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WO2015179852A1 - Cristaux massifs de nitrure du groupe iii et leur procédé de fabrication - Google Patents

Cristaux massifs de nitrure du groupe iii et leur procédé de fabrication Download PDF

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Publication number
WO2015179852A1
WO2015179852A1 PCT/US2015/032330 US2015032330W WO2015179852A1 WO 2015179852 A1 WO2015179852 A1 WO 2015179852A1 US 2015032330 W US2015032330 W US 2015032330W WO 2015179852 A1 WO2015179852 A1 WO 2015179852A1
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Prior art keywords
crystal
seed crystal
group iii
bulk
seed
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Ceased
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English (en)
Inventor
Tadao Hashimoto
Edward Letts
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Seoul Semiconductor Co Ltd
SixPoint Materials Inc
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Seoul Semiconductor Co Ltd
SixPoint Materials Inc
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Priority to EP15727806.0A priority Critical patent/EP3146093A1/fr
Publication of WO2015179852A1 publication Critical patent/WO2015179852A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • 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
    • C30B29/406—Gallium nitride

Definitions

  • the invention relates to a bulk crystal of semiconductor material used to produce semiconductor wafers for various devices including optoelectronic devices such as light emitting diodes (LEDs) and laser diodes (LDs), and electronic devices such as transistors. More specifically, the invention provides a bulk crystal of group III nitride such as gallium nitride. The invention also provides various methods of making these crystals.
  • Gallium nitride (GaN) and its related group III nitride alloys are the key material for various optoelectronic and electronic devices such as LEDs, LDs, microwave power transistors, and solar-blind photo detectors.
  • LEDs are widely used in displays, indicators, general illuminations, and LDs are used in data storage disk drives.
  • the majority of these devices are grown epitaxially on heterogeneous substrates, such as sapphire and silicon carbide because GaN substrates are extremely expensive compared to these heteroepitaxial substrates.
  • the heteroepitaxial growth of group III nitride causes highly defected or even cracked films, which hinder the realization of high-end optical and electronic devices, such as high-brightness LEDs for general lighting or high-power microwave transistors.
  • HVPE hydride vapor phase epitaxy
  • GaN substrates having dislocation density less than 10 5 cm "2 can be obtained by ammonothermal growth. Since the ammonothermal method can produce a true bulk crystal, one can grow one or more thick crystals and slice them to produce GaN wafers. We have been developing bulk crystals of GaN by the ammonothermal method.
  • this invention is intended to obtain crack- free bulk group III nitride crystals using any bulk growth method, such as growth in supercritical ammonia or from a melt of group III metals.
  • the invention provides a bulk crystal of group III nitride having a thickness of more than 1 mm without cracking above the sides of a seed crystal.
  • This bulk group III nitride crystal is expressed as Ga x iAlyiIni-xi- y iN (0 ⁇ xl ⁇ l, 0 ⁇ xl+yl ⁇ l) and the seed crystal is expressed as Ga X 2Aly2lni-x2- y 2 (0 ⁇ x2 ⁇ l, 0 ⁇ x2+y2 ⁇ l).
  • the bulk crystal of group III nitride can be grown in supercritical ammonia or a melt of group III metal using at least one seed crystal having basal planes of one orientation and all sidewalls of one or more other orientations that are slow-growing compared to the basal plane.
  • the group III nitride seed crystal may have c-orientation basal planes and all sidewalls may be prismatic crystal faces with m-plane orientation. By exposing only c-planes and m-planes, cracks originating from the sides of the seed crystal are avoided.
  • the invention also provides a new seed crystal that can be used to grow bulk group III nitride.
  • the seed crystal is expressed as Ga X 2Aly2lni-x2- y 2 (0 ⁇ x2 ⁇ l, 0 ⁇ x2+y2 ⁇ l) and has one or more of the following traits in any combination: (A) the seed crystal may have (1) exposed basal planes on which most growth occurs and (2) exposed sidewalls that grow slowly compared to the basal planes; (B) each of the sidewalls of a seed crystal may grow at a rate that is less than 20 ⁇ per day, while optionally a face essentially parallel to a basal plane may grow at a rate that is greater than 20 ⁇ per day; (C) all sidewalls may grow at a rate that is less than 20 % of the rate at which a face grows; (D) the basal planes of the seed crystal may be c-planes, and the sidewalls of the seed crystal may all be m-plane; (E) the seed crystal may
  • the seed crystal may have a hexagonal shape, a triangular shape, or a shape of a rhombus having no right angles. Sidewalls may be prismatic sidewalls of the seed crystal.
  • the invention provides new methods of making a seed crystal as well as new methods of making a bulk crystal of group III nitride as well as wafers, optical devices, and semiconductor devices. The following methods may be used alone or in any combination.
  • a seed crystal as described above can be made by growing group III nitride having the formula Gax2Al y 2lni-x2- y 2 (0 ⁇ x2 ⁇ l, 0 ⁇ x2+y2 ⁇ l) by vapor-phase epitaxy
  • HVPE molecular beam epitaxy
  • MBE molecular beam epitaxy
  • MOVPE metal organic vapor-phase epitaxy
  • ammonothermal growth for example, and removing a portion of the group III nitride to form a seed that has a first face, a second face, and a plurality of side-walls extending between the faces at the faces' periphery, with all of the sidewalls being slow-growing as compared to growth on the first face.
  • the sidewalls may each have a length that is within +/- 10% of the average length of the sidewalls.
  • a seed crystal may be made by forming a raw seed crystal from group III nitride using HVPE, MBE, or MOVPE, and shaping this raw seed crystal to have slow-growing sidewalls and a faster-growing face.
  • the method may further comprise placing two essentially identical group III nitride crystals together such that Ga-polar faces touch one another to form a new seed prior to making a bulk crystal.
  • the method of making a bulk crystal may comprise making a seed crystal from group III nitride formed using HVPE, MBE, or MOVPE, shaping this group III nitride to have slow-growing sidewalls and a faster-growing face, and using the seed crystal in a bulk growth process such as ammonothermal growth or flux growth to form the bulk crystal.
  • the invention also provides a new ingot or bulk crystal of group III nitride.
  • the bulk crystal is expressed as Ga x iAlyiIni-xi- y iN (0 ⁇ xl ⁇ l, 0 ⁇ xl+yl ⁇ l).
  • the bulk crystal has one or more of the following traits in any combination: (a) the bulk crystal has a thickness greater than 1 mm without any cracks in the crystal above the seed's sidewall edge (in the area bridging the sidewall and new growth on the sidewall of the seed); (b) the bulk crystal has a thickness greater than 1 mm and has fewer cracks in the crystal above the original seed's edge than a comparative bulk crystal grown under otherwise identical conditions but grown using a square seed having the same surface area as the original seed but having m-plane and a-plane walls.
  • the invention provides new wafers of group III nitride and
  • FIG. 1 is a schematic drawing of the top view of a bulk crystal of group III nitride in a conventional method.
  • FIG. 2 is a schematic drawing of the top view of a bulk crystal of group III nitride in this invention.
  • the bulk crystal of the present invention is typically sliced to produce group III nitride wafers suitable for fabricating various optoelectronic and electronic devices such as LEDs, LD, transistors, and photodetectors by known techniques.
  • group III nitride alloys i.e. alloys of GaN, A1N and InN.
  • the group III nitride alloys are typically expressed as Ga x AlyIni-x- y N (0 ⁇ x ⁇ l, 0 ⁇ x+y ⁇ l). Since the group III metallic elements (i.e. Al, Ga, In) shows similar chemical characteristics, nitrides of these group III elements makes alloys or solid solution. In addition, crystal growth nature of these group III nitrides are quite similar.
  • the device Due to limited availability and high cost of single crystalline substrates of group III nitride, these devices have been fabricated on so-called heteroepitaxial substrates such as sapphire and silicon carbide. Since the heteroepitaxial substrates are chemically and physically different from the group III nitride, the device typically has a high density of dislocations (10 8 ⁇ 10 10 cm 2 ) generated at the interface between the heteroepitaxial substrate and the device layer. Such dislocations deteriorate performance and reliability of devices, thus substrates composed of crystalline group III nitride such as GaN and A1N are favorable.
  • ammonothermal growth which utilizes supercritical ammonia, has been developed.
  • the ammonothermal method can produce GaN substrates with dislocation density less than 10 5 cm 2 .
  • One advantage of the ammonothermal method is that bulk crystals having a thickness larger than 1 mm can be grown.
  • the ammonothermal method can also be used to grow crystals having various dopants such as donors (i.e. electron), acceptors (i.e. hole) or magnetic dopants.
  • donors i.e. electron
  • acceptors i.e. hole
  • magnetic dopants such as magnetic dopants
  • the current invention provides a method of making a bulk crystal of group III nitride in which a single-crystal seed has (1) exposed basal planes on which most growth occurs and (2) exposed sidewalls that grow slowly compared to the basal planes.
  • the exposed surfaces may optionally have a small miscut angle (e.g. within approximately +/- 5 degrees) from the crystallographic planes, but the miscut is not sufficiently large to cause rapid growth on the sidewalls.
  • the single-crystal seed may be grown by hydride vapor-phase epitaxy (HVPE), molecular beam epitaxy (MBE), metal organic vapor-phase epitaxy (MOVPE), ammonothermal growth, or other method.
  • the sidewalls of this seed crystal grow more slowly than the face or basal plane grows when forming a bulk crystal of group III nitride using the seed. All sidewalls may grow at a rate that is less than 20% of the rate at which a face grows. All sidewalls instead or additionally may grow at a rate that is less than 20 ⁇ per day in another instance, while optionally a face essentially parallel to a basal plane may grow at a rate that is greater than 20 ⁇ per day.
  • the seed crystal may have c-planes (i.e. ⁇ 0001 ⁇ planes) as basal planes and only m-planes (i.e. ⁇ 10-10 ⁇ planes) as sidewalls.
  • the exposed surface optionally has a small miscut angle (within approximately +/- 5 degrees) from the crystallographic planes.
  • the m-plane sidewalls may grow at a rate that is less than 20% of the rate at which a c-plane face grows. Instead or additionally, the m-plane sidewalls may grow at a rate that is less than 20 ⁇ per day, while optionally a face essentially parallel to a basal c-plane may grow at a rate that is greater than 20 ⁇ per day.
  • freestanding GaN wafers fabricated by HVPE are commonly used as a seed crystal.
  • the free- standing GaN wafers are typically supplied in a round shape or a square shape.
  • the seed shape is either a round shape or a square shape. If smaller pieces are cut from the whole piece, the shape is commonly square or rectangular.
  • This type of seed crystal has c-planes, m-planes, and a-planes (i.e. ⁇ 1 1-20 ⁇ planes) or other semipolar planes (e.g. ⁇ 1 1-21 ⁇ planes).
  • the current invention utilizes a seed crystal which exposes only slow-growing sidewalls such as m-plane sidewalls in addition to fast growing basal planes such as c-oriented basal planes as shown in Figure 2.
  • the grown crystal (22 in Figure 2) does not expand much toward the lateral direction from the seed crystal (21 in Figure 1), and crack generation is greatly reduced.
  • the current invention minimizes the number of different crystallographic planes exposed for crystal growth.
  • the seed crystal in one instance has only c-planes and m-planes exposed, with c-planes forming the basal planes and m-planes forming the sidewalls.
  • two seeds are attached together on Ga-polar c-planes to expose only N-polar c-planes and m-planes. This way, it is possible to reduce/eliminate cracks in bulk group III nitride crystal.
  • This invention is particularly effective when the seed crystal is grown by HVPE, although the seed crystal can be grown by other methods such as an ammonothermal method, MOVPE, and MBE.
  • MOVPE ammonothermal method
  • MOVPE metal-organic chemical vapor deposition
  • MBE metal-organic chemical vapor deposition
  • Single crystalline GaN seed crystal having a basal plane of c-plane is prepared with HVPE.
  • the thickness of the GaN seed is approximately 430 microns.
  • the HVPE GaN seed is made square shape exposing m-plane and a-plane sidewalls.
  • GaN crystal is grown on the seed crystal by ammonothermal method using a high-pressure reactor made of Ni-Cr superalloy.
  • the inner room of the high-pressure reactor is divided into lower part and the upper part with baffle plates. Approximately 15 g of polycrystalline GaN is used as a nutrient and approximately 3.1 g of sodium is used as a mineralizer. Mineralizer and the seed crystal are placed in the lower part of the high-pressure reactor and the nutrient is placed in the upper part of the high-pressure reactor. Then, the high-pressure reactor is sealed, pumped to a vacuum and filled with anhydrous liquid ammonia. The volumetric ammonia fill factor is approximately 53%.
  • the high-pressure reactor is heated at about 510 ⁇ 520°C to allow crystal growth of GaN on the seed. After sufficient amount of time, the ammonia is released and the high- pressure reactor is cooled.
  • the resultant bulk GaN crystal has a thickness of approximately 5 mm.
  • the full-width half maximum (FWHM) of the X-ray 002 peak is less than 150 arcsec, showing a good microstructure.
  • the crystal has yellowish transparent color.
  • the crystal as observed with an optical microscope has small cracks as shown in Fig. 1 , 13 A and also has a large crack as shown in Fig. 1, 13B. This result demonstrates that cracks in the bulk GaN crystal tend to originate from the interface between the grown crystal and non-m- plane edge of the seed crystal.
  • Example 2
  • Two single crystalline GaN seed crystals having a basal plane of c-plane are prepared with HVPE.
  • the HVPE GaN seed is made hexagonal shape exposing only m-plane sidewalls.
  • the thickness of the seed crystals is approximately 430 microns.
  • the length of each side is approximately 1 cm with +/- 10% error.
  • the orientation of the sidewall is m-plane with unintentional miscut angle within 5 degrees.
  • the two seed crystals are attached together on Ga-polar c-plane surfaces to make a piece which only exposes N-polar c-planes and m-plane sidewalls.
  • a bulk GaN crystal is grown on the hexagonal seed crystals by ammonothermal method using a high-pressure reactor made of Ni-Cr superalloy.
  • a hexagonal shape bulk GaN having thickness approximately 5 mm is grown.
  • the yellowish transparent crystal does not have small cracks and does not have large cracks that originate above the interface between the seed sidewalls and the grown crystal.
  • the X-ray FWHM is less than 150 arcsec, representing a good microstructure.
  • Single crystalline GaN seed crystal having a basal plane of c-plane is prepared with HVPE.
  • the HVPE GaN seed is made hexagonal shape exposing only m-plane sidewalls.
  • the thickness of the seed crystal was approximately 430 microns. Since dicing creates rougher sidewall than cleavage, the seed crystal was immersed in concentrated phosphoric acid maintained at approximately 120 °C for 30 minutes to remove surface or subsurface damage caused by dicing.
  • the length of each side is approximately 1 cm with +/- 10% error.
  • the orientation of the sidewall is m-plane with unintentional miscut angle within 5 degrees.
  • a bulk GaN crystal is grown on the hexagonal seed crystal by ammonothermal method using a high-pressure reactor made of Ni-Cr superalloy.
  • a hexagonal shape bulk GaN having thickness approximately 5 mm is grown.
  • the yellowish transparent crystal shows neither of small cracks and large cracks originating the interface between the seed sidewalls and the grown crystal.
  • the X-ray FWHM is less than 150 arcsec, representing a good
  • a hexagonal shaped, single crystalline GaN seed crystal having a basal plane of c-plane is prepared by slicing a bulk crystal of GaN grown by the ammonothermal method.
  • the bulk GaN crystal grown by the ammonothermal method in this example has hexagonal polyhedron shape having m-plane sidewalls, and the crystal is sliced parallel to c-plane to form hexagonal-shaped seeds having only m-plane sidewalls.
  • the thickness of the seed is approximately 500 microns and the length of each side is approximately 1 cm with +/- 10% error.
  • the orientation of the sidewall is m-plane with unintentional miscut angle within 5 degrees.
  • GaN crystal is grown on the hexagonal seed crystal by ammonothermal method using a high-pressure reactor made of Ni-Cr superalloy.
  • a hexagonal shape bulk GaN having thickness approximately 5 mm is grown.
  • the yellowish transparent crystal shows neither small cracks nor large cracks originating above the interface between the seed sidewalls and the grown crystal.
  • the X-ray FWHM is less than 150 arcsec, representing a good microstructure.
  • a hexagonal shaped, single crystalline GaN seed crystal having a basal plane of c-plane is prepared by slicing a bulk crystal of GaN grown by a sodium flux method.
  • the bulk GaN crystal grown by a sodium flux method has hexagonal pyramid shape having ⁇ 10-11 ⁇ plane sidewalls. Slicing the crystal parallel to c-plane makes hexagonal-shaped seeds having ⁇ 10-1 1 ⁇ plane sidewalls. Then, the sidewall is cut along m- plane with a crystal dicer followed by etching in hot phosphoric acid as explained in Example 3.
  • the thickness of the seed is approximately 560 microns and the length of each side is approximately 1 cm within +/- 10% error.
  • the orientation of the sidewall is m- plane with unintentional miscut angle within 5 degrees.
  • the hexagonal seed crystal is used to grow an ingot of single-crystal GaN by ammonothermal method using a high- pressure reactor made of Ni-Cr superalloy.
  • a hexagonal shape bulk GaN having thickness approximately 5 mm is grown.
  • the yellowish transparent crystal shows neither small cracks nor large cracks originating above the interface between the seed sidewalls and the grown crystal.
  • the X-ray FWHM is less than 150 arcsec, representing a good microstructure.
  • Wafers are formed from bulk group III nitride of the examples above.
  • An electronic device is formed on wafers of each of the examples above using conventional circuit fabrication techniques known to those in the field of making electronic devices using group III nitride (e.g. by ion implantation, etching, and placing additional layers of materials on the wafers).
  • optical and optoelectronic devices are formed on wafers using conventional fabrication techniques.
  • the bulk GaN crystal of this invention contains no small or large cracks originating the interface between the sidewall of a seed crystal and the grown crystal.
  • the obtained crack-free bulk GaN crystals are sliced into wafers. These wafers are used for optical devices such as LEDs and laser diodes or electronic devices such as high-power transistors. Since cracks deteriorate performances and reliability of these devices significantly, this invention can improve the device performance and reliability. Possible modifications
  • GaN seed crystal having thickness about 430 microns, 500 microns, 560 microns, similar benefit of this invention can be expected for other thicknesses between 100 microns to 2000 microns.
  • the preferred embodiment describes a seed crystal having a width from one sidewall to a parallel sidewall of approximately 1 cm, similar benefit of this invention is expected for a larger seed such as 1", 2", 4", 6" and larger.
  • a bulk crystal as described, as made, or as used in any of the description above may have a thickness greater than or equal to: 1mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, 10mm, for instance.

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

Abstract

Dans un exemple, l'invention concerne un cristal massif de nitrure du groupe III présentant une épaisseur de plus de 1 mm sans fissuration au-dessus des côtés d'un cristal d'ensemencement. Ce cristal massif de nitrure du groupe III est exprimé par Gax1Aly1In1-x1-y1N (0≤x1≤1, 0<x1+y1≤1) et le cristal d'ensemencement est exprimé par Gax2Aly2In1-x2-y2N (0≤x2≤1, 0≤x2+y2≤1). On peut faire croître le cristal massif de nitrure du groupe III dans de l'ammoniac supercritique ou dans une masse fondue du métal du groupe III à l'aide d'au moins un cristal d'ensemencement présentant des plans de base d'orientation c et des parois latérales d'orientation m. En laissant apparaître, uniquement, des plans c et m dans ce cas, les fissures provenant des côtés du cristal d'ensemencement sont évitées.
PCT/US2015/032330 2014-05-23 2015-05-24 Cristaux massifs de nitrure du groupe iii et leur procédé de fabrication Ceased WO2015179852A1 (fr)

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US9790617B2 (en) 2006-04-07 2017-10-17 Sixpoint Materials, Inc. Group III nitride bulk crystals and their fabrication method

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US10611008B2 (en) 2016-11-20 2020-04-07 Custom Molded Products, Llc Installation tools for a water containing structure, components suitable for use therewith, and systems and methods of use therefor

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US9790617B2 (en) 2006-04-07 2017-10-17 Sixpoint Materials, Inc. Group III nitride bulk crystals and their fabrication method
US10161059B2 (en) 2006-04-07 2018-12-25 Sixpoint Materials, Inc. Group III nitride bulk crystals and their fabrication method

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