US3335084A - Method for producing homogeneous crystals of mixed semiconductive materials - Google Patents

Method for producing homogeneous crystals of mixed semiconductive materials Download PDF

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Publication number
US3335084A
US3335084A US352061A US35206164A US3335084A US 3335084 A US3335084 A US 3335084A US 352061 A US352061 A US 352061A US 35206164 A US35206164 A US 35206164A US 3335084 A US3335084 A US 3335084A
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charge
vessel
heating means
crystal
constituents
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US352061A
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Robert N Hall
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General Electric Co
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General Electric Co
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Priority to US352061A priority Critical patent/US3335084A/en
Priority to DEG43030A priority patent/DE1265126B/de
Priority to GB10898/65A priority patent/GB1044848A/en
Priority to FR9370A priority patent/FR1427444A/fr
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    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/003—Heating or cooling of the melt or the crystallised material
    • 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
    • C30B11/00—Single-crystal growth by normal freezing or freezing under temperature gradient, e.g. Bridgman-Stockbarger method
    • C30B11/007—Mechanisms for moving either the charge or the heater
    • 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
    • C30B13/00—Single-crystal growth by zone-melting; Refining by zone-melting

Definitions

  • This invention relates to the production of homogeneous crystals of mixed, mutually soluble, semiconductive materials.
  • the resultant crystal selectively exhibits certain desirable characteristics of the individual constituents to an extent that is controllable, as by regulating the relative proportions of the constituents in the resultant crystal.
  • Many characteristics of the resultant crystal can be controlled to selectively fall within a range defined by the extremes of two or more constituents considered individually.
  • a given characteristic is selected from a continuous range of optimize performance of the resultant semiconductive crystal in a given application, rather than resort to selection from the discrete group of characteristics offered by individual semiconductive materials.
  • Another object of my invention is to provide an efficient and economical process for growing and refining homogeneous crystals of mixed, mutually soluble, semiconductive materials.
  • Yet another object of my invention is to provide apparatus and process for efliciently and effectively producing homogeneous crystals of mixed semiconductive materials and conductivity-determining impurities wherein the relative concentrations of constituents are accurately and precisely controlled.
  • the constituents desired in a homogeneous crystal are sealed in a flask and reacted by heating to a temperature at which the mixture is in the liquid phase.
  • the constituents are then cooled in a furnace having a transverse thermal gradient until deposition of a solid occurs on the cooler side of the flask.
  • the flask is thereafter continuously and slowly rotated, While maintaining the average furnace temperature constant, causing one end of the deposit to be dissolved and the other end to be the site of crystalline redeposition.
  • the deposit is digested in this manner several times, until the liquid and solid phases reach their respective steady-state equilibrium conditions and thereafter continued until a crystal of the desired degree of homogeneity is obtained.
  • FIGURE 1 is a cross-sectional view of apparatus suitable for use in the practice of my invention
  • FIGURE 2 is a sectional top view of the flask in the apparatus of FIGURE 1;
  • FIGURE 3 is a view as in FIGURE 2, but schematically showing operation of the process.
  • the apparatus of FIGURES 1 and 2 comprises an outer support and housing 1 having a shaft 2 positioned vertically and journaled in the top of housing 1 for rotation about its vertical axis.
  • the lower portion of shaft 2, that projects into housing 1 includes an end portion 3 thereof having a concentric annular recess 4 formed therein that is adapted to receive and closely surround the neck portion 5 of a flask, or reaction vessel 6.
  • Vessel 6 is conveniently made of a suitable inert refractory material, as for example, quartz, aluminum nitride, or carbon.
  • a fastening device 7 is carried by the lower portion 3 of shaft 2 and projects inwardly into recess 4 to securely fix neck portion 5 with respect to shaft 2.
  • fastening device 7 also may be formed, conveniently, from fused quartz.
  • a ring gear 8 is securely fastened to shaft 2 externally of enclosure 1.
  • Gear 8 is engaged by drive gear 9 that is turned by motor 10 to effect rotation of shaft 2 and vessel 6 that is secured thereto by fastening device 7.
  • Additional vertical support for shaft 2 is provided by spider 11 that is secured to the upper extremity of shaft 2 and includes legs 12 that bear down upon the top surface of housing 1 along circular surface 13.
  • Heating means for the contents of vessel 6 include a thin walled cylinder 14 closely surrounding the outer periphery of vessel 6 and having imbedded therein a helical winding comprising a plurality of turns of resistance wire 15.
  • Cylinder 14 is fabricated from a refractory insulating material and is supported atop a lower platform 16 that in turn rests upon the inner floor of housing 1.
  • Support 16 includes a duct 17 that communicates with a passage 18 formed in an otherwise solid cylindrical member 19 that fits tightly within cylinder 14 and includes an upper surface 20 that is shaped to receive the lower portion of vessel 6.
  • Means for circulating the atmosphere within housing 1 into duct 17 is illustrated schematically as including a motor 21 driving a fan blade 31 disposed near the entrance 22 of duct 17. The cooling atmosphere is directed by passage 18 toward one peripheral segment of vessel 6.
  • the efiiciency of the heating means is increased by providing annular insulating blocks 23 and 24, conveniently made from refactory heat insulating material, externally of and closely surrounding cylinder 14. Further means for increasing the efficiency of the heating means includes a bat of refractory insulating material 25 inside cylinder 14 and covering the top of vessel 6.
  • the insulating material is, conveniently, quartz wool, in order to provide the required porosity to release the cooling atmosphere delivered from passage 18.
  • stirring means is provided and takes the form of an annular yoke 26 having integral pole pieces 27 extending inwardly therefrom and terminating adjacent the outer periphery of cylinder 14 and in vertical alignment with the largest diameter portion of vessel 6.
  • a plurality of turns 28 of electrically conducting, insulated wire on each of poles 26 comprise the electric circuit necessary to cause a magnetomotive force sufficient to establish magnetic flux linking the various poles and including as a portion of the path the contents of vessel 6.
  • Yoke 26 can, for example, take the form of a conventional induction motor stator and electrical connections sufiicient to provide a revolving magnetic field in the vicinity of vessel 6 are WGll-kIlOWIl and can be obtained easily from most text books which treat the subject of alternating current machinery.
  • My invention is used to greatest advantage for growing and refining homogeneous mixed semiconductive crystals having concentrations of constituents differing appreciably from the concentrations of constituents in the melt from which the crystal is grown. For this reason, my invention is particularly useful for providing mixed, or solid solution, homogeneous semiconductive crystals in various systems including, indium antimonide-gallium antimonide, indium *antimonide-aluminum antimonide, gallium antimonide-aluminum antimonide, indium arsenide-gallium arsenide, indium arsenide-indium phosphide, and gallium arsenide gallium phosphide.
  • My invention is also advantageously employed to grow and refine various mixed semiconductive crystals from the II-VI compounds, as for example, cadmium telluride-cadmium sulfide, zinc telluridezinc sulfide.
  • Other systems include germanium-silicon crystals grown from a solution of tin or gold having germanium and silicon introduced therein, or quaternary solid solution systems such as gallium-indium-arsenicphosphorus and gallium-indiumarsenic-antimony.
  • the mixed semiconductive crystal system consisting essentially of gallium arsenide-gallium phosphi-de, with suitable acceptor or donor impurities therefor in some cases. This system is typical of the complex-compound semiconductive materials produced in homogeneous crystalline form, in accord with my invention.
  • vessel 6 there is enclosed a charge, or mixture of reaction products, that is partially in the liquid phase and partially in the solid phase.
  • a portion of a given change deposits as a solid and another portion is in the liquid state.
  • the relative concentrations of constituents in the solid and liquid phases correspond to the proportions given by what is known in the art as a phase diagram of the system.
  • the above described heating means for heating the charge within vessel 6, is adapted to establish within the charge a temperature distribution with a transverse thermal gradient such that substantially all, and preferably greater than 80 percent, of the change is in the liquid phase in order to encourage homogeneity and thorough mixing of the liquid constituents.
  • the heating means is preferably adapted to establish a temperature gradient having a coolest temperature adjacent one peripheral segment of vessel 6, in order to promote deposition of the solid portion and growth of a crystal thereat. Freezing of the latter portion occurs to a solid state body, represented as crystalline body 29 shown growing on the side of one peripheral segment of vessel6 that is the coolest segment, due to the cooling atmosphere from passage 18.
  • the charge is selected to contain a predominant concentration of gallium that serves as a solvent into which arsenic and phosphorus are introduced and, preferably, the upper extremity, or tip 34, of neck portion 5 of vessel 6 is sealed.
  • phosphorus and arsenic can be introduced, as gaseous reaction partners, continuously during the growing and refining process into a solvent of gallium by providing a suitable gaseous carrier therefor such as hydrogen or argon.
  • FIGURES 2 and 3 which are horizontal cross-sectional views of vessel 6 of FIGURE 1 taken along section lines 22, illustrate the method of operation of the specific apparatus shown in FIGURE 1.
  • the heating means has been energized for sufficient time to establish the temperature gradient described above, a deposit of the same materials as the molten mass is formed on the peripheral segment of vessel 6 wherein the lower temperature is maintained. The remainder of the charge 30 is in the liquid state.
  • seed crystal 29 is continuously displaced relative to the heating means, as by continuous rotation of vessel 6 about its vertical axis by motor 10, as seen in FIGURE 1.
  • motor 10 as seen in FIGURE 1.
  • the displacement of crystalline body 29 is clockwise, relative to the heating means, as shown more particularly in FIG- URE 3, there is simultaneously established a freezing interface 32 and melting interface 33 in body 29 at respective opposite ends thereof.
  • body 29 With any fixed displacement of body 29 relative to the heating means, the melting and freezing occurs until body 29 achieves the same equilibrium position (shown in FIGURE 2) relative to the heating means that it occupied prior to the displacement.
  • body 29 may be considered to creep around the peripheral surface of vessel 6 in the direction opposite to small angular displacements thereof, about a vertical axis, relative to the heating means.
  • the freezing and melting interfaces reverse positions at the ends of body 29 to effect the described movement of body 29 back to the equilibrium position.
  • the crystalline body is continually displaced relative to the heating means, as by means of motor 10 in FIG- URE 1, that is adapted to provide continuous rotation of vessel 6 relative to the heating means.
  • the particular direction of rotation selected is immaterial, and, of course, in some applications it is equally advantageous to rotate the heating means while maintaining the reaction vessel in a fixed position.
  • Circulation, or stirring, of the portion of the charge that is in the liquid phase is advantageously used to accelerate diffusion within the liquid phase to promote a more uniform concentration, resulting in increased homogeneity within body 29, and permitting more rapid growth.
  • the circulation, or rotation is in the direction from the melting interface to the freezing interface, as shown in FIGURE 3, in order to provide maximum opportunity for diffusion, since the longitudinal dimension of body 29 is norm-ally small relative to, and usually less than A, the circumference of vessel 6 at that section wherein crystal growth occurs.
  • a further effect of rotating the liquefied portion of charge 30 is to shift the equilibrium position of crystal 29, relative to the heating means, by a predetermined fixed angular displacement that is in the same direction as rotation.
  • a homogeneous crystal constituted of 35 mol percent gallium phosphide remainder essentially gallium arsenide, having a donor concentration of 10 cm.- is produced as follows.
  • a charge constituted of 42.8 grams gallium, 6.27 grams arsenic, 0.915 gram phosphorus, and 0.024 gram tellurium (donor impurity) is provided in a quartz flask, as shown in FIG- URE 1, having a bulb diameter of 1% inches. The flask is then sealed in an inert atmosphere and heated to a temperature of about 1050 C. to react the constituents.
  • the most desirable flask rotation rates fall within the range of from /2 to /s revolution per day with flasks of the above-mentioned bulb diameter.
  • the rate is advantageously selected to be less with larger diameter flasks and vice versa.
  • the duration of time during which the process is carried out varies directly with the desired degree of homogeneity required in the crystal.
  • a large high purity homogeneous gallium phosphide crystal is produced in accord with my invention as follows: 90 grams of gallium are placed in an open quartz flask, 5 centimeters in diameter, and supported on an insulating slab. Three pole pieces providing a three-phase rotating magnetic field are disposed substantially symmetrically about the outer lower peripheral surface of the flask. Approximate distance between pole pieces is about 2 /2 inches and each core is about A. square inch in cross section. The cores each contained 900 turns of conductive wire and the current measured was about 2 amperes, resulting in an electromotive force of approximately 1800 ampere-turns. In the presence of this field the gallium rotated about 20 rounds per minute.
  • a homogeneous crystal consisting essentially of 60 mol percent gallium arsenide, remainder indium arsenide is advantageously produced in accord with the previous example by introducing 30 grams of gallium, 60 grams of indium and 20 grams of arsenic into the flask. However, in this case, the flask is sealed, heated to an average temperature of 760 C. and a rotation of /2 revolution per day continued for 4 days in the presence of the magnetic stirring.
  • a large single homogeneous crystal constituted of mutually soluable constituents is produced in accord with my invention by a continuous regrowing technique from a supersaturated solution. This is accomplished by slowly rotating the reaction vessel containing the constituents relative to heating means that provides a thermal gradient. Preferably, the melt is rotated, or circulated, but at a much faster rate than the vessel is turned. The crystal is constrained to a substantially constant spatial relationship with respect to the heating means. Continuous regrowth by freezing and melting is continued until equilibrium conditions, with respect to relative concentrations, have been established.
  • This technique is particularly suitable for producing large homogeneous crystals constituted of mixtures of complex semiconductive compounds and readily lends itself to introduction of desired impurities.
  • a process for producing a homogeneous semiconductive crystal constituted essentially of predetermined mutually soluble constituents comprises:
  • step of displacing said body relative to said heating means comprises rotating said vessel relative to said heating means, said circulation being in the same angular direction as said vessel rotates relative to said heating means.
  • a process for growing and refining a homogeneous mixed semiconductive crystal constituted essentially of predetermined mutually soluble semiconductive constituents which process comprises: i
  • a process for growing and refining a homogeneous mixed semiconductive crystal constituted essentially of predetermined mutually soluble constituents which process comprises:
  • step of con- References Cited tinuously displacing said body relative to said heating UNITED STATES PATENTS means comprises rotating said vessel relative to said heat- 2 739 045 3/1956 Pfann ing means, said circulation being in the same angular direction as said vessel rotates relative to said heating 5 TOBIAS LEVOW, Primary Examiner means. R. D. EDMONDS, Assistant Examiner.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Liquid Deposition Of Substances Of Which Semiconductor Devices Are Composed (AREA)
US352061A 1964-03-16 1964-03-16 Method for producing homogeneous crystals of mixed semiconductive materials Expired - Lifetime US3335084A (en)

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Application Number Priority Date Filing Date Title
US352061A US3335084A (en) 1964-03-16 1964-03-16 Method for producing homogeneous crystals of mixed semiconductive materials
DEG43030A DE1265126B (de) 1964-03-16 1965-03-09 Verfahren zum Herstellen homogener Mischkristalle aus ineinander loeslichen halbleitenden Verbindungen
GB10898/65A GB1044848A (en) 1964-03-16 1965-03-15 Method for producing homogeneous crystals of mixed semiconductive materials
FR9370A FR1427444A (fr) 1964-03-16 1965-03-16 Procédés de fabrication de cristaux homogènes composés d'un mélange de matériaux semiconducteurs

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Cited By (38)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3464812A (en) * 1966-03-29 1969-09-02 Massachusetts Inst Technology Process for making solids and products thereof
US3468363A (en) * 1967-10-10 1969-09-23 Texas Instruments Inc Method of producing homogeneous ingots of mercury cadmium telluride
US3537912A (en) * 1968-03-20 1970-11-03 Gen Electric Method of growing chalcogenide pseudo-binary crystals of uniform composition
US3656944A (en) * 1970-02-16 1972-04-18 Texas Instruments Inc Method of producing homogeneous ingots of a metallic alloy
US3873463A (en) * 1972-02-23 1975-03-25 Philips Corp Method of and device for manufacturing substituted single crystals
US3898051A (en) * 1973-12-28 1975-08-05 Crystal Syst Crystal growing
US3957693A (en) * 1968-03-19 1976-05-18 Siemens Aktiengesellschaft Process for producing selenium homogeneously doped with tellurium
US4373988A (en) * 1974-09-20 1983-02-15 Max-Planck-Gesellschaft Zur Forderung Der Wissenschaften E.V. Method of growing epitaxial layers from a liquid phase
WO2009149254A1 (en) * 2008-06-05 2009-12-10 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US20090301387A1 (en) * 2008-06-05 2009-12-10 Soraa Inc. High pressure apparatus and method for nitride crystal growth
US20090320744A1 (en) * 2008-06-18 2009-12-31 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US20100003492A1 (en) * 2008-07-07 2010-01-07 Soraa, Inc. High quality large area bulk non-polar or semipolar gallium based substrates and methods
US20100025656A1 (en) * 2008-08-04 2010-02-04 Soraa, Inc. White light devices using non-polar or semipolar gallium containing materials and phosphors
US20100031874A1 (en) * 2008-08-07 2010-02-11 Soraa, Inc. Process and apparatus for growing a crystalline gallium-containing nitride using an azide mineralizer
US20100031876A1 (en) * 2008-08-07 2010-02-11 Soraa,Inc. Process and apparatus for large-scale manufacturing of bulk monocrystalline gallium-containing nitride
US8148801B2 (en) 2008-08-25 2012-04-03 Soraa, Inc. Nitride crystal with removable surface layer and methods of manufacture
US8284810B1 (en) 2008-08-04 2012-10-09 Soraa, Inc. Solid state laser device using a selected crystal orientation in non-polar or semi-polar GaN containing materials and methods
US8299473B1 (en) 2009-04-07 2012-10-30 Soraa, Inc. Polarized white light devices using non-polar or semipolar gallium containing materials and transparent phosphors
US8306081B1 (en) 2009-05-27 2012-11-06 Soraa, Inc. High indium containing InGaN substrates for long wavelength optical devices
US20120297580A1 (en) * 2009-10-21 2012-11-29 Fabrizio Dughiero Method and device for obtaining a multicrystalline semiconductor material, in particular silicon
US8354679B1 (en) 2008-10-02 2013-01-15 Soraa, Inc. Microcavity light emitting diode method of manufacture
US8430958B2 (en) 2008-08-07 2013-04-30 Soraa, Inc. Apparatus and method for seed crystal utilization in large-scale manufacturing of gallium nitride
US8435347B2 (en) 2009-09-29 2013-05-07 Soraa, Inc. High pressure apparatus with stackable rings
US8455894B1 (en) 2008-10-17 2013-06-04 Soraa, Inc. Photonic-crystal light emitting diode and method of manufacture
US8461071B2 (en) 2008-12-12 2013-06-11 Soraa, Inc. Polycrystalline group III metal nitride with getter and method of making
US8482104B2 (en) 2012-01-09 2013-07-09 Soraa, Inc. Method for growth of indium-containing nitride films
US8729559B2 (en) 2010-10-13 2014-05-20 Soraa, Inc. Method of making bulk InGaN substrates and devices thereon
US8786053B2 (en) 2011-01-24 2014-07-22 Soraa, Inc. Gallium-nitride-on-handle substrate materials and devices and method of manufacture
US8871024B2 (en) 2008-06-05 2014-10-28 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US8878230B2 (en) 2010-03-11 2014-11-04 Soraa, Inc. Semi-insulating group III metal nitride and method of manufacture
US8979999B2 (en) 2008-08-07 2015-03-17 Soraa, Inc. Process for large-scale ammonothermal manufacturing of gallium nitride boules
US8987156B2 (en) 2008-12-12 2015-03-24 Soraa, Inc. Polycrystalline group III metal nitride with getter and method of making
US9157167B1 (en) 2008-06-05 2015-10-13 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US9175418B2 (en) 2009-10-09 2015-11-03 Soraa, Inc. Method for synthesis of high quality large area bulk gallium based crystals
US9543392B1 (en) 2008-12-12 2017-01-10 Soraa, Inc. Transparent group III metal nitride and method of manufacture
US9564320B2 (en) 2010-06-18 2017-02-07 Soraa, Inc. Large area nitride crystal and method for making it
US10036099B2 (en) 2008-08-07 2018-07-31 Slt Technologies, Inc. Process for large-scale ammonothermal manufacturing of gallium nitride boules
USRE47114E1 (en) 2008-12-12 2018-11-06 Slt Technologies, Inc. Polycrystalline group III metal nitride with getter and method of making

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Patent Citations (1)

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Cited By (51)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3464812A (en) * 1966-03-29 1969-09-02 Massachusetts Inst Technology Process for making solids and products thereof
US3468363A (en) * 1967-10-10 1969-09-23 Texas Instruments Inc Method of producing homogeneous ingots of mercury cadmium telluride
US3957693A (en) * 1968-03-19 1976-05-18 Siemens Aktiengesellschaft Process for producing selenium homogeneously doped with tellurium
US3537912A (en) * 1968-03-20 1970-11-03 Gen Electric Method of growing chalcogenide pseudo-binary crystals of uniform composition
US3656944A (en) * 1970-02-16 1972-04-18 Texas Instruments Inc Method of producing homogeneous ingots of a metallic alloy
US3873463A (en) * 1972-02-23 1975-03-25 Philips Corp Method of and device for manufacturing substituted single crystals
US3898051A (en) * 1973-12-28 1975-08-05 Crystal Syst Crystal growing
US4373988A (en) * 1974-09-20 1983-02-15 Max-Planck-Gesellschaft Zur Forderung Der Wissenschaften E.V. Method of growing epitaxial layers from a liquid phase
US8986447B2 (en) 2008-06-05 2015-03-24 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US8871024B2 (en) 2008-06-05 2014-10-28 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US20090301387A1 (en) * 2008-06-05 2009-12-10 Soraa Inc. High pressure apparatus and method for nitride crystal growth
WO2009149254A1 (en) * 2008-06-05 2009-12-10 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US9157167B1 (en) 2008-06-05 2015-10-13 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US8097081B2 (en) 2008-06-05 2012-01-17 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US20090320744A1 (en) * 2008-06-18 2009-12-31 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US8303710B2 (en) 2008-06-18 2012-11-06 Soraa, Inc. High pressure apparatus and method for nitride crystal growth
US20100003492A1 (en) * 2008-07-07 2010-01-07 Soraa, Inc. High quality large area bulk non-polar or semipolar gallium based substrates and methods
US20100025656A1 (en) * 2008-08-04 2010-02-04 Soraa, Inc. White light devices using non-polar or semipolar gallium containing materials and phosphors
US8956894B2 (en) 2008-08-04 2015-02-17 Soraa, Inc. White light devices using non-polar or semipolar gallium containing materials and phosphors
US8124996B2 (en) 2008-08-04 2012-02-28 Soraa, Inc. White light devices using non-polar or semipolar gallium containing materials and phosphors
US8284810B1 (en) 2008-08-04 2012-10-09 Soraa, Inc. Solid state laser device using a selected crystal orientation in non-polar or semi-polar GaN containing materials and methods
US8558265B2 (en) 2008-08-04 2013-10-15 Soraa, Inc. White light devices using non-polar or semipolar gallium containing materials and phosphors
USRE47711E1 (en) 2008-08-04 2019-11-05 Soraa, Inc. White light devices using non-polar or semipolar gallium containing materials and phosphors
US8323405B2 (en) 2008-08-07 2012-12-04 Soraa, Inc. Process and apparatus for growing a crystalline gallium-containing nitride using an azide mineralizer
US20100031874A1 (en) * 2008-08-07 2010-02-11 Soraa, Inc. Process and apparatus for growing a crystalline gallium-containing nitride using an azide mineralizer
US8430958B2 (en) 2008-08-07 2013-04-30 Soraa, Inc. Apparatus and method for seed crystal utilization in large-scale manufacturing of gallium nitride
US10036099B2 (en) 2008-08-07 2018-07-31 Slt Technologies, Inc. Process for large-scale ammonothermal manufacturing of gallium nitride boules
US8444765B2 (en) 2008-08-07 2013-05-21 Soraa, Inc. Process and apparatus for large-scale manufacturing of bulk monocrystalline gallium-containing nitride
US20100031876A1 (en) * 2008-08-07 2010-02-11 Soraa,Inc. Process and apparatus for large-scale manufacturing of bulk monocrystalline gallium-containing nitride
US8021481B2 (en) 2008-08-07 2011-09-20 Soraa, Inc. Process and apparatus for large-scale manufacturing of bulk monocrystalline gallium-containing nitride
US8979999B2 (en) 2008-08-07 2015-03-17 Soraa, Inc. Process for large-scale ammonothermal manufacturing of gallium nitride boules
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US8329511B2 (en) * 2008-08-25 2012-12-11 Soraa, Inc. Nitride crystal with removable surface layer and methods of manufacture
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DE1265126B (de) 1968-04-04

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