WO2006130622A2 - Growth of planar non-polar{1-1 0 0} m-plane gallium nitride with metalorganic chemical vapor deposition (mocvd) - Google Patents

Growth of planar non-polar{1-1 0 0} m-plane gallium nitride with metalorganic chemical vapor deposition (mocvd) Download PDF

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WO2006130622A2
WO2006130622A2 PCT/US2006/020995 US2006020995W WO2006130622A2 WO 2006130622 A2 WO2006130622 A2 WO 2006130622A2 US 2006020995 W US2006020995 W US 2006020995W WO 2006130622 A2 WO2006130622 A2 WO 2006130622A2
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polar
substrate
plane
nitride
growing
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French (fr)
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WO2006130622A3 (en
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Bilge M. Imer
James S. Speck
Steven P. Denbaars
Shuji Nakamura
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Japan Science and Technology Agency
University of California Berkeley
University of California San Diego UCSD
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Japan Science and Technology Agency
University of California Berkeley
University of California San Diego UCSD
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Priority to KR1020127010536A priority Critical patent/KR101499203B1/ko
Priority to EP06760566A priority patent/EP1897120A4/en
Priority to JP2008514783A priority patent/JP2008543087A/ja
Publication of WO2006130622A2 publication Critical patent/WO2006130622A2/en
Publication of WO2006130622A3 publication Critical patent/WO2006130622A3/en
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    • H—ELECTRICITY
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    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/20—Deposition of semiconductor materials on a substrate, e.g. epitaxial growth solid phase epitaxy
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C—CHEMISTRY; METALLURGY
    • C30—CRYSTAL GROWTH
    • C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B25/00—Single-crystal growth by chemical reaction of reactive gases, e.g. chemical vapour-deposition growth
    • C30B25/02—Epitaxial-layer growth
    • C30B25/18—Epitaxial-layer growth characterised by the substrate
    • 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
    • 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
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    • H01L21/02612—Formation types
    • H01L21/02617—Deposition types
    • H01L21/0262—Reduction or decomposition of gaseous compounds, e.g. CVD

Definitions

  • DenBaars entitled “DEFECT REDUCTION OF NON-POLAR GALLIUM NITRIDE WITH SINGLE-STEP SIDEWALL LATERAL EPITAXIAL OVERGROWTH,” attorneys' docket no. 30794.135-US-P1 (2005-565); United States Utility Patent Application Serial No. 10/537,385, filed June 3,
  • the present invention relates to the growth of planar non-polar ⁇ 1 -1 0 0 ⁇ m- plane gallium nitride (GaN) with metalorganic chemical vapor deposition (MOCVD). 2. Description of the Related Art.
  • Gallium nitride (GaN) and its ternary and quaternary compounds are prime candidates for fabrication of visible and ultraviolet high-power and high-performance optoelectronic devices and electronic devices. These devices are typically grown epitaxially by growth techniques including molecular beam epitaxy (MBE), metalorganic chemical vapor deposition (MOCVD), or hydride vapor phase epitaxy (HVPE).
  • MBE molecular beam epitaxy
  • MOCVD metalorganic chemical vapor deposition
  • HVPE hydride vapor phase epitaxy
  • substrate is critical for achieving the desired GaN growth orientation.
  • Some of the most widely used substrates for III-N growth include SiC, Al 2 O 3 , and LiAlO 2 .
  • Various crystallographic orientations of these substrates are commercially available.
  • FIGS. l(a) and l(b) are schematics of crystallographic directions and planes of interest in hexagonal GaN. Specifically, these schematics show the different crystallographic growth directions and also the planes of interest in the hexagonal wurtzite GaN structure, wherein FIG. l(a) shows the crystallographic directions al, a2, a3, c, ⁇ 10-10> and ⁇ 11-20>, and FIG. l(b) shows planes a (11-20), m (10-10) and r (10-12).
  • the fill patterns of FIG. l(b) are intended to illustrate the planes of interest, but do not represent the materials of the structure.
  • 2(b) is a graph of energy (eV) vs. depth (nm) and represents a non-polar quantum well.
  • eV energy
  • nm depth
  • Such polarization effects decrease the likelihood of electrons and holes recombining, causing the final device to perform poorly.
  • One possible approach for eliminating piezoelectric polarization effects in GaN optoelectronic devices is to grow the devices on non-polar planes of the crystal such as a- ⁇ 11-20 ⁇ and m- ⁇ l-100 ⁇ planes family of GaN. Such planes contain equal numbers of Ga and N atoms and are charge-neutral.
  • Planar ⁇ 1-100 ⁇ m-plane GaN growth has been developed by HVPE and MBE methods. However, prior to the invention described herein, planar m-plane GaN growth had not been accomplished with MOCVD.
  • the general purpose of the present invention is to grow planar non-polar m- ⁇ 1-100 ⁇ plane GaN material using MOCVD.
  • the method includes performing a solvent clean and acid dip of an m-SiC substrate to remove oxide from the surface of the substrate ex situ prior to growth, in situ annealing of the substrate, growing an aluminum nitride (AlN) nucleation layer on the annealed substrate, and growing the non-polar m-plane GaN epitaxial layer on the nucleation layer with MOCVD.
  • AlN aluminum nitride
  • the present invention takes advantage of non-polar nature of m-plane GaN to eliminate polarization fields, and gives rise to flexibility in growth variables, such as temperature, pressure and precursor flows, utilizing the advantage of m-GaN stability during growth.
  • FIGS. l(a) and l(b) are schematics of crystallographic directions and planes of interest in hexagonal GaN.
  • FIGS. 2(a) and 2(b) are schematics of band bending and electron hole separation as a result of polarization.
  • FIG. 3 provides a structural characterization of non-polar planar m-plane GaN on m-plane SiC, from top to bottom, wherein the crystal plane of interest is shown in a unit cell/
  • FIG. 4 is a 5 ⁇ m x 5 ⁇ m atomic force microscopy (AFM) surface image with a surface roughness value 2.54nm.
  • AFM atomic force microscopy
  • FIG. 5 is a graph that illustrates the xray diffraction rocking curves for on-axis and off-axis.
  • FIG. 6 is a flowchart that illustrates the processing steps for growing planar m- plane Ill-Nitrides using MOCVD according to the preferred embodiment of the present invention.
  • FIG. 7 further illustrates the results of the processing steps of FIG. 6 according to the preferred embodiment of the present invention.
  • FIG. 3 illustrates the non-polar m-plane GaN (1-100) crystal plane of interest in the unit cell.
  • V /IH ratios of 400-5500 and 200-3000 growth pressures varying in between 50-760 Torr, and temperature series of 1100 0 C - 1275 0 C and 1000 0 C - 1160 0 C for AlN and GaN layers were tested, respectively.
  • a 5 ⁇ m x 5 ⁇ m atomic force microscopy (AFM) surface image of the resulting m-plane GaN material is shown in FIG. 4.
  • the grains are oriented along the ⁇ 11-20> direction and the surface roughness value (root mean square) is ⁇ 2.54 ran for a 5 ⁇ m x 5 ⁇ m scan.
  • FIG. 5 is a graph of omega (degrees) vs. counts/second showing the x-ray diffraction rocking curves on-axis and off-axis.
  • on-axis (1-100) full width at half max (FWHM) values are measured as low as 0.22° and 1.2°, for a-mosaic and c-mosaic, respectively, and the off-axis (10-12) reflection has FWHM value of 0.38°.
  • FIG. 6 is a flowchart that illustrates the processing steps for growing a planar non polar ⁇ 1-100 ⁇ m-plane Ill-Nitride epitaxial film using MOCVD according to the preferred embodiment of the present invention, wherein the planar non polar m-plane Ill-Nitride epitaxial film may comprise a planar m-plane GaN epitaxial layer.
  • FIG. 7 further illustrates the results of each of the processing steps of FIG. 6.
  • Block 600 represents a solvent clean and acid dip of a suitable substrate (700), for example, in a 1 : 10 diluted BHF:DI solution, to remove oxide (702) from the substrate (700) surface before loading the substrate (700) into a reactor for the growth step. (Although this step is recommended, its omission would not significantly alter the results.)
  • the substrate (700) may comprise an m-SiC or any substrate that is suitable for non-polar m-plane Ill-Nitride growth.
  • Block 602 represents in situ annealing of the substrate (700), for example, in hydrogen, prior to the growth step. (Although this step is recommended, its omission would not significantly alter the results.)
  • Block 604 represents growing a nucleation layer (704) on the substrate (700).
  • the nucleation layer (704) typically comprises an aluminum nitride (AlN) nucleation layer or interlayer, but may comprise any nucleation layer (704) that is appropriate for non-polar m-plane Ill-Nitride growth.
  • the nucleation layer (704) may be grown after the annealing step, and prior to the non polar m-plane Ill-Nitride growth.
  • Block 606 represents growing the non-polar m-plane Ill-Nitride epitaxial layer (706) using MOCVD.
  • the non-polar m-plane Ill-Nitride epitaxial layer (706) typically comprises a non-polar m-plane GaN epitaxial layer, but may comprise other non-polar m-plane Ill-Nitride epitaxial layers as well.
  • the non-polar m- plane Ill-Nitride epitaxial layer (706) may be grown on the nucleation layer (704), or on the substrate (700) itself.
  • the end result is a device, or a free standing wafer, or a substrate, or a template, having a planar epitaxial layer of the non-polar m-plane Ill-Nitride.
  • non-polar m-GaN on m-SiC using an AlN interlayer alternative suitable substrates, on which the non-polar m-plane Ill-Nitride epitaxial film could be formed, include, but are not limited to, 6H or 4H m-plane SiC, freestanding m-GaN, LiGaO 2 and LiAlO 2 .
  • the suitable substrate Prior to growth, the suitable substrate can be treated in many different ways in-situ or ex-situ, or it may not be treated at all.
  • the non-polar epitaxial film can be nucleated and grown over different nucleation layers, such as GaN or AlN grown at various conditions and methods, or over a bare substrate.
  • the epitaxial film can be any non-polar m-plane IE-Nitride material including, but not limited to, GaN, AlN, AlGaN and InGaN with various thicknesses.
  • the growth parameters required for the growth of non-polar m-plane Ill- Nitride material may vary from reactor to reactor.
  • the growth of m- ⁇ l-100 ⁇ plane GaN has been successfully demonstrated by HVPE and MBE.
  • the present invention is the first-ever successful demonstration of high-quality planar non-polar m- ⁇ l-100 ⁇ plane GaN growth by MOCVD.
  • planar m-plane GaN has an advantage over growth of planar a- ⁇ l 1- 20 ⁇ GaN with MOCVD in terms of its stability with a large growth window. This was shown when growth variables such as temperature, pressure and precursor flows for AlN nucleation layer and GaN epitaxial film were changed.
  • V/m ratios of 400-5500 and 200-3000, growth pressures varying in between 50-760 Torr, and temperature series of 1100 0 C - 1275 0 C and 1000 0 C - 1160 0 C for AlN and GaN layers were tested, respectively. Alterations in such conditions did not affect the crystal and surface quality significantly unlike the planar non-polar a-plane GaN films in which crystal and surface quality are extremely susceptible to change in growth conditions and constrained with small growth window.

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PCT/US2006/020995 2005-05-31 2006-05-31 Growth of planar non-polar{1-1 0 0} m-plane gallium nitride with metalorganic chemical vapor deposition (mocvd) Ceased WO2006130622A2 (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
KR1020127010536A KR101499203B1 (ko) 2005-05-31 2006-05-31 유기금속 화학기상증착법을 이용한 평면 비극성 （１­１００） ｍ­면 갈륨 질화물의 성장
EP06760566A EP1897120A4 (en) 2005-05-31 2006-05-31 GROWTH OF PLANAR NICHEPOLAR {1-1 0 0} M-LEVEL GALLIUM NITRIDE WITH METAL-ORGANIC CHEMICAL MISTAKING (MOCVD)
JP2008514783A JP2008543087A (ja) 2005-05-31 2006-05-31 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

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US68590805P 2005-05-31 2005-05-31
US60/685,908 2005-05-31

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WO2009066466A1 (ja) * 2007-11-21 2009-05-28 Mitsubishi Chemical Corporation 窒化物半導体および窒化物半導体の結晶成長方法ならびに窒化物半導体発光素子
US9508898B2 (en) 2014-08-28 2016-11-29 Samsung Electronics Co., Ltd. Nanostructure semiconductor light emitting device

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US9130119B2 (en) * 2006-12-11 2015-09-08 The Regents Of The University Of California Non-polar and semi-polar light emitting devices
TWI377602B (en) * 2005-05-31 2012-11-21 Japan Science & Tech Agency Growth of planar non-polar {1-100} m-plane gallium nitride with metalorganic chemical vapor deposition (mocvd)
JP2007277074A (ja) * 2006-01-10 2007-10-25 Ngk Insulators Ltd 窒化アルミニウム単結晶の製造方法及び窒化アルミニウム単結晶
GB2436398B (en) * 2006-03-23 2011-08-24 Univ Bath Growth method using nanostructure compliant layers and HVPE for producing high quality compound semiconductor materials
CN101437987A (zh) * 2006-04-07 2009-05-20 加利福尼亚大学董事会 生长大表面积氮化镓晶体
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JP2010512661A (ja) * 2006-12-11 2010-04-22 ザ リージェンツ オブ ザ ユニバーシティ オブ カリフォルニア 高特性無極性ｉｉｉ族窒化物光デバイスの有機金属化学気相成長法（ｍｏｃｖｄ）による成長
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GB0701069D0 (en) * 2007-01-19 2007-02-28 Univ Bath Nanostructure template and production of semiconductors using the template
US7598108B2 (en) * 2007-07-06 2009-10-06 Sharp Laboratories Of America, Inc. Gallium nitride-on-silicon interface using multiple aluminum compound buffer layers
US8652947B2 (en) * 2007-09-26 2014-02-18 Wang Nang Wang Non-polar III-V nitride semiconductor and growth method
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US8097481B2 (en) 2012-01-17
US8795440B2 (en) 2014-08-05
JP2014099616A (ja) 2014-05-29
JP2008543087A (ja) 2008-11-27
US7338828B2 (en) 2008-03-04
TW200703470A (en) 2007-01-16
EP1897120A2 (en) 2008-03-12
WO2006130622A3 (en) 2007-08-02
TWI377602B (en) 2012-11-21
KR101499203B1 (ko) 2015-03-18
US20080026502A1 (en) 2008-01-31
US20060270087A1 (en) 2006-11-30
KR20080014077A (ko) 2008-02-13
US20120074429A1 (en) 2012-03-29
KR20120064713A (ko) 2012-06-19

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