaisseur pelliculaire supérieure ou égale à100µm, et de préférence supérieure ou égale à 300µm. Enfin, le substrat de base de saphir et la couche cristalline de nitrure de gallium sont décollés par refroidissement.
PCT/JP2013/056940 2012-03-19 2013-03-13 Substrat autoporteur cristallin au nitrure de gallium, et procédé de fabrication de celui-ci WO2013141099A1 (fr)

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FR3021454B1 (fr) * 2014-05-20 2019-12-13 Centre National De La Recherche Scientifique (Cnrs) Procede de fabrication d'un materiau semi-conducteur incluant une couche de nitrure d'element iii semi-polaire
JP6831486B2 (ja) * 2020-01-23 2021-02-17 古河機械金属株式会社 基板の製造方法、ｉｉｉ族窒化物半導体系素子の製造方法

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