WO2013010117A1 - Procédé de croissance d'un cristal de nitrure du groupe iii au moyen d'un flux et de l'utilisation du cristal de nitrure du groupe ii en tant que grain pour une recristallisation ammonothermale - Google Patents

Procédé de croissance d'un cristal de nitrure du groupe iii au moyen d'un flux et de l'utilisation du cristal de nitrure du groupe ii en tant que grain pour une recristallisation ammonothermale Download PDF

Info

Publication number
WO2013010117A1
WO2013010117A1 PCT/US2012/046756 US2012046756W WO2013010117A1 WO 2013010117 A1 WO2013010117 A1 WO 2013010117A1 US 2012046756 W US2012046756 W US 2012046756W WO 2013010117 A1 WO2013010117 A1 WO 2013010117A1
Authority
WO
WIPO (PCT)
Prior art keywords
group
nitride crystal
ill
crystal
growth
Prior art date
Application number
PCT/US2012/046756
Other languages
English (en)
Inventor
Siddha Pimputkar
Shuji Nakamura
James S. Speck
Original Assignee
The Regents Of The University Of California
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by The Regents Of The University Of California filed Critical The Regents Of The University Of California
Publication of WO2013010117A1 publication Critical patent/WO2013010117A1/fr

Links

Classifications

    • 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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes
    • C30B7/105—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes using ammonia as solvent, i.e. ammonothermal processes
    • 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
    • C30B9/00—Single-crystal growth from melt solutions using molten solvents
    • C30B9/04—Single-crystal growth from melt solutions using molten solvents by cooling of the solution
    • C30B9/08—Single-crystal growth from melt solutions using molten solvents by cooling of the solution using other solvents
    • C30B9/12—Salt solvents, e.g. flux growth

Definitions

  • This invention relates to a method of fabricating Group-Ill nitride crystals and, more specifically, a method of growing a Group-Ill nitride crystal using a flux growth, and then using the Group-Ill nitride crystal as a seed for ammonothermal re- growth of the Group-Ill nitride crystal.
  • the invention also relates to apparatus for performing the method and compositions of matter fabricated using the method.
  • True bulk Group-Ill nitride crystals can be grown through various means, such as an ammonothermal method, a high pressure nitrogen solution growth method, or other flux methods, such as a sodium flux method, wherein a major component of the flux is elemental sodium.
  • a sodium flux method wherein a major component of the flux is elemental sodium.
  • the sodium flux method appears the most promising due to the currently demonstrated growth rates and resulting properties of the crystals.
  • GaN Gallium Nitride
  • the ammonothermal method has proven to be a viable one, it has its shortcomings in that the growth rate in a nonpolar direction is approximately 4-5 times slower than those in a polar direction. Therefore, in order to scale from small seeds to truly large crystals, a significant amount of time is needed to grow out the crystal in nonpolar directions. What is needed in the art, then, is a method that combines the best attributes of both the sodium flux method and the ammonothermal method for the growth of bulk Group-Ill nitride crystals. The present invention satisfies this need.
  • the present invention discloses a method of growing a Group-Ill nitride crystal using a flux method, wherein a fluid containing at least one Group-Ill metal and at least one alkali metal is contained within a vessel and is subject to conditions that allow for the addition or removal of nitrogen to or from the fluid, and the fluid is brought into contact with one or more surfaces of a seed upon which the Group-Ill nitride crystal is formed.
  • the present invention also discloses a method for using the Group-Ill nitride crystal grown using the flux method as a seed for re- growth using an ammonothermal method.
  • FIG. 1 is a schematic of an apparatus used in the sodium flux method according to one embodiment of the present invention.
  • FIG. 2 illustrates an embodiment of the present invention where the apparatus used in the sodium flux method includes a growth chamber connected to a preparation chamber.
  • FIG. 3 is a flowchart that illustrates an exemplary process for performing sodium flux growth followed by ammonothermal growth according to one
  • the sodium flux method grows Group-Ill nitride crystals in a flux comprising a fluid or melt containing at least one Group-Ill metal, such as Al, Ga and/or In, and at least one alkali metal, such as Na.
  • the fluid is contained within a chamber or vessel, and is subject to conditions that allow for the addition or removal of nitrogen to or from the fluid.
  • the fluid may be placed within a nitrogen-containing atmosphere and heated to a desirable temperature (typically greater than 700°C), wherein the fluid is brought into contact with one or more surfaces of a seed upon which the Group-Ill nitride crystal is formed.
  • This growth method faces are primarily related to the solubility of nitrogen into the flux and, once the nitrogen has been dissolved, the diffusion time required for the nitrogen to come into the vicinity of the growing Group-Ill nitride crystal.
  • Multiple methods have been proposed to enhance stirring of the fluid to increase the amount of dissolved nitrogen in close proximity of the crystal and, although these methods may be effective, they are not necessarily scalable and economic.
  • This invention proposes an alternative method of preparing the flux by saturating it with nitrogen prior to coming in contact with the crystal, and furthermore allowing the flux to be prepared under conditions other than those used for the growth of the Group-Ill nitride crystal.
  • FIG. 1 is a schematic of an apparatus used in the sodium flux method in its most general form.
  • the sodium flux method makes use of a vessel or chamber 100 (which may be open or closed) having a crucible 102 that contains a fluid 104 that is a crystal growth solution comprised of at least one Group-Ill metal, such as Al, Ga and/or In, and at least one alkali metal, such as Na.
  • the fluid 104 may contain any number of additional elements, compounds, or molecules to modify growth characteristics and crystal properties, such as B, Li, K, Rb, Cs, Be, Mg, Ca, Sr, Ba, Sr, C, Bi, Sb, Sn, Be, Si, Ge, Zn, P and/or N.
  • the chamber 100 contains a growth atmosphere 106 in which the fluid 104 is placed that can be a nitrogen-containing atmosphere 106, including, but not limited to, molecules such as diatomic N 2 , ammonia NH 3 , hydrazine N 2 H 6 , and atomic nitrogen N, or an atmosphere 106 with only trace amounts of nitrogen present, for example, an atmosphere comprised mainly of hydrogen, argon, etc.
  • the atmosphere 106 may be at vacuum, or may have a pressure greater than
  • the crucible 102 may include one or more heaters 108 so that fluid 104 may be heated and then held at one or more set temperatures, and one or more temperature gradients may be established within the chamber 100.
  • the fluid 104 is held at a temperature greater than approximately 200°C and below
  • the fluid 104 and atmosphere 106 in which it has been placed may be subject to electromagnetic fields, both static and/or dynamic.
  • the chamber 100 containing the fluid 104 can then be brought into contact with a seed 110, wherein the seed 110 is at least partially exposed to the nitrogen-containing atmosphere 106.
  • the seed 110 and/or fluid 104 may be subject to mechanical movements 112, such as stirring or agitating, to shorten the time required to saturate the fluid 104 with nitrogen.
  • the seed 110 is a Group-Ill nitride crystal, such as GaN, and may be a single crystal or a polycrystal. However, this should not be seen as limiting for this invention.
  • This invention specifically includes growing a Group- Ill nitride crystal on an arbitrary material, wherein the seed 110 may be an amorphous solid, a polymer containing material, a metal, a metal alloy, a semiconductor, a ceramic, a non-crystalline solid, a poly-crystalline material, an electronic device, an optoelectronic device.
  • the seed 110 may be an amorphous solid, a polymer containing material, a metal, a metal alloy, a semiconductor, a ceramic, a non-crystalline solid, a poly-crystalline material, an electronic device, an optoelectronic device.
  • the seed 110 When the seed 110 is a Group-Ill nitride crystal, it may have one or more facets exposed, including polar, nonpolar and semipolar planes.
  • the Group-Ill nitride seed crystal 110 may have a large polar c-plane ⁇ 0001 ⁇ facet or a
  • the Group-Ill nitride seed crystal 110 may have a large nonpolar m-plane ⁇ 10-10 ⁇ facet or a ⁇ 10-10 ⁇ approaching facet exposed; or the Group-Ill nitride seed crystal 110 may have a large semipolar ⁇ 10-11 ⁇ facet or a ⁇ 10-11 ⁇ approaching facet exposed; or the Group-Ill nitride seed crystal 110 may have a large nonpolar a-plane ⁇ 11-20 ⁇ facet or a ⁇ 11-20 ⁇ approaching facet exposed.
  • the flux method that is used to coat the seed 110 and form a resulting Group- Ill nitride crystal on the seed 110 is based on evaporation from the fluid 104, but may also include a solid source containing Group-Ill and/or alkali metals, which results in the formation of a layer of Group-Ill and alkali metal on the surfaces of the seed 110.
  • the flux method used to coat the seed 110 and form the Group-Ill nitride crystal on the seed 110 is based on bringing the seed 1 10 into contact with the fluid 104, intermittently or otherwise, by means of dripping and/or flowing the fluid 104 over one or more surfaces of the seed 110.
  • the flux method used to coat the seed 110 and form the Group-Ill nitride crystal on the seed 110 involves submersing or submerging the seed 110 within the fluid 104 and placing one facet of the seed 110 within some specified distance, such as 5 mm, of the interface between the fluid 104 and the atmosphere 106. Further, the seed 110 may be rotated and/or moved on a continuous or intermittent basis.
  • the Group-Ill nitride crystal may be A1N, GaN, InN, AlGaN, AlInN, InGaN, etc.
  • the Group-Ill nitride crystal may be at least 2 inches in length when measuring along at least one direction.
  • the Group-Ill nitride crystal may also have layers with different compositions, and the Group-Ill nitride crystal may have layers with different structural, electronic, optical, and/or magnetic properties.
  • the seed crystal 110 may be brought into contact with the fluid 104 by moving the crystal 110 into the fluid 104, as shown in FIG. 1.
  • the seed crystal 110 may be brought into contact with the fluid 104 by transporting the fluid 104 to be in contact with the crystal 110, as shown in FIG. 2.
  • FIG. 2 illustrates an embodiment where the apparatus used in the sodium flux method includes a growth chamber 200 connected to a preparation chamber 202, where the crystal is grown in the growth chamber 200 and the fluid is prepared in the preparation chamber 202.
  • a pump 204 moves the fluid from the preparation chamber 202 to the growth chamber 200 and a controller 208 controls the operation of a mechanism 208 in the growth chamber 200 for stirring or agitating the fluid, as well as one or more heaters 210 in the growth chamber 200 for heating the fluid. Excess fluid is then returned from the growth chamber 200 to the preparation chamber 202 for possible reuse and recycling.
  • the preparation chamber 202 is separate from the growth chamber 200, it is possible to expose the fluid to conditions that would not be favorable in the presence of a Group-Ill nitride crystal.
  • the preparation chamber 202 may subject the fluid to different conditions, such as different temperatures or pressures. Additional materials may also be added to the fluid, such as nitrogen- containing materials, one or more alkali metals, one or more alkali earth metals, and/or one or more Group-Ill elements.
  • the additional material may be added to the fluid in any state of matter, including solid, liquid or gas states, or as a plasma, and at any time during the process.
  • an electrical field may be applied to the fluid, or the fluid may be agitated to enhance mixing, or to enhance dissolution or evaporation of nitrogen from the fluid.
  • the crystal may be stationary, rotated around one or more axes, moved in any possible direction, and placed at any arbitrary angle with respect to the fluid and any applicable forces, such as the gravitational force;
  • Possible modifications and variations to this invention could include the use of a plurality of different preparation chambers, each of which would modify the fluid in a different way.
  • each of the different preparation chambers could modify the temperature or pressure, add or subtract elements or compounds, subject the fluid to electrical fields or mechanical forces, etc.
  • the fluid may be modified, for example, by subjecting it to higher temperature and nitrogen pressures, thereby increasing the amount of dissolved nitrogen in the fluid.
  • the plurality of different preparation chambers could be connected serially or in parallel before connecting to the growth chamber, or they could be connected separately to the growth chamber.
  • the present invention solves a problem of getting nitrogen through the flux to the crystal.
  • the problem of getting nitrogen through the flux to the crystal may be solved by using a thin layer, wherein the nitrogen goes through the thin layer.
  • nitrogen may already be in the flux (e.g., the fluid is pre-charged with nitrogen), thereby solving the problem of getting nitrogen through the flux to the crystal.
  • any coating (a thin or thick layer) may be used, for example.
  • the present invention may provide lower cost bulk Group-Ill nitride crystals, with better optical properties, and higher yields.
  • Other benefits of this production method may include the following:
  • this invention can be used in reverse, meaning, instead of supplying a high nitrogen containing flux to the crystal surface, a depleted flux layer may be provided, thereby encouraging the Group-III nitride material to be etched.
  • the facets which are formed during the etch may be controlled through modifying the melt and/or growth chamber conditions. This may be useful, for example, for performing an etch-back step prior to growth, or providing a surface roughening layer, which may be useful for enhanced light extraction when applied in optoelectronic devices such as LEDs. Additionally, the surface roughening layer may be useful as an anti-reflection coating as is, for example, useful for solar cell applications.
  • the surface roughening may be useful for reduction in dislocation density by performing a regrowth on it after etching back.
  • the flux method has shown that significantly enhanced growth rates in the nonpolar direction are possible and hence is a favorable method of growing large Group-III nitride crystals. Additionally, since it is possible to grow large crystals with significantly improved crystal quality and wafer curvature, as compared to Group-III nitride crystals grown using the HVPE (Hydride Vapor Phase Epitaxy) method, it may be financially desirable to use the flux method as a source of seeds for ammonothermal growth. Therefore, the use of Group-III nitride crystals grown using a flux method as seeds for a regrowth using the ammonothermal method also forms the basis of this invention.
  • HVPE Hydrodride Vapor Phase Epitaxy
  • the present invention also includes regrowing a Group-Ill nitride crystal using an ammonothermal method using as a seed the Group-Ill nitride crystal grown using the flux method.
  • the ammonothermal method is well known in the art, as described in, for example, U.S. Utility Patent Application Serial No. 13/128,083, filed on May 6, 2011, by Siddha Pimputkar, Derrick S. Kamber, James S. Speck and Shuji Nakamura, entitled "REACTOR DESIGNS FOR USE IN
  • the ammonothermal growth may use ammonia, ammonia and one or more other gases, or other nitrogen-containing gases, for example.
  • the ammonothermal method may be either acidic, basic, or neutral.
  • the acidic method utilizes one or more halogens containing materials, while the basic method utilizes one or more alkali metals containing materials.
  • the ammonothermally-grown Group -III nitride crystal may be used to fabricate Group-Ill nitride based electronic or optoelectronic devices, for example.
  • the Group- Ill nitride crystal may be A1N, GaN, InN, AlGaN, AlInN, InGaN, etc.
  • the Group-Ill nitride crystal may be at least 2 inches in length when measuring along one or more directions.
  • the Group-Ill nitride crystal may have layers with different compositions, and the Group-Ill nitride crystal may have layers with different structural, electronic, optical, and/or magnetic properties.
  • ammonothermal method does not need to be the as-grown Group-Ill nitride crystal resulting from the flux method. Instead, the Group-Ill nitride crystal resulting from the flux method may be modified before being used as a seed crystal in the ammonothermal method.
  • Modifications of interest include:
  • adding material to or removing additional from the seed using one or more techniques such as MOCVD, MBE, HVPE, sputtering, other deposition techniques, etching techniques, etc.
  • the present invention may enable price reduction in cost of producing substrates, and increased throughput and size of grown Group-Ill nitride crystals.
  • FIG. 3 is a flowchart that illustrates an exemplary process for performing the method of sodium flux growth followed by ammonothermal growth according to one embodiment of the present invention.
  • Block 300 represents the step of growing a Group-Ill nitride crystal using a sodium flux method (or obtaining a Group-Ill nitride crystal grown using a flux method).
  • Block 302 represents the end result of Block 300, namely a flux-grown Group- Ill nitride crystal.
  • Block 304 represents an (optional) step of modifying the crystal grown using the flux method prior to re-growth using the ammonothermal method. These modifications may include the following:
  • adding material to, or removing material from, the crystal, or surfaces of the crystal using one or more techniques, such as MOCVD, MBE, HVPE, sputtering, other deposition techniques, etching techniques, etc.
  • Block 306 represents the step of re-growing the Group-Ill nitride crystal ammonothermally, using the flux-grown Group-Ill nitride crystal of Block 302, as modified by Block 304, as a seed crystal for the ammonothermal re-growth.
  • Block 308 represents the end result of the process, namely an ammonothermally-grown Group-Ill nitride crystal.
  • These terms as used herein are intended to be broadly construed to include respective nitrides of the single species, Al, B, Ga, and In, as well as binary, ternary and quaternary compositions of such Group III metal species.
  • compositions and materials within the scope of the invention may further include quantities of dopants and/or other impurity materials and/or other inclusional materials.
  • This invention also covers the selection of particular crystal terminations and polarities of Group-Ill nitrides.
  • Many Group-Ill nitride devices are grown along a polar orientation, namely a c-plane ⁇ 0001 ⁇ of the crystal, although this results in an undesirable quantum-confined Stark effect (QCSE), due to the existence of strong piezoelectric and spontaneous polarizations.
  • QCSE quantum-confined Stark effect
  • One approach to decreasing polarization effects in Group-Ill nitride devices is to grow the devices along nonpolar or semipolar orientations of the crystal.
  • nonpolar includes the ⁇ 11-20 ⁇ planes, known collectively as a- planes, and the ⁇ 10-10 ⁇ planes, known collectively as m-planes. Such planes contain equal numbers of Group-Ill and Nitrogen atoms per plane and are charge-neutral. Subsequent nonpolar layers are equivalent to one another, so the bulk crystal will not be polarized along the growth direction.
  • semipolar can be used to refer to any plane that cannot be classified as c-plane, a-plane, or m-plane.
  • a semipolar plane would be any plane that has at least two nonzero h, i, or k Miller indices and a nonzero 1 Miller index. Subsequent semipolar layers are equivalent to one another, so the crystal will have reduced polarization along the growth direction.
  • braces When identifying orientations using Miller indices, the use of braces, ⁇ ⁇ , denotes a set of symmetry-equivalent planes, which are represented by the use of parentheses, ( ).
  • brackets, [ ] denotes a direction
  • brackets, ⁇ > denotes a set of symmetry-equivalent directions.
  • JP2004300024A2 published on October 28, 2004.
  • Kitaoka Method for Growing Group-Ill Nitride Crystal, Japanese Patent Publication No. JP2009051686A2, published on March 12, 2009.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

La présente invention concerne un procédé de croissance d'un cristal de nitrure du groupe III qui consiste à utiliser un flux de croissance dans lequel un fluide contenant au moins un métal du groupe III et au moins un métal alcalin est contenu dans un récipient et soumis à des conditions qui permettent d'ajouter de l'azote dans le fluide ou bien d'en enlever, ledit fluide étant mis en contact avec une ou plusieurs surfaces d'un grain sur lequel pousse le cristal de nitrure du groupe III. La présente invention concerne également un procédé d'utilisation du cristal de nitrure du groupe III qui a poussé au moyen du procédé reposant sur un flux, en tant que grain pour la recristallisation au moyen d'un procédé ammonothermal.
PCT/US2012/046756 2011-07-13 2012-07-13 Procédé de croissance d'un cristal de nitrure du groupe iii au moyen d'un flux et de l'utilisation du cristal de nitrure du groupe ii en tant que grain pour une recristallisation ammonothermale WO2013010117A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US201161507187P 2011-07-13 2011-07-13
US201161507170P 2011-07-13 2011-07-13
US61/507,170 2011-07-13
US61/507,187 2011-07-13

Publications (1)

Publication Number Publication Date
WO2013010117A1 true WO2013010117A1 (fr) 2013-01-17

Family

ID=47506586

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2012/046756 WO2013010117A1 (fr) 2011-07-13 2012-07-13 Procédé de croissance d'un cristal de nitrure du groupe iii au moyen d'un flux et de l'utilisation du cristal de nitrure du groupe ii en tant que grain pour une recristallisation ammonothermale

Country Status (1)

Country Link
WO (1) WO2013010117A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2014192904A1 (ja) * 2013-05-31 2017-02-23 日本碍子株式会社 窒化ガリウム結晶の育成方法、複合基板、発光素子の製造方法および溶解防止治具

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060191472A1 (en) * 2002-05-17 2006-08-31 Robert Dwilinski Bulk single crystal production facility employing supercritical ammonia
US20080156254A1 (en) * 2004-11-26 2008-07-03 Ammono Sp. Z O.O. Nitride Single Crystal Seeded Growth in Supercritical Ammonia with Alkali Metal Ion
US20080303032A1 (en) * 2004-06-11 2008-12-11 Robert Dwilinski Bulk Mono-Crystalline Gallium-Containing Nitride and Its Application
US20090092536A1 (en) * 2005-07-01 2009-04-09 Tohoku University Crystal production process using supercritical solvent, crystal growth apparatus, crystal and device
US20100104495A1 (en) * 2006-10-16 2010-04-29 Mitsubishi Chemical Corporation Method for producing nitride semiconductor, crystal growth rate increasing agent, single crystal nitride, wafer and device
US20100111808A1 (en) * 2008-11-05 2010-05-06 The Regents Of The University Of California Group-iii nitride monocrystal with improved crystal quality grown on an etched-back seed crystal and method of producing the same

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20060191472A1 (en) * 2002-05-17 2006-08-31 Robert Dwilinski Bulk single crystal production facility employing supercritical ammonia
US20080303032A1 (en) * 2004-06-11 2008-12-11 Robert Dwilinski Bulk Mono-Crystalline Gallium-Containing Nitride and Its Application
US20080156254A1 (en) * 2004-11-26 2008-07-03 Ammono Sp. Z O.O. Nitride Single Crystal Seeded Growth in Supercritical Ammonia with Alkali Metal Ion
US20090092536A1 (en) * 2005-07-01 2009-04-09 Tohoku University Crystal production process using supercritical solvent, crystal growth apparatus, crystal and device
US20100104495A1 (en) * 2006-10-16 2010-04-29 Mitsubishi Chemical Corporation Method for producing nitride semiconductor, crystal growth rate increasing agent, single crystal nitride, wafer and device
US20100111808A1 (en) * 2008-11-05 2010-05-06 The Regents Of The University Of California Group-iii nitride monocrystal with improved crystal quality grown on an etched-back seed crystal and method of producing the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPWO2014192904A1 (ja) * 2013-05-31 2017-02-23 日本碍子株式会社 窒化ガリウム結晶の育成方法、複合基板、発光素子の製造方法および溶解防止治具

Similar Documents

Publication Publication Date Title
Kucharski et al. Growth of bulk GaN crystals
KR100848380B1 (ko) 갈륨 함유 질화물의 벌크 단결정 및 그의 어플리케이션
Mori et al. Growth of bulk GaN crystals by Na flux method
JP2014099616A (ja) 有機金属化学気相成長法（ＭＯＣＶＤ）による平坦な無極性｛１−１００｝ｍ面窒化ガリウムの成長方法及び装置
JP2006509707A (ja) ガリウム含有窒化物のバルク単結晶を得るための改良されたプロセス
US8647967B2 (en) Hexagonal wurtzite type epitaxial layer possessing a low alkali-metal concentration and method of creating the same
EP3094766B1 (fr) Cristaux massifs de nitrure d'élément du groupe iii et procédé de fabrication correspondant
Konishi et al. Growth of Prismatic GaN Single Crystals with High Transparency on Small GaN Seed Crystals by Ca–Li-Added Na Flux Method
Kucharski et al. Ammonothermal and HVPE bulk growth of GaN
US20130015560A1 (en) Growth of bulk group-iii nitride crystals after coating them with a group-iii metal and an alkali metal
KR20110021961A (ko) 육방정 우르차이트 단결정
Wu et al. GaN substrate and GaN homo-epitaxy for LEDs: Progress and challenges
WO2013010117A1 (fr) Procédé de croissance d'un cristal de nitrure du groupe iii au moyen d'un flux et de l'utilisation du cristal de nitrure du groupe ii en tant que grain pour une recristallisation ammonothermale
Siche et al. Growth of bulk gan from gas phase
Boćkowski et al. Recent progress in crystal growth of bulk GaN
KR101335937B1 (ko) Ｌｌｏ 방식을 이용한 질화갈륨 웨이퍼 제조 방법
Nanishi et al. Plasma-excited MBE—Proposal and achievements through R&D of compound semiconductor materials and devices
Okada et al. Thermodynamic aspects of growth of AlGaN by high-temperature metal organic vapor phase epitaxy
US9279194B2 (en) Method of growing III-nitride crystal
JP5640427B2 (ja) Ｉｉｉ族窒化物半導体結晶の製造方法
US20130099180A1 (en) Use of alkaline-earth metals to reduce impurity incorporation into a group-iii nitride crystal grown using the ammonothermal method
Mori et al. Growth of bulk nitrides from a Na flux
US20130183225A1 (en) Crystal growth using non-thermal atmospheric pressure plasmas
US20130224100A1 (en) Electromagnetic mixing for nitride crystal growth
Imanishi et al. Growth of a High Quality GaN Wafer from Point Seeds by the Na-Flux Method

Legal Events

Date Code Title Description
121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 12811037

Country of ref document: EP

Kind code of ref document: A1

NENP Non-entry into the national phase

Ref country code: DE

122 Ep: pct application non-entry in european phase

Ref document number: 12811037

Country of ref document: EP

Kind code of ref document: A1