WO2016194931A1 - Dispositif d'observation in situ du gauchissement d'un substrat et appareil de croissance de cristal - Google Patents

Dispositif d'observation in situ du gauchissement d'un substrat et appareil de croissance de cristal Download PDF

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WO2016194931A1
WO2016194931A1 PCT/JP2016/066135 JP2016066135W WO2016194931A1 WO 2016194931 A1 WO2016194931 A1 WO 2016194931A1 JP 2016066135 W JP2016066135 W JP 2016066135W WO 2016194931 A1 WO2016194931 A1 WO 2016194931A1
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substrate
crystal
crystal growth
light
base substrate
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PCT/JP2016/066135
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English (en)
Japanese (ja)
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憲次朗 池尻
英雄 会田
浩司 小山
聖祐 金
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並木精密宝石株式会社
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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
    • C30B25/16—Controlling or regulating
    • 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
    • C30B35/00—Apparatus not otherwise provided for, specially adapted for the growth, production or after-treatment of single crystals or of a homogeneous polycrystalline material with defined structure
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/24—Measuring arrangements characterised by the use of optical techniques for measuring contours or curvatures

Definitions

  • the present invention relates to an in-situ observation apparatus and a crystal growth apparatus for substrate warpage.
  • Warpage of the semiconductor substrate finally taken out after completion of the semiconductor process can be measured with a non-destructive and non-contact dedicated measuring device.
  • the semiconductor process performs processing with complicated temperature changes continuously, it is not enough to measure the semiconductor substrate after the process is completed.
  • In-situ observation of warpage changes due to stress changes during the semiconductor process ( Hereinafter, it is important to follow in-situ observation).
  • in-situ observation is very important for semiconductor crystal growth with large temperature changes.
  • various stresses are generated in the semiconductor substrate due to differences in growth methods and differences in characteristics from the base substrate. Specifically, the stress caused by the difference in thermal expansion due to the temperature distribution in the thickness direction of the underlying substrate, the lattice relaxation and coalescence of hetero growth, the stress due to the difference in thermal expansion coefficient, and the lattice generated due to the difference in growth method of homoepitaxial growth Stress generated due to the constant difference is generated.
  • These stresses cause warping in the growing semiconductor substrate. This warpage due to stress causes uneven temperature during growth, and not only causes poor quality of the semiconductor crystal but also causes cracks and breaks in the semiconductor crystal.
  • In-situ observation in the field of crystal growth includes in-situ observation for obtaining surface thin film information typified by ellipsometry, film thickness measurement by laser reflection (Non-Patent Document 1), in-warp of a semiconductor substrate. There is in situ observation (Non-Patent Document 2).
  • a conventional apparatus observes the surface of a growing semiconductor crystal and performs complex measurement including warping.
  • MOCVD Metal-Organic-Chemical-Vapor-Deposition
  • MOCVD Metal-Organic-Chemical-Vapor-Deposition
  • warping during growth as shown in Patent Document 1 is in- Situ observation is performed. Based on the obtained information, optimization of the base substrate and feedback to growth conditions are performed, and warpage is controlled.
  • the crystal growth surface is directly observed. Therefore, the in-situ observation is restricted by the morphology and thickness uniformity of the crystal growth surface, and accurate information cannot be obtained. For example, in the MOCVD nucleation phase, the signal drops due to surface roughness, so no information on warpage can be obtained.
  • the present invention has been made in view of the above circumstances, and it is an object of the present invention to provide an apparatus and a crystal growth apparatus that enable in-situ observation of the warping behavior of a crystal growth substrate.
  • the apparatus of the present invention includes at least a substrate, a light source that emits laser light, and a light receiving unit that receives the laser light, and at least one of the surfaces of the substrate is a crystal growth surface, The back surface is a reflecting surface, the laser light emitted from the light source is reflected by the reflecting surface, and the reflected light is received by the light receiving unit, and in-situ observation of the warpage of the substrate is performed. To do.
  • the laser light is two parallel separated lights separated before incidence of the reflecting surface, and an optical path difference occurs between the separated lights due to reflection on the back surface.
  • the wavelength of the laser light is preferably in the visible light range.
  • the wavelength of the laser light is preferably in the range of 620 nm to 660 nm.
  • the surface roughness Ra of the reflecting surface is preferably 20 nm or less.
  • the surface roughness Ra of the reflecting surface is preferably 1 nm or less.
  • the surface roughness Ra of the reflecting surface is preferably 0.1 nm or less.
  • the crystal growth apparatus of the present invention is provided with the apparatus described in any one of (1) to (7) above, and grows a crystal on the surface of the crystal growth surface.
  • the crystal grows any one of a nitride semiconductor, diamond, and SiC.
  • the apparatus and the crystal growth apparatus of the present invention it is possible to observe in-situ observation of the warp behavior of a crystal growth substrate on the back surface without being restricted by the morphology and thickness uniformity of the crystal growth surface. It becomes.
  • FIG. 6 is a partial cross-sectional explanatory view schematically showing the state of crystal growth by vertical HVPE and in-situ observation of substrate warpage on the back surface.
  • FIG. 6 is a partial cross-sectional explanatory view schematically showing the state of crystal growth by horizontal HVPE and in-situ observation of substrate warpage on the back surface.
  • FIG. 2 is a partial cross-sectional explanatory view schematically showing a schematic configuration of a microwave CVD apparatus, which is an example of a crystal growth apparatus for a diamond single crystal, and an in-situ observation state of substrate warpage on the back surface.
  • a microwave CVD apparatus which is an example of a crystal growth apparatus for a diamond single crystal, and an in-situ observation state of substrate warpage on the back surface.
  • It is a CCD observation image which shows the laser spot image of a semiconductor laser beam in an Example.
  • the first feature of the present embodiment is that the apparatus includes at least a substrate, a light source that emits laser light, and a light receiving unit that receives the laser light, and at least one of the surfaces of the substrate is a crystal growth surface.
  • the back surface is a reflecting surface, the laser light emitted from the light source is reflected by the reflecting surface, and the reflected light is received by the light receiving unit, and in-situ observation of the warpage of the substrate is performed. It was decided.
  • the warping behavior of the growth substrate (the substrate) during the film formation of the crystal is not limited by the morphology and thickness uniformity of the crystal growth surface, In-situ observation is possible from the back side.
  • a crystal is formed (growth) on a substrate when the crystal is formed so as to be in contact with the substrate, or a crystal is formed on the substrate via one or more layers. It is meant to include being done.
  • the back surface refers to a surface of the substrate on which the crystal is not grown or is not formed.
  • a second feature is that the laser light is two parallel separated lights separated before incidence on the reflecting surface, and an optical path difference occurs between the separated lights due to reflection on the back surface, and the optical path. Due to the difference, the in-situ observation of the warp was performed. According to this configuration, the optical path between the two reflected lights (separated light) reflected on the back surface is in a non-parallel state, and an optical path difference corresponding to the shape of the back surface (the warp shape and warpage amount of the substrate) occurs In-situ observation of the warpage of the substrate can be performed.
  • the third feature is that the wavelength of the laser beam is in the visible light range. According to this configuration, in-situ observation can be visually observed using a CCD or the like.
  • the fourth feature is that the wavelength of the laser beam is in the range of 620 nm to 660 nm. This configuration is optimal for in-situ observation because it has the lowest loss when reflected on the back surface of the substrate and does not absorb light even if there is a light transmissive part in the propagation optical path.
  • the fifth feature is that the surface roughness Ra of the reflecting surface is 20 nm or less. According to this configuration, scattering of laser light can be prevented.
  • the sixth feature is that the surface roughness Ra of the reflecting surface is 1 nm or less. According to this configuration, it is possible to further prevent laser light from being scattered and further prevent the laser light signal from dropping.
  • the seventh feature is that the surface roughness Ra of the reflecting surface is 0.1 nm or less. According to this configuration, it is possible to further prevent laser light from being scattered and further prevent the laser light signal from dropping.
  • the eighth feature is that the apparatus according to any one of the above is provided and a crystal growth apparatus for growing a crystal on the surface of the crystal growth surface.
  • the warping behavior of the growth substrate (the substrate) during the film formation of the crystal is not limited by the morphology and thickness uniformity of the crystal growth surface, In-situ observation is possible from the back side. Therefore, the warping behavior of the substrate can be optimally controlled.
  • the ninth feature is that the crystal grows a nitride semiconductor, diamond, or SiC crystal. According to this configuration, in-situ observation on the back surface of various crystals becomes possible.
  • FIG. 1 is an explanatory view schematically showing a schematic configuration of a vertical hydride vapor phase epitaxy (HVPE) apparatus suitable for a method for manufacturing a nitride semiconductor crystal.
  • the HVPE apparatus according to the present invention may be either a vertical type or a horizontal type.
  • the HVPE apparatus of FIG. 1 includes a reactor (reaction chamber) 1, a susceptor (substrate mounting portion) 3 for supporting a base substrate 4, which is a substrate disposed in the reactor 1, on a support surface, and a heater 2. .
  • the base substrate 4 is a substrate for growing an epitaxial growth film made of a GaN-based material on one surface 4a.
  • a total of five introduction pipes are installed: a pipe 8 for the carrier gas G 1, a pipe 9 for the group 3 source gas G 4, and a pipe 10 for the group 5 source gas G 3.
  • an exhaust pipe 6 is installed below the reactor 1 so that the gas flow is guided from above to below.
  • the apparatus according to the present invention includes a warp measuring apparatus 7 to be described later.
  • illustration of a vacuum device is abbreviate
  • a container 11 containing Ga liquid which is a Group 3 raw material of nitride semiconductor is disposed, and the Group 3 source gas G4 introduced into the reactor 1 is combined with the Ga liquid in the container 11.
  • a Group 3 metal chloride gas G2 is generated and introduced into the crystal growth surface of the base substrate 4.
  • a nitride semiconductor crystal 5 is grown as an epitaxially grown single crystal film on the underlying substrate 4.
  • the base substrate 4 is a substrate in which at least one side 4a on the crystal growth surface side of the nitride semiconductor crystal 5 is mirror-polished. Therefore, in the growth step of the nitride semiconductor crystal 5 described later, the nitride semiconductor crystal 5 is grown and formed on the mirror-polished surface. If necessary, a base substrate whose both surfaces are mirror-polished may be used. In this case, any one surface can be arbitrarily used as the crystal growth surface of the nitride semiconductor crystal 5.
  • the mirror polishing may be performed so that the nitride semiconductor crystal 5 is smooth enough to grow on at least one side 4a.
  • the surface roughness Ra is preferably 1 nm or less, preferably 0.8 nm or less. More preferably, it is 0.7 nm or less. If the Ra of the single side 4a exceeds 1 nm, the quality of the nitride semiconductor crystal 5 grown on the single side 4a is deteriorated. Furthermore, as a measure of the extent to which the nitride semiconductor crystal 5 can be epitaxially grown, it is preferable that the surface roughness Ra be 0.1 nm or less. Ra can be determined by measuring surface irregularities with a surface roughness measuring machine or an atomic force microscope (AFM). It is assumed that there is no crack on one side 4a on which nitride semiconductor crystal 5 is formed.
  • AFM atomic force microscope
  • the surface roughness Ra of the back surface (reflecting surface) is preferably such that the laser light 7b is not scattered as described above, and is specifically set to 20 nm or less.
  • the surface roughness Ra of the back surface (reflection surface) when using a base substrate that has been mirror-polished on both sides is preferably 1 nm or less, and more preferably 0.1 nm or less.
  • the formation of the nitride semiconductor crystal 5 on the base substrate 4 means that the nitride semiconductor crystal 5 is formed so as to be in contact with the base substrate 4, or one or more layers on the base substrate 4. It is assumed that the nitride semiconductor crystal 5 is formed via
  • the concave surface of the one side 4 a is caused by the temperature difference between the upper and lower surfaces of the base substrate 4.
  • the shape becomes stronger and the curvature changes greatly.
  • the temperature is lowered to about 500 to 600 ° C. and (b) the low temperature buffer layer is grown, the concave shape of the base substrate 4 is weakened and the curvature is slightly reduced.
  • the temperature is raised to about 1000 ° C., and (c) at the stage where the n-GaN layer is grown as a kind of the nitride semiconductor crystal 5, due to the lattice constant difference between the n-GaN layer and the base substrate 4,
  • the concave shape of the base substrate 4 is strengthened and the curvature is increased. Further, as the film formation proceeds and the thickness increases, the curvature increases.
  • the temperature is lowered to about 700 to 800 ° C.
  • the thickness of the InGaN-based active layer and the In composition in the InGaN Since the uniformity affects the in-plane uniformity of the emission wavelength, it affects the production yield of LED chips and the like. Since the thickness and In composition of the InGaN layer are affected by the film formation temperature, it is ideal that the curvature of the base substrate 4 during film formation be as close to 0 as possible in order to improve temperature uniformity within the substrate surface. is there. Finally, when the base substrate 4 is cooled down (e), the base substrate 4 is greatly warped again due to the difference in coefficient of thermal expansion, so that the curvature of the base substrate 4 after a series of film forming steps is large. Become.
  • the back surface refers to the surface of the base substrate 4 on which the nitride semiconductor crystal 5 is not grown or not formed.
  • the warpage measuring device 7 includes an optical element (preferably a semiconductor laser) which is a light source (not shown) inside and is connected to the HVPE device.
  • the laser beam 7 a emitted from the optical element is emitted from one emission port of the warpage measuring device 7 and is incident on the back surface of both surfaces of the base substrate 4. That is, the back surface of the base substrate 4 becomes a reflection surface of the laser light 7a.
  • the laser beam 7 a is reflected on the back surface of the base substrate 4. Further, the reflected reflected light (laser light 7b) is incident on the warp measuring device 7 again and received by a light receiving unit (not shown) inside the device 7, thereby forming the nitride semiconductor crystal 5 of the base substrate 4. Changes in the warp shape and warpage amount in the film are observed in-situ.
  • the laser beam 7a Before the laser beam 7a is incident on the reflecting surface of the base substrate 4, as shown in FIG. 2, the laser beam 7a is already separated into two separated light beams 7a1 and 7a2 having optical paths parallel to each other. Examples of the separation operation include birefringence.
  • the two parallel separated lights 7a1 and 7a2 have optical paths parallel to each other before entering the back surface, and the optical path difference (optical path length difference) between them is set to zero.
  • the separated lights 7a1 and 7a2 are reflected so that their optical paths are separated by reflection, and become reflected lights 7b1 and 7b2, respectively. Therefore, regardless of the concave shape or the convex shape, the optical path between the reflected lights 7b1 and 7b2 reflected on the back surface is in a non-parallel state, and between the reflected lights 7b1 and 7b2, the shape of the back surface (that is, the warped shape and warpage of the base substrate 4). An optical path difference corresponding to the amount is generated. The reflected light 7b1 and 7b2 are received by the light receiving unit and the optical path difference is observed, whereby in-situ observation of the warpage of the base substrate 4 is performed by the optical path difference.
  • the wavelength of the laser beam 7b is preferably a visible light region as a wavelength region that can be visually observed using a CCD (Charge-Coupled Device) or the like, and is specifically set to 360 nm to 830 nm. Further, in the visible light range, the wavelength range of 620 nm to 660 nm is the lowest loss when reflected on the back surface of the base substrate 4 and is not absorbed even if there is a light transmissive part in the propagation optical path. Since it is a wavelength, it is preferable.
  • the warp measuring device 7 can detect the laser light 7b reflected from the back surface without being scattered. Accordingly, the signal of the laser beam 7b does not drop (the laser beam 7b is scattered and cannot be detected by the warp measuring device 7), and the warp shape and warp during the film formation of the nitride semiconductor crystal 5 on the base substrate 4 are avoided. The amount can be observed in-situ.
  • the nitride semiconductor crystal 5 may be subjected to another process such as etching, polishing, or slicing.
  • the warping behavior of the base substrate 4 that causes the base substrate 4 or the crystal (nitride semiconductor crystal 5) to be broken or cause quality or performance failure is determined by the laser beam on the back surface. Reflection enables in-situ observation.
  • the warpage behavior of the base substrate 4 is the warpage behavior (change in warpage shape and amount of warpage) of the base substrate 4 during the growth of the nitride semiconductor crystal 5. Since the back surface of the substrate 4 is warped in-situ, the back surface can be observed in-situ without being limited by the morphology and thickness uniformity of the crystal growth surface (single surface 4a). Therefore, the warping behavior of the base substrate 4 can be optimally controlled.
  • FIG. 3 is an explanatory view schematically showing a schematic configuration of a horizontal HVPE apparatus suitable for the method for producing a nitride semiconductor crystal of the present invention.
  • the same number is attached
  • a total of three introduction pipes that is, a pipe 8 for the carrier gas G 1, a pipe 9 for the group 3 source gas G 4, and a pipe 10 for the group 5 source gas G 4 are installed horizontally.
  • Each introduction pipe extends toward the center of the reactor 1. The illustration of the vacuum device is omitted.
  • the reactor 1 is formed in a cylindrical shape, and is arranged in a laid-down state so as to face each other with the upper surface and the bottom surface standing in a direction perpendicular to the horizontal plane. Furthermore, a heater 2 is disposed around the reactor 1.
  • the susceptor 3 is disposed in a cantilevered manner on the other end side of the reactor 1 where the introduction pipe is installed, and the mounting surface of the base substrate 4 is in a horizontal plane. They are arranged in parallel.
  • the carrier gas G1, the group 3 source gas G4, and the group 5 source gas G3 pass through the pipes 8 to 10 in the reactor 1 to form the base substrate. 4 is introduced horizontally.
  • a container 11 containing Ga liquid as shown in FIG. 1 is arranged inside the pipe 9 (not shown in FIG. 3), and the Group 3 source gas G4 introduced from one end side of the pipe 9 is provided.
  • the Group 3 source gas G4 introduced from one end side of the pipe 9 is provided.
  • a Group 3 metal chloride gas G 2 is generated and introduced into the crystal growth surface of the base substrate 4.
  • N 2 gas G1 and GaCl gas G2 and NH 3 gas G3 are formed on one surface 4a of the base layer or the base substrate 4.
  • the nitride semiconductor crystal 5 (especially the GaN film) is grown over a predetermined time while introducing.
  • the laser beam 7a is emitted from the warp measuring device 7 during the formation of the nitride semiconductor crystal 5, is incident on and reflected from the back surface of the base substrate 4, and reflected light 7b1, 7b2 as shown in FIG. Observe the optical path difference. Such observation enables in-situ observation of changes in the warp shape and the warp amount during the formation of the nitride semiconductor crystal 5 on the base substrate 4.
  • the warpage shape and the warpage amount are not limited by the morphology and thickness uniformity of the crystal growth surface (single surface 4a).
  • the change can be observed in-situ on the back surface. Therefore, the warping behavior of the base substrate 4 can be optimally controlled.
  • FIG. 4 is a perspective view showing an example of the base substrate 4 according to the third embodiment.
  • FIG. 5 is an explanatory view schematically showing a schematic configuration of a microwave CVD (Chemical Vapor Deposition) apparatus suitable for the method for producing a diamond single crystal of the present invention.
  • the same number is attached
  • a base substrate 4 is prepared.
  • the material of the base substrate 4 include magnesium oxide (MgO), aluminum oxide ( ⁇ -Al 2 O 3 : sapphire), Si, quartz, platinum, iridium, and strontium titanate (SrTiO 3 ).
  • the base substrate 4 is a mirror whose at least one side 4a is mirror-polished.
  • the diamond single crystal growth step which will be described later, the diamond single crystal is grown and formed on the mirror-polished surface side (on the surface of the one surface 4a). If necessary, a base substrate whose both surfaces are mirror-polished may be used. In this case, any one surface can be arbitrarily used as a growth surface of the diamond single crystal.
  • the mirror polishing may be performed so as to be smooth to the extent that a diamond single crystal can be grown on at least one side 4a.
  • a guideline it is preferable to polish the surface to a surface roughness Ra of 10 nm or less. If the Ra of the single side 4a exceeds 10 nm, the quality of the diamond single crystal grown on the single side 4a is deteriorated. Furthermore, it is assumed that there is no crack on one side 4a. Ra may be measured with a surface roughness measuring machine.
  • a diamond single crystal is grown on one side 4a of the base substrate 4.
  • the method for growing the diamond single crystal is not particularly limited, but in this embodiment, a microwave plasma CVD apparatus 12 (hereinafter referred to as apparatus 12) as shown in FIG. 5 is used.
  • a water cooling holder 20 equipped with a heating body such as a heater and a water flow device is disposed in a chamber 15 provided with a gas introduction pipe 13 and a gas discharge pipe.
  • a microwave power source 16 is connected to the microwave introduction window 18 via the waveguide 17 so that plasma can be generated in the chamber 15.
  • a water flow device (not shown) is mounted inside the water cooling holder 20 and cools the base substrate 4 and a diamond single crystal 19 described later with a water flow.
  • a diamond single crystal 19 which is a film-like crystal is heteroepitaxially grown for a predetermined time (about 10 hours).
  • the laser beam 7 a is emitted from the warpage measuring device 7 during the film formation of the diamond single crystal 19, propagates through the optical window 21 provided in the water-cooled holder 20, and laser is applied to the back surface of the base substrate 4.
  • the light 7a is incident and reflected, and the optical path difference between the reflected lights 7b1 and 7b2 is observed as shown in FIG. By such observation, it becomes possible to observe in-situ changes in the warp shape and the warp amount during the film formation of the diamond single crystal 19 on the base substrate 4.
  • the warp measuring device 7 can detect the laser light 7b reflected from the back surface without being scattered. Therefore, the signal of the laser beam 7b does not drop (the laser beam 7b is scattered and cannot be detected by the warp measuring device 7), and the warp shape and the warp amount during the film formation of the diamond single crystal 19 on the base substrate 4 are reduced. Can be observed in-situ.
  • the surface roughness Ra of the back surface (reflective surface) is preferably such that the laser beam 7b is not scattered as described above, and is specifically set to 20 nm or less.
  • the surface roughness Ra of the back surface (reflection surface) when using a base substrate that has been subjected to mirror polishing on both sides is preferably 1 nm or less, and most preferably 0.1 nm or less.
  • the warpage behavior (change in warpage shape and amount of warpage) of the base substrate 4 during the growth of the diamond single crystal 19 is reflected by the laser light reflection on the back surface. -Situ observation is possible.
  • the warping behavior causes destruction of the base substrate 4 and the crystal (diamond single crystal 19), or quality and performance defects. Since the back surface of the substrate 4 is warped in-situ, the back surface can be observed in-situ without being limited by the morphology and thickness uniformity of the crystal growth surface (single surface 4a). Therefore, the warping behavior of the base substrate 4 can be optimally controlled.
  • the in-situ observation target process of the base substrate 4 is not limited to the film forming process of the nitride semiconductor crystal 5 and the diamond single crystal 19, In-situ observation of the warping behavior of the base substrate 4 in the annealing process performed before and after the film formation may be performed. In this case as well, in-situ observation may be performed by reflecting the semiconductor laser light from the warp measuring device 7 on the back surface of the base substrate 4.
  • the nitride semiconductor crystal 5 to be epitaxially grown may be a single crystal of AlN or BN in addition to the above embodiments.
  • the crystal to be epitaxially grown on the base substrate may be a SiC single crystal in addition to the nitride semiconductor crystal or diamond.
  • a metal film may be formed on the back surface, and the separated lights 7a1 and 7a2 may be reflected on the metal film.
  • the surface roughness Ra of the metal film surface serving as a reflecting surface for reflecting the separated lights 7a1 and 7a2 is preferably such that the laser light 7b is not scattered, and is specifically set to 20 nm or less.
  • the metal film material is preferably Pt, Ir, or Ta, but is not limited thereto.
  • the vertical HVPE apparatus shown in FIG. 1 is used for the apparatus according to the present embodiment, the substrate has a thickness of 0.43 mm, the planar shape is circular, the diameter is 2 inches, the crystal growth surface and the back surface are ( A sapphire single crystal substrate set with a (0001) plane was used.
  • the (0001) plane was mirror-polished to have a surface roughness Ra of 1 nm or less.
  • GaN was grown as a nitride semiconductor crystal 5 with a thickness of 200 ⁇ m.
  • the container 11 contains Ga liquid, and the carrier gas G1 is N 2 gas, the Group 3 source gas G4 is HCl, the Group 3 metal chloride gas G2 is GaCl, and the Group 5 source gas G3 is ammonia (NH 3 ). .
  • the sapphire substrate after the growth of GaN was annealed at 1020 ° C., and the semiconductor laser light was reflected on the back surface of the sapphire substrate, and the warpage behavior of the sapphire substrate in the annealing treatment was observed in-situ.
  • the semiconductor laser light was set to conditions in the wavelength range of 620 nm to 660 nm.
  • FIG. 6 shows a laser spot image of the semiconductor laser light obtained by reflection from the back surface of the sapphire substrate during the in-situ observation.
  • the portion surrounded by a square frame is a laser spot image of the semiconductor laser light detected during in-situ observation.
  • an elliptical semiconductor laser beam was detected during in-situ observation, and it was confirmed that the warping behavior of the sapphire substrate can be observed in-situ.
  • the same sapphire single crystal substrate and HVPE apparatus as in the example were prepared, and the semiconductor laser light was reflected on the (0001) plane of the crystal growth surface opposite to the back surface.
  • the configuration of the HVPE apparatus was the same as that of the above example except that the reflection surface of the semiconductor laser light was changed to a crystal growth surface.
  • the sapphire single crystal substrate after the growth of GaN was heated to 1020 ° C., and in-situ observation of the warpage behavior of the sapphire substrate was attempted, and a semiconductor laser obtained by reflection from the crystal growth surface of the sapphire substrate The light is shown in FIG.
  • the portion surrounded by the square frame is the semiconductor laser light detected during annealing.
  • the semiconductor laser light was detected as a turbulent spot image.
  • the disorder of the semiconductor laser light seems to be due to the deterioration of the surface morphology of the crystal growth surface due to the growth by the HVPE method. Further, it was confirmed that the warping behavior of the sapphire substrate could not be observed in-situ due to the disturbance of the semiconductor laser light.

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  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

Le problème à résoudre dans le cadre de la présente invention consiste à fournir un dispositif capable d'une observation in situ d'un comportement de gauchissement d'un substrat de croissance de cristal, ainsi qu'un appareil de croissance de cristal. Par conséquent, un dispositif d'après la présente invention comprend au moins un substrat, une source de lumière qui émet une lumière laser et une unité de réception de lumière qui reçoit la lumière laser. Le gauchissement du substrat est observé in situ par l'intermédiaire de la lumière laser provenant de la source de lumière et réfléchie par une surface réfléchissante qui est la surface arrière du substrat, la lumière réfléchie étant reçue au niveau de l'unité de réception de lumière. La lumière laser est constituée de deux lumières parallèles séparées avant de pénétrer dans la surface réfléchissante. La réflexion de la surface arrière génère une différence de trajets optiques entre les lumières séparées et le gauchissement est observé in situ par l'intermédiaire de cette différence de trajets optiques. En outre, un tel dispositif est monté sur l'appareil de croissance de cristal dans lequel le cristal est développé sur une surface de croissance de cristal du substrat.
PCT/JP2016/066135 2015-06-02 2016-06-01 Dispositif d'observation in situ du gauchissement d'un substrat et appareil de croissance de cristal WO2016194931A1 (fr)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09126913A (ja) * 1995-10-30 1997-05-16 Hitachi Ltd 応力測定装置および半導体製造装置
JPH10146753A (ja) * 1996-11-15 1998-06-02 Nec Corp 基板の研磨方法及び研磨装置
JP2003014446A (ja) * 2001-07-02 2003-01-15 Misawa Homes Co Ltd 反り測定装置
JP2005197621A (ja) * 2004-01-09 2005-07-21 Nec Saitama Ltd Ｃｓｐ取り外し装置及び方法
JP2007217216A (ja) * 2006-02-15 2007-08-30 Sumitomo Electric Ind Ltd ＧａＮ結晶基板およびその製造方法、ならびに半導体デバイスの製造方法
JP2011246749A (ja) * 2010-05-25 2011-12-08 Tokuyama Corp アルミニウム系ｉｉｉ族窒化物製造装置、およびアルミニウム系ｉｉｉ族窒化物の製造方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH09126913A (ja) * 1995-10-30 1997-05-16 Hitachi Ltd 応力測定装置および半導体製造装置
JPH10146753A (ja) * 1996-11-15 1998-06-02 Nec Corp 基板の研磨方法及び研磨装置
JP2003014446A (ja) * 2001-07-02 2003-01-15 Misawa Homes Co Ltd 反り測定装置
JP2005197621A (ja) * 2004-01-09 2005-07-21 Nec Saitama Ltd Ｃｓｐ取り外し装置及び方法
JP2007217216A (ja) * 2006-02-15 2007-08-30 Sumitomo Electric Ind Ltd ＧａＮ結晶基板およびその製造方法、ならびに半導体デバイスの製造方法
JP2011246749A (ja) * 2010-05-25 2011-12-08 Tokuyama Corp アルミニウム系ｉｉｉ族窒化物製造装置、およびアルミニウム系ｉｉｉ族窒化物の製造方法

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