WO2009093753A1 - Iii族金属窒化物単結晶の製造方法 - Google Patents
Iii族金属窒化物単結晶の製造方法 Download PDFInfo
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- WO2009093753A1 WO2009093753A1 PCT/JP2009/051394 JP2009051394W WO2009093753A1 WO 2009093753 A1 WO2009093753 A1 WO 2009093753A1 JP 2009051394 W JP2009051394 W JP 2009051394W WO 2009093753 A1 WO2009093753 A1 WO 2009093753A1
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- single crystal
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- metal nitride
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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
- 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
-
- 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
- C30B19/00—Liquid-phase epitaxial-layer growth
- C30B19/12—Liquid-phase epitaxial-layer growth characterised by the substrate
Definitions
- the present invention relates to a method for producing a group III metal nitride single crystal.
- Gallium nitride thin film crystals are attracting attention as an excellent blue light-emitting device, put into practical use in light-emitting diodes, and expected as a blue-violet semiconductor laser device for optical pickups.
- the GaN single crystal grown by the Na flux method the GaN single crystal grows up to the back side of sapphire at the edge of the substrate, and the edge of the sapphire is firmly captured by the GaN single crystal. (See Fig. 12 and Fig. 13).
- stress other than the interface between the grown GaN single crystal and the sapphire was subjected to stress due to the difference in thermal expansion coefficient, preventing natural peeling and causing cracks.
- a large-area nitride single crystal film is obtained by providing a plurality of island-shaped base films on a substrate and growing the nitride single crystal on the island-shaped base film. Then, it was difficult to spontaneously peel the single crystal film from the substrate. In some cases, stress remains in the single crystal film and eventually cracks occur.
- the present applicant applied the single crystal It has been disclosed that when forming the base film, the base film is divided into islands, and an elongated arm portion is provided on the island-shaped base film.
- the growth start time at the confluence where the transition is concentrated tends to be delayed from other points.
- the thickness of the grown gallium nitride single crystal tends to be uneven.
- An object of the present invention is to suppress variation in the thickness of a single crystal film when growing a group III metal nitride single crystal by a liquid phase method using a template substrate. This is to prevent the single crystal film from cracking due to the difference in thermal expansion and to achieve natural peeling.
- the present invention uses a template substrate that includes a substrate body having a side surface and a pair of main surfaces, and a base film of a group IV metal nitride single crystal formed on at least one main surface of the substrate body.
- Group III metal nitride single crystal grown from the underlying film with the underlying film forming a convex shape when seen in a plane, and an unformed surface without the underlying film surrounding the entire circumference of the underlying film Is not in contact with Group III metal nitride single crystals grown from other underlayers.
- the base film since the base film has a convex shape when seen in a plan view, the nitride single layer caused by the difference between the growth start time at the confluence where the crystal transition is concentrated and the growth start time from the base film is obtained. Variations in crystal thickness can be suppressed.
- the imperfect surface surrounds the entire circumference of the base film, it is difficult for single crystals grown from the base film to reach the outer peripheral edge of the substrate body, and it is possible to prevent the cover on the side and back surfaces. .
- the group III metal nitride single crystal grown from the underlying film is prevented from coming into contact with the group III metal nitride single crystal grown from the other underlying film.
- the Group III metal nitride single crystal was grown independently from the Group III metal nitride single crystal grown from the other base film.
- FIG. 1 (a) is a plan view showing a template substrate 10 A according to an embodiment of the present invention
- FIG. 1 (b) shows a state where a nitride single crystal 3 is formed on the template substrate 10 A.
- Fig. 2 (a) is a plan view of the template substrate 10 B viewed from one main surface 1 a side, and Fig. 2 (b) shows the template substrate 10 B on the other main surface 1 c side.
- FIG. 3 (a) is a cross-sectional view of the template substrate 10A of the present invention
- FIG. 3 (b) is a cross-sectional view of the template substrate 10B of the present invention.
- FIG. 4A is a sectional view of the template substrate and the single crystal 13 in the comparative example
- FIG. 4B is a sectional view showing the template substrate and the single crystal 23 in the comparative example.
- FIGS. 5 (a), (b), (c), (d), (e) and (f) are plan views showing the respective underlying films and single crystals which can be used in the present invention.
- FIG. 6 is a plan view showing a template substrate 10 J and a single crystal thereon according to an embodiment of the present invention.
- FIG. 7 shows an appearance photograph of the GaN single crystal after completion of the growth in Example 1.
- Fig. 8 is a photograph showing the appearance after the GaN single crystal of Fig. 7 is peeled from the substrate body.
- FIG. 9 shows a photograph of the appearance of the GaN single crystal after completion of the growth in Example 2.
- FIG. 10 shows an appearance photograph after the GaN single crystal of FIG. 9 is peeled from the main surface of the substrate.
- Fig. 11 shows an external photograph of the surface of the GaN single crystal after completion of growth in Comparative Example 1.
- Fig. 12 shows an appearance photograph of the back side of the template substrate on which the GaN single crystal of Fig. 11 was formed.
- Fig. 13 shows an external view of the GaN single crystal and template substrate of Fig. 11 as seen from the side.
- FIG. 1 (a) is a plan view showing a template substrate 10A according to an embodiment of the present invention
- FIG. 1 (b) shows a state in which a nitride single crystal 3 is formed on the template substrate 10A.
- the substrate body 1 has a pair of main surfaces and side surfaces 1b.
- the substrate body 1 is a quadrilateral.
- a base film 2 made of a group III metal nitride single crystal is formed on one main surface 1 a of the substrate body 1.
- a base film is not formed on the other main surface of the substrate body 1.
- an unformed surface 4 on which no base film is formed is formed between the base film 2 and the outer peripheral edge of the main surface 1a of the substrate body. That is, unformed surfaces 4 a, 4 b, 4 c, and 4 d are formed between the four pieces of the base film 2 and the outer peripheral edge of the substrate body, respectively.
- the liquid phase method is applied on the undercoat film 2.
- a single crystal 3 is formed.
- the single crystal 3 tends to spread from the edge of the base film 2 to the outside.
- the non-formed surface 4 is formed between the edge of the base film 2 and the outer peripheral edge of the main surface 1a. For this reason, since the single crystal 3 extends laterally on the non-formed surface 4, it is possible to prevent the single crystal from extending to the side surface 1b and further to the main surface 1c on the opposite side.
- Fig. 2 (a) is a plan view of the template substrate 10B viewed from one main surface 1a side
- Fig. 2 (b) is a plan view of the template substrate 10B from the other main surface 1c side.
- the substrate body 1 is a quadrilateral.
- a base film 2 A made of a group III metal nitride single crystal is formed on one main surface 1 a of the substrate body 1.
- a base film 2 B made of a group III metal nitride single crystal is formed on the other main surface 1 c of the substrate body 1.
- an unformed surface 4 of the substrate body on which the base film is not formed is formed. That is, an unformed surface 4 is formed between the four pieces of the base films 2 A and 2 B and the outer peripheral edge of the substrate body.
- Single crystals 3 A and 3 B are formed on 2 B by the liquid phase method.
- Single crystal 3 A, 3 B are formed on 2 B by the liquid phase method.
- the single crystal 1 3 becomes the side surface 1 b of the substrate body 1, Furthermore, it turned out that it extended like 1 3 a and 1 3 b toward the edge of the opposite main surface 1 c. Thereby, the single crystal 13 is firmly captured by the side surface 1 b and the main surface 1 c of the substrate body. In this state, if a stress due to the difference in thermal expansion coefficient is applied between the substrate body and the single crystal, the single crystal 1 3 is likely to crack.
- the non-formed surface 4 on which the base film is not formed is formed between the outer peripheral edge of the substrate body 1 and the base film so as to surround the base film over the entire circumference.
- the single crystals 3, 3A, 3B can be prevented from extending so as to cover the side surface 1b and the opposite main surface 1c of the substrate body.
- the base films 2, 2 A, and 2 B are formed into convex figures when seen in a plan view. This means that a line segment connecting any two points of the outer contour line of the base film is located inside the outer contour line of the base film.
- Examples of such a figure include polygons such as a circle, an ellipse, a race track shape, a triangle, a square, a rectangle, a hexagon, and an octagon as illustrated in FIG. If the base film has an arm or a dent when viewed in plan, the thickness of the single crystal is likely to be uneven around it. However, in the present invention, since the base film of the convex figure having no such arm portion or dent portion is formed, nonuniformity of the thickness of the single crystal can be prevented.
- the group III metal nitride single crystal is independently grown from the base film so as not to contact the group III metal nitride single crystal grown from other seed crystals.
- a plurality of island-shaped circular base films are provided on a substrate body, and single crystals are grown from each base film to form a large bulk single crystal film. That is, as schematically shown in FIG. 4 (b), a large number of circular base films 2 2 are provided on the main surface 1 a of the substrate body 1. Clearance 24 is provided between the underlying films 22. In this state, a single crystal is grown from the base film 22 to form a Balta single crystal film 23. The single crystal films are connected to each other on the clearance 24 to form a connecting portion 23a.
- FIGS. 5A to 5F are plan views showing examples of planar patterns of the base film and the single crystal formed thereon, respectively.
- the base film 8C is circular, and the single crystal film 9C is grown thereon.
- the base film 8D has an elliptical shape or a racetrack shape, and a single crystal film 9D is grown thereon.
- the base film 8E has a triangular shape, and the single crystal film 9E has grown thereon.
- the base film 8F has a square shape, and the single crystal film 9F has grown thereon.
- the base film 8 G is rectangular, and the single crystal film 9 G is grown thereon.
- the base film 8H is hexagonal, and the single crystal film 9H is grown on it.
- one base film is formed on one base plate body, and an unformed surface is provided between the base film and the edge of the substrate main body.
- a plurality of base films may be formed on one substrate body.
- a plurality of base films 8 J are formed on the main surface 1 a of the substrate body 1.
- a single crystal 9 J is formed on each base film.
- a non-formed surface 14 is formed between adjacent base films. The widths of adjacent base films need to be wide enough that the single crystals grown from each base film do not contact each other.
- the distance d between the base film and the edge of the substrate body is preferably 1 mm or more from the viewpoint of preventing the single crystal from wrapping around the side surface. More preferably it is.
- the upper limit of d is not particularly limited, but d is preferably 10 mm or less from the viewpoint of productivity because the productivity of single crystals decreases when d is large.
- the distance between adjacent base films (minimum value) D prevents the single crystal from wrapping around the side surface of the substrate body.
- it is preferably 2 mm or more, and more preferably 4 mm or more.
- the upper limit of D is not particularly limited, but if D is large, the productivity of single crystals decreases. From the viewpoint of productivity, D is preferably 10 mm or less.
- 0% area of the uncompleted surface of the substrate main body is preferably from 1 0-9 0% 3 0-5 More preferably, it is 0%.
- the location of the base film may be located in the center of the substrate body, but it is more preferable that the base film is biased to the upper part of the substrate body.
- the GaN single crystal grows thicker as it gets closer to the bottom of the crucible, and the wrap-around growth is promoted.
- the seed crystal region is unevenly distributed at the top of the sapphire, so that it is possible to effectively prevent wraparound and secure an epitaxial growth area.
- the method for providing the base film and the unformed surface on the substrate body is not particularly limited, and the following can be exemplified.
- a base film is formed on the entire main surface of the substrate body, and then the base film is etched and removed by grinding.
- the material of the substrate body is not particularly limited, sapphire, silicon Tan'yui crystal, S i C single crystal, M g O single crystal, spinel (M g A 1 2 O 4 ),
- Examples thereof include perovskite complex oxides such as N d G a O 3 .
- A is a rare earth element
- D is one or more elements selected from the group consisting of niobium and tantalum
- y 0.3 to 0.98
- SCAM ScAlM g 0 4
- SCAM ScAlM g 0 4
- the group III metal nitride single crystal constituting the underlayer is a nitride of one or more metals selected from G a, A 1 and In, G a N, A 1 N, G a A 1 N, G a A 1 In n etc. G a N, A 1 N and G a A I N are preferable, and A 1 .N is particularly preferable.
- the thickness of the base film is not particularly limited. From the viewpoint of suppressing the melt back to the flux of the base film, it is preferably 1 ⁇ m or more. Also, if the base film is made thick, it takes time to form the base film. From this point of view, the thickness of the base film can be reduced to 50 zm or less.
- the present invention is applicable to the liquid phase method.
- a liquid phase method examples include a flux method, a high pressure solution method, and a low temperature method.
- the type of the flux is a group III metal nitride single crystal. There is no particular limitation as long as it can be generated.
- a flux containing at least one of Al-strength metal and Al-strength earth metal is used, and a flux containing sodium metal is particularly preferred.
- This group III metal nitride single crystal is a nitride of one or more metals selected from G a, A l, In and B, and G a N, A 1 N, G a A 1 N, G a A 1 In n, BN, etc.
- the raw materials constituting the flux are selected according to the target Group III metal nitride single crystal.
- gallium simple metal As the raw material of gallium, a gallium simple metal, a gallium alloy, and a gallium compound can be applied, but a gallium simple metal is preferable in terms of handling.
- aluminum source material an aluminum simple metal, an aluminum alloy, and an aluminum compound can be applied, but an aluminum simple metal is preferable in terms of handling.
- indium raw material indium simple metals, indium alloys, and indium compounds can be applied, but indium simple metals are also preferable in terms of handling.
- the growth temperature of the group III metal nitride single crystal and the holding time during the growth are not particularly limited, and are appropriately changed according to the type of the target single crystal and the flux composition. In one example, when growing a gallium nitride single crystal using a flux containing sodium or lithium, the growth temperature is set to 8
- It can be set to 0 0 to 1 0 0 ° C.
- the group III metal nitride single crystal is grown in an atmosphere composed of a mixed gas containing nitrogen gas.
- the total pressure of the atmosphere is not particularly limited, it is preferably 10 atm or higher, more preferably 30 atm or higher from the viewpoint of preventing evaporation of the flux.
- the total pressure of the atmosphere is preferably 20 0 atm or less. More preferably, it is less than 0 atm.
- the nitrogen partial pressure in the atmosphere is not particularly limited, it is preferably 10 to 200 atm, more preferably 100 to 100 atm when growing a gallium nitride single crystal. .
- the nitrogen partial pressure in the atmosphere is preferably 10 to 200 atm, more preferably 100 to 100 atm when growing a gallium nitride single crystal. .
- To 50 atm is preferable, and 1 to 10 atm is more preferable.
- Gases other than nitrogen in the atmosphere are not limited, but inert gases are preferable, and argon, helium, and neon are particularly preferable.
- the partial pressure of gases other than nitrogen is the total pressure minus the nitrogen gas partial pressure.
- a template substrate can be immersed in a flux in a crucible, the crucible can be accommodated in a pressure vessel, and heated while supplying a nitrogen-containing atmosphere in the pressure vessel. Further, the flux can be brought into contact with the surface of the base film by fixing the template substrate at a predetermined position and raising the crucible containing the flux upward.
- the present invention provides a crack of a grown single crystal even when a template substrate having a nonpolar plane seed crystal film such as m-plane GaN or a-plane GaN and a semipolar plane seed crystal film such as r-plane GaN is used. It was confirmed that it is effective for prevention.
- a nonpolar plane seed crystal film such as m-plane GaN or a-plane GaN
- a semipolar plane seed crystal film such as r-plane GaN
- a gallium nitride film was formed on the template substrate 1OA according to the method described with reference to FIGS. Specifically, the planar dimension of the substrate body 1 is a rectangle of 13 X 18 mm.
- a GaN film with a thickness of 30 ⁇ was deposited over the entire main surface 1 a of the substrate body by the HVPE method to form an underlayer. This base film was polished to leave base film 2 of 9 ⁇ 13 mm. d is 2 mm.
- Metal gallium (Ga) 3 g as a raw material, metal sodium (Na) 4 g as a flux and the template substrate were weighed and accommodated in a growth vessel.
- the growth conditions were as follows: nitrogen pressure 4MPa, temperature 875 ° C, and growth was performed for 200 hours.
- Figure 7 shows a photograph of the appearance of the GaN single crystal after growth.
- Figure 8 shows an external view of the GaN single crystal after it was peeled from the substrate body (the back of the GaN single crystal).
- a GaN single crystal has grown up to the back of the sapphire substrate body at one edge, and cracks occurred in the surrounding area, but in the approximately 80% area where no wraparound of the GaN single crystal was observed, The sapphire on the back side peeled off spontaneously after the growth was completed. Furthermore, when the surrounding GaN single crystal was removed, the remaining sapphire was also peeled off.
- a gallium nitride film was formed on each main surface of the template substrate 10B.
- the planar dimension of the substrate body 1 is a rectangle of 13 X 18 mm.
- a 5 ⁇ m-thick GaN film was formed over the entire main surfaces 1 a and 1 c of the substrate body by MOCVD to form an underlying film.
- This base film was polished to leave a base film 2 having a length of 9 mm x 13 mm. d is 2 mm.
- Metal gallium (Ga) 3 g as a raw material, metal sodium (Na) 4 g as a flux and the template substrate were weighed and accommodated in a growth vessel.
- the growth conditions were as follows: nitrogen pressure 4MPa, temperature 875 ° C, and growth was performed for 200 hours. '
- Figure 9 shows an external view of the GaN single crystal after the growth.
- Figure 10 shows a photograph of the appearance after the GaN single crystal is peeled from the main surface of the substrate (the back surface of the GaN single crystal).
- GaN single crystal grown on the back and front of the template substrate is the edge It was not connected at all. After the growth was completed, the GaN single crystals on both sides were naturally separated from the sapphire, and no cracks were found in one GaN single crystal. The other GaN single crystal cracked only at one location.
- a G a N single crystal was grown according to the method described with reference to Fig. 4 (a). Specifically, a base film 1 2 made of GaN having a thickness of 30 ⁇ m was formed on the main surface 1 a of the substrate body 1 made of 13 ⁇ 18 mm square sapphire by the HVPE method. The base film 12 covers the entire main surface 1a.
- a GaN single crystal was grown under the same weighing method and growth conditions as in Example 1.
- Figure 11 shows an external view of the surface of the GaN single crystal after the growth.
- Figure 12 shows an external view of the back side of the template substrate on which the GaN single crystal was formed.
- Fig. 13 shows an external view of the GaN single crystal and template substrate as seen from the side. The single crystal grew to the back of the sapphire and did not peel off. In addition, many cracks occurred on the GaN single crystal surface.
- a substrate body 1 made of 10 ⁇ 10 mm square sapphire was prepared.
- a strip-shaped base film made of a seed crystal having a thickness was patterned in a strip shape.
- the period of the base film is 9 ⁇ m
- the width of each base film is 3 111
- the distance between adjacent base films is 6 / Zm.
- a GaN single crystal was grown under the same weighing method and growth conditions as in Example 1. After the growth, the GaN single crystal was not peeled off from sapphire, and cracks were confirmed.
- a G a N single crystal was grown according to the method described with reference to Fig. 4 (b). Specifically, a substrate body 1 made of sapphire 1 Omm long by 10 mm wide was prepared. On the main surface 1 a of the substrate body, a large number of circular base films 2 2 made of GaN seed crystals having a diameter of 3 im and a thickness of ⁇ ⁇ ⁇ were formed. The distance D between adjacent subsurface films 22 is 6 ⁇ .
- G a single crystal growth was performed using the same weighing method and growth conditions as in Example 1. After the growth, the G a N single crystal was integrated as a single film. The G a N single crystal was not peeled off from sapphire, and cracks were confirmed.
Abstract
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Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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CN2009801031540A CN101925696B (zh) | 2008-01-24 | 2009-01-22 | Ⅲ族金属氮化物单晶的制造方法 |
JP2009550591A JP4595030B2 (ja) | 2008-01-24 | 2009-01-22 | Iii族金属窒化物単結晶の製造方法 |
DE112009000195.5T DE112009000195B4 (de) | 2008-01-24 | 2009-01-22 | Verfahren zum Herstellen eines III-Metall-Nitrid-Einkristalls |
US12/804,521 US7988784B2 (en) | 2008-01-24 | 2010-07-23 | Method for manufacturing III metal nitride single crystal |
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JP2008-013689 | 2008-01-24 | ||
JP2008013689 | 2008-01-24 |
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US12/804,521 Continuation US7988784B2 (en) | 2008-01-24 | 2010-07-23 | Method for manufacturing III metal nitride single crystal |
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JP (1) | JP4595030B2 (ja) |
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WO (1) | WO2009093753A1 (ja) |
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JP2011046548A (ja) * | 2009-08-26 | 2011-03-10 | Panasonic Corp | テンプレートと、このテンプレートの製造方法と、このテンプレートを用いて育成した結晶と、この結晶の製造方法および製造装置 |
JP2011057479A (ja) * | 2009-09-08 | 2011-03-24 | Panasonic Corp | テンプレートと、このテンプレートの製造方法と、このテンプレートを用いて成長した結晶と、この結晶の製造方法および製造装置 |
JP2012126602A (ja) * | 2010-12-15 | 2012-07-05 | Ngk Insulators Ltd | Iii族窒化物単結晶の製造方法およびこれに用いる種結晶基板 |
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JP5310534B2 (ja) | 2009-12-25 | 2013-10-09 | 豊田合成株式会社 | Iii族窒化物半導体の製造方法 |
CN103243389B (zh) * | 2012-02-08 | 2016-06-08 | 丰田合成株式会社 | 制造第III族氮化物半导体单晶的方法及制造GaN衬底的方法 |
CN102748562A (zh) * | 2012-07-26 | 2012-10-24 | 江苏明江机械制造有限公司 | 隔热立管支撑环 |
JP5999443B2 (ja) | 2013-06-07 | 2016-09-28 | 豊田合成株式会社 | III 族窒化物半導体結晶の製造方法およびGaN基板の製造方法 |
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JPWO2009093753A1 (ja) | 2011-05-26 |
JP4595030B2 (ja) | 2010-12-08 |
DE112009000195T5 (de) | 2011-02-24 |
US20100307404A1 (en) | 2010-12-09 |
DE112009000195B4 (de) | 2015-12-10 |
CN101925696B (zh) | 2012-12-05 |
CN101925696A (zh) | 2010-12-22 |
US7988784B2 (en) | 2011-08-02 |
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