WO2001004940A1 - Procede de dopage de substrats en nitrure de gallium (gan) et substrat en gan dope ainsi produit - Google Patents

Procede de dopage de substrats en nitrure de gallium (gan) et substrat en gan dope ainsi produit Download PDF

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Publication number
WO2001004940A1
WO2001004940A1 PCT/US2000/018897 US0018897W WO0104940A1 WO 2001004940 A1 WO2001004940 A1 WO 2001004940A1 US 0018897 W US0018897 W US 0018897W WO 0104940 A1 WO0104940 A1 WO 0104940A1
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Prior art keywords
neutrons
doped gan
gan
substrates
isotope
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PCT/US2000/018897
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English (en)
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WO2001004940A9 (fr
WO2001004940A8 (fr
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Sang Kyu Kang
Hak Dong Cho
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Gan Semiconductor, Inc.
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Priority claimed from KR1019990028285A external-priority patent/KR100329718B1/ko
Application filed by Gan Semiconductor, Inc. filed Critical Gan Semiconductor, Inc.
Priority to AU60872/00A priority Critical patent/AU6087200A/en
Publication of WO2001004940A1 publication Critical patent/WO2001004940A1/fr
Publication of WO2001004940A8 publication Critical patent/WO2001004940A8/fr
Publication of WO2001004940A9 publication Critical patent/WO2001004940A9/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L33/02—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor bodies
    • H01L33/26—Materials of the light emitting region
    • H01L33/30—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table
    • H01L33/32—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen
    • H01L33/325—Materials of the light emitting region containing only elements of Group III and Group V of the Periodic Table containing nitrogen characterised by the doping materials
    • 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
    • C30B31/00—Diffusion or doping processes for single crystals or homogeneous polycrystalline material with defined structure; Apparatus therefor
    • C30B31/20—Doping by irradiation with electromagnetic waves or by particle radiation
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • 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
    • H01L21/26—Bombardment with radiation
    • H01L21/261—Bombardment with radiation to produce a nuclear reaction transmuting chemical elements

Definitions

  • This invention relates to the field of materials science and more particularly to the doping of Gallium Nitride (GaN) substrates.
  • GaN Gallium Nitride
  • III-V nitrides as a consequence of their electronic and optical properties and heterostructure character, are highly advantageous for use in the fabrication of a wide range of microelectronic structures.
  • the III-V nitrides also have direct band gaps and are able to form alloys which permit fabrication of well lattice-matched heterostructures. Consequently, devices made from the III-V nitrides can operate at high temperatures, with high power capabilities, and can efficiently emit light in the blue and ultraviolet regions of the electromagnetic spectrum.
  • Devices fabricated from III-V nitrides have applications in full color displays, super- luminescent light-emitting diodes (LEDs), high density optical storage systems, and excitation sources for spectroscopic analysis applications.
  • LEDs super- luminescent light-emitting diodes
  • the nitride semiconductor materials are direct transition semiconductor materials and, compared to the available Gallium Arsenide (GaAs) and Indium Phosphide (InP) semiconductor materials, are known to have high thermal conductivity, high-speed electron mobility, a high degree of strength, and are highly stable materials both thermally and chemically.
  • GaAs Gallium Arsenide
  • InP Indium Phosphide
  • the typical nitride semiconductor materials are different from other compound semiconductor materials and, as such, are not able to be produced in the form of ingot-type or bulk-type Gallium Nitride (GaN).
  • heteroepitaxy substrate materials One problem with the heteroepitaxy substrate materials is found in their high defect density, a defect density on the order of 10 9 - 10 10 defects per square centimeter (cm " ).
  • the high defect density results from a large mismatch factor resulting from a difference in lattice constants.
  • This defect density in conjunction with the different thermal expansion coefficients associated with the base substrate material and the growth layer leads to cracks in the growth layer or substrate material.
  • nitride semiconductor substrates The production of nitride semiconductor substrates is complicated by the fact that the GaN dopant partially occupies the Gallium site or the Nitride site. This results in mutual chemical reactions occurring among defects in the material and other impurities. Therefore, obtaining good quality doping in the production of nitride semiconductor substrates is not as easy as in single atom silicon semiconductor materials because it requires precise control of uniform doping and carrier concentrations as well as accurate control of impurities. Consequently, there is a need for a method that overcomes these complications and provides for the production of good quality doped GaN substrates.
  • a method for doping Gallium Nitride (GaN) substrates wherein Gallium (Ga) is transmuted to Germanium (Ge) by applying thermal neutron irradiation to a GaN substrate material or wafer.
  • the Ge is introduced as an impurity in GaN and acts as a donor.
  • the concentration of Ge introduced is controlled by the thermal neutron flux.
  • the thermal neutron irradiation is applied to a GaN wafer the fast neutrons are transmuted together with the former and cause defects such as the collapse of the crystallization.
  • the GaN wafer is thermally treated or processed at a fixed temperature to eliminate such defects.
  • Figure 1 is a flow chart of a method that provides doped single crystal Gallium Nitride (GaN) substrates and GaN substrate thin films by subjecting GaN substrates to Neutron Transmutation Doping (NTD).
  • GaN Gallium Nitride
  • NTD Neutron Transmutation Doping
  • Figure 2 shows thermal neutron irradiation conditions of an embodiment.
  • Figure 3 shows a photoluminescence (PL) spectrum measured at 1 OK for GaN samples of an embodiment resulting from application of three thermal neutron flux values and thermal annealing.
  • Figure 4 shows the PL spectrum measured at 10K for the GaN samples of an embodiment after thermal annealing for 30 minutes at approximately 950°C.
  • Figure 5 shows the PL spectrum measured at 10K for the GaN samples of an embodiment after thermal annealing for 30 minutes at approximately 1000°C.
  • Figure 6 shows results of the Hall effects measured at room temperature for the GaN samples of an embodiment after treatment with transfer fluxes of approximately 4.146 x 10 neutrons cm “ , 5.29 x 10 neutrons cm “ , and 1.09 x 10 19 neutrons cm “2 , respectively, and thermal annealing for approximately 30 minutes in a nitrogen environment at approximately 1000°C and 1100°C.
  • Figure 7 shows SIMS results measured at room temperature for the GaN samples of an embodiment after treatment with transfer fluxes of approximately 4.146 x 10 17 neutrons cm “2 and 30 minutes of thermal annealing at approximately 1000°C.
  • Figure 8 shows SIMS results measured at room temperature for the GaN samples of an embodiment after treatment with a transfer flux of approximately 5.29 x 10 18 neutrons cm "2 and 30 minutes of thermal annealing at approximately 1000°C.
  • Figure 9 shows SIMS results measured at room temperature for the GaN samples of an embodiment after treatment with a transfer flux of approximately 1.09 x 10 neutrons cm " and approximately 30 minutes of thermal annealing at approximately 1000°C.
  • FIG. 1 is a flow chart of a method that overcomes the technical barriers encountered in the doping of Gallium Nitride (GaN) substrates and provides doped single crystal GaN substrates and GaN substrate thin films by subjecting GaN substrates to Neutron Transmutation Doping (NTD), a thermal neutron transmutation method.
  • the method of an embodiment includes doping the GaN material by transmuting Gallium (Ga) into Germanium (Ge) using thermal neutron irradiation fluence 102, or thermal neutron flux, applied to the GaN material.
  • the concentration of the doped Ge is controlled by the flux of the thermal neutrons to which the substrate is subjected.
  • the method further includes thermal annealing 104 of the GaN substrate material doped with Ge at a fixed temperature substantially in the range of 700 to 1200 degrees Celsius. A fixed temperature approximately equal to 1000 degrees Celsius is optimal in an embodiment, but the embodiment is not so limited.
  • the NTD process takes place when undoped silicon substrates are irradiated in a thermal neutron flux.
  • the purpose of semiconductor doping is to create free electrons.
  • Most compound semiconductors contain at least one element that consists of more than one stable isotope, for example Ga.
  • NTD NTD to dope semiconductor materials the largest effects due to isotopic composition occur after the capture of a thermal neutron by the nucleus of a specific isotope. Either the new nucleus is stable and the element remains unchanged, or it decays, transmuting into a new element.
  • this NTD is used to introduce Ge donors into high-purity GaN substrates when the Ge donor atoms are created in the beta decay of an unstable Ga isotope formed when a Ga isotope captures a thermal neutron.
  • the NTD of an embodiment, as applied to GaN substrates has numerous advantages when compared with other doping methods.
  • One advantage is that the neutrons do not possess an electrical charge. This allows for rather extreme uniformity of doping of impurities regardless of material thickness because, as compared with other doping methods the NTD has the advantage that, provided the isotopes of Ga and N are uniformly distributed, the neutrons are uniformly captured, and therefore the transmuted impurities are distributed uniformly in the samples.
  • Another advantage is that the concentration of impurities is precisely controlled by controlling the neutron dosages.
  • GaN material is doped by transmuting Ga to Ge by applying thermal neutron irradiation to the GaN substrate.
  • the transmutation of Ga to Ge introduces Ge as an impurity, and the Ge acts as a donor in the GaN substrate.
  • the concentration of the Ge is determined by the thermal neutron flux.
  • the doped GaN substrates are thermally annealed at a predetermined temperature.
  • the annealing temperature of an embodiment is a fixed temperature of approximately 1000 degrees Celsius, but is not so limited.
  • NTD was performed using thermal neutron irradiation of a GaN substrate with flux values of 4.146 x 10 17 neutrons/cm 2 -
  • the GaN substrate samples were thermally annealed in a nitrogen environment at 900, 950, 1000, and 1100 degrees Celsius. The features of the samples were examined by measuring sample Photoluminescence (PL), the Hall effect, and Secondary Ion Mass Spectroscopy (SIMS).
  • PL Photoluminescence
  • SIMS Secondary Ion Mass Spectroscopy
  • N 14 (49.82%, 1.8 barn)
  • the first item within the parenthesis is the natural isotope abundance ratio, and the second item denotes the absorption cross-section.
  • the isotopes above capture the neutrons first and are transmuted into unstable isotopes as indicated in equation 2, which is followed by their collapse as isotopes by the irradiation of gamma rays and beta rays:
  • Ga (n, ⁇ ) Ga and Ga (n, ⁇ ) Ga expressions indicate that Ga and G due to irradiation with gamma rays, which is the result of the transfer of neutrons.
  • the N 14 (n, p) C 14 denotes the transmutation of N 14 to C 14 by the transfer of neutrons, which leads to the discharge of protons.
  • the Ga , Ga and C each radiate beta rays and are transmuted into Ge 70 , Ge 72 and N 14 , respectively.
  • the beta is an electron of nuclear origin, and it shares the total energy of the reaction with an electronic antineutrino. These two particles are leptons and in nuclear reactions the sum of the leptons is conserved.
  • the concentrations of Ge 70 , Ge 7 and N 14 are proportional to the concentrations of Ga 70 , Ga 72 and C 14 , respectively, the integrated thermal neutron flux, and the thermal neutron capture cross section.
  • the time given in parentheses in these expressions is the half-life during which the ⁇ " collapse of
  • GaN occurs. Both the Ga and Ga formed from the nuclear reactions are introduced as impurities in the GaN substrate and act as donors.
  • N nt a The doping concentration of impurities at the time of transmission of neutrons to a compound semiconductor, N nt a, is expressed in equation 3 as:
  • N ntd ⁇ t ⁇ Equation 3
  • ⁇ is the flux of thermal neutrons
  • t is the time of transfer
  • ⁇ is the ith isotope
  • ⁇ C 1 absorption cross section of the ith isotope.
  • Transmuted atoms are not typically located in the original crystal lattice surface following nuclear reactions.
  • the transmuted atoms move to the surface of the crystal or empty Ga and N sites. This results in the formation of defect levels in the GaN substrate.
  • the fast neutrons are not captured in the GaN and form defect levels in the GaN owing to collisions with the crystal lattice.
  • defect levels including Noa, GaN, Voa, V N , Ga;, and N t are produced in GaN by both thermal neutrons and fast neutrons.
  • No a indicates that N is present in the site of Ga
  • Ga indicates that Ga is present in the site of N.
  • V N and Gas indicate that each site of N is vacant and Ga occupies intermediate sites.
  • the defect levels in GaN formed in this manner are reduced in an embodiment using thermal annealing.
  • a Ge atom that is transmuted and doped in GaN at the critical temperature of at least 1000 degrees Celsius forms a donor level, contributing to the activation of the carrier.
  • the Hanaro nuclear reactor located in the Korea Atomic Energy Research Institute was used for the irradiation of the thermal neutrons of a GaN sample, a representative semiconductor among nitride semiconductors.
  • the generating power of the nuclear reactor used in the experiment was 20 megawatts (MW).
  • the irradiation processes of thermal neutrons included the hydraulic transfer system (HTS) and isotope production (IP).
  • Figure 2 shows thermal neutron irradiation conditions of an embodiment. At the time of irradiation, samples were irradiated in a temperature range of 125 to 210 degrees Celsius (°C) after being wrapped with aluminum foil under different conditions and double-sealed together with Fe and Ni wire
  • the samples were thermally annealed in a nitrogen environment at the temperatures of approximately 900, 950, 1000, and 1100°C.
  • Photo luminescence (PL) was measured at a temperature of approximately 10 Kelvin (K) to confirm the crystallization recovery properties and the optical properties of these samples.
  • the Hall effect was measured at room temperature in order to examine the doping properties of the Ge atoms transmuted and doped from Ga atoms.
  • the properties of the samples transmuted and doped by neutrons were examined for 30 minutes at approximately 900°C in a nitrogen environment by measuring SIMS based on the use of the cesium (Cs) ion for a fixed quantity analysis of the Ge atom.
  • Figure 3 shows a photoluminescence (PL) spectrum measured at 1 OK for GaN samples of an embodiment resulting from application of three thermal neutron flux values and thermal annealing.
  • Spectrum (a) is a spectrum of a GaN sample resulting from treatment with a transfer flux of approximately 4.146 x 10 17 neutrons cm “2 .
  • Spectrum (b) is a spectrum of a GaN sample resulting from treatment with a transfer flux of approximately 5.29 x 10 18 neutrons cm “2 .
  • Spectrum (c) is a spectrum of a GaN sample resulting from treatment with a transfer flux of approximately 1.09 x 10 19 neutrons cm “2 .
  • the intensity of the peak associated with the band gap of GaN differs depending upon the size of the flux of thermal neutrons transferred. This is due not only to the thermal neutrons associated with doping at the time of transfer of neutrons to the semiconductor, but also due to the fact that the fast neutrons that cause crystal defects are transferred to the sample, which in turn causes an increase of fast neutrons with the increase of the flux of thermal neutrons transferred, and this is followed by an increase of crystal defects of each sample. Thus, it can be seen that the extent of re-crystallization is different despite the same thermal annealing conditions.
  • Figure 4 shows the PL spectrum measured at 10K for the GaN samples of an embodiment after thermal annealing for 30 minutes at approximately 950°C.
  • Spectrum (a) is a spectrum of a GaN sample resulting from treatment with a transfer flux substantially in the range of 4.146 x 10 17 neutrons cm “2 .
  • Spectrum (b) is a spectrum of a GaN sample resulting from treatment with a transfer flux of approximately 5.29 x 10 neutrons cm " .
  • Spectrum (c) is a spectrum of a GaN sample resulting from treatment with a transfer flux of approximately 1.09 x 10 19 neutrons cm “2 .
  • Figure 5 shows the PL spectrum measured at 10K for the GaN samples of an embodiment after thermal annealing for 30 minutes at approximately 1000°C.
  • Spectrum (a) is a spectrum of a GaN sample resulting from treatment
  • Spectrum (b) is a spectrum of a GaN sample resulting from treatment with a transfer flux of approximately 5.29 x 10 neutrons cm " .
  • Spectrum (c) is a spectrum of a GaN sample resulting from treatment with a transfer flux of approximately 1.09 x 10 19 neutrons cm “2 .
  • Figure 6 shows results of the Hall effects measured at room temperature for the GaN samples of an embodiment after treatment with transfer fluxes of approximately 4.146 x 10 17 neutrons cm “2 , 5.29 x 10 18 neutrons cm “2 , and 1.09 x 10 19 neutrons cm “2 , respectively, and thermal annealing for approximately 30 minutes in a nitrogen environment at approximately 1000°C.
  • the total flux of transferred thermal neutrons is about 100 times higher than the concentration of the carrier. This indicates that the Ga atoms in the GaN crystal are about 50% of the atom rate.
  • crystallization has almost fully recovered.
  • the electron mobility is the highest at 386V*Cm "3 .
  • Figure 7 shows SIMS results measured at room temperature for the GaN samples of an embodiment after treatment with transfer fluxes of approximately 4.146 x 10 17 neutrons cm "2 and 30 minutes of thermal annealing at approximately 1000°C.
  • the concentration of Ge transmuted from Ga in GaN crystals is approximately 1.1 x 10 cm "3 . This value is about 10 percent of the total flux of transferred neutrons and about 10 times larger than the measurements for the Hall effect.
  • this result is associated with the fact that Ga atoms have about 50% of the atom rate in GaN crystals, and the result shows that crystal defects have not been fully solved and crystallization has not yet fully recovered by thermal annealing.
  • Figure 8 shows SIMS results measured at room temperature for the GaN samples of an embodiment after treatment with a transfer flux of

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Abstract

L'invention se rapporte à un procédé de dopage de substrats en nitrure de gallium (GaN), selon lequel le Gallium subit une transmutation en Germaniun (Ge) du fait de l'application d'un rayonnement neutronique thermique sur le matériau du substrat en GaN ou sur une plaquette. Ce germanium est introduit en tant qu'impureté dans le nitrure de gallium et il joue le rôle de donneur. La concentration du germanium introduit est régulée par le flux neutronique thermique. Lorsque le rayonnement neutronique thermique est appliqué sur une plaquette en GaN, les neutrons rapides sont soumis à une transmutation en même temps que les atomes de gallium et ils sont à l'origine de défauts tels que l'effondrement de la cristallisation. La plaquette en GaN est soumise à un traitement thermique ou elle est traitée à température fixe aux fins de la suppression de ces défauts.
PCT/US2000/018897 1999-07-13 2000-07-12 Procede de dopage de substrats en nitrure de gallium (gan) et substrat en gan dope ainsi produit WO2001004940A1 (fr)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AU60872/00A AU6087200A (en) 1999-07-13 2000-07-12 Method for doping gallium nitride (gan) substrates and the resulting doped gan substrate

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Application Number Priority Date Filing Date Title
KR1019990028285A KR100329718B1 (ko) 1999-07-13 1999-07-13 질화갈륨 기판의 도핑 방법 및 도핑된 질화갈륨 기판
KR99/28285 1999-07-13
US16416200P 2000-07-11 2000-07-11
US09/164,162 2000-07-11

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2433991A1 (de) * 1974-07-15 1976-02-05 Siemens Ag Verfahren zum dotieren einer halbleiterschicht
US4135951A (en) * 1977-06-13 1979-01-23 Monsanto Company Annealing method to increase minority carrier life-time for neutron transmutation doped semiconductor materials

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2433991A1 (de) * 1974-07-15 1976-02-05 Siemens Ag Verfahren zum dotieren einer halbleiterschicht
US4135951A (en) * 1977-06-13 1979-01-23 Monsanto Company Annealing method to increase minority carrier life-time for neutron transmutation doped semiconductor materials

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
POPOVICI G: "Transmutation doping of III-nitrides", WIDE-BANDGAP SEMICONDUCTORS, SAN FRANCISCO, 5-8 APR 1999, pages 519 - 522, XP002150628 *
SHMIDT N M ET AL: "Effect of annealing on defects in gamma-irradiated n-GaN layers", NITRIDE SEMICONDUCTORS, MONTPELLIER, 4-9 JULY 1999, vol. 216, no. 1, Physica Status Solidi B, 1 Nov. 1999, pages 533 - 536, XP000956060, ISSN: 0370-1972 *

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