GOX 2023 Session EG+BG+MD-WeM: Epitaxial III

Wednesday, August 16, 2023 9:15 AM in Room Davis Hall 101

Wednesday Morning

Session Abstract Book
(331KB, Aug 7, 2023)
Time Period WeM Sessions | Abstract Timeline | Topic EG Sessions | Time Periods | Topics | GOX 2023 Schedule

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9:15 AM EG+BG+MD-WeM-4 Growth of ⍺-(AlxGa1-x)2O3 by Suboxide Molecular-Beam Epitaxy
Jacob Steele, Kathy Azizie, Naomi Pieczulewski, Jon McCandless, David A. Muller, Huili Grace Xing, Debdeep Jena (Cornell University); Takeyoshi Onuma (Kogakuin University); Darrell Schlom (Cornell University (USA) and Leibniz-Institut für Kristallzüchtung (Germany))

Ga2O3 has attracted significant interest due to its ultra-wide bandgap, high electron mobility, and large breakdown field. These properties exceed the current benchmarks set by materials such as SiC and GaN, making Ga2O3 optimal for next-generation power devices. Still, it has been proposed that the properties of Ga2O3 can be extended further by alloying with Al to form (AlxGa1-x)2O3 which can raise the bandgap to 8.6 eV. This goal presents a challenge for the most researched phase, β, as β-Ga2O3 thermodynamically prefers a monoclinic structure and α-Al2O3 is stable in the corundum structure. This structural mismatch limits the compositional range and the range of attainable bandgaps. In contrast, α-Ga2O3 occupies the corundum structure and has been shown to alloy over the full compositional range, enabling bandgaps from 5.3 - 8.6 eV. One method of growing α-(AlxGa1-x)2O3 is molecular-beam epitaxy (MBE). MBE is a powerful and highly controllable growth technique for α-(AlxGa1-x)2O3 thin films with drawbacks being slow growth rates of a few hundred nm/h and narrow adsorption-controlled growth windows. One method to improve the growth rate is the technique of suboxide MBE, which allows growth of β-Ga2O3 thin films at rates exceeding 1 μm/h with large adsorption-controlled growth regimes.


We show that suboxide MBE can be used for the epitaxial growth of high quality α-(AlxGa1-x)2O3 thin films on A plane sapphire substrates over the full range of x at greater than 1 μm/h. For our study, gallium suboxide, Ga2O, and elemental Al are the MBE sources. The oxidant is 80% distilled ozone which is held at constant pressure (5 x 10-6 Torr) while the Ga2O and Al fluxes are varied to control composition. We measure the composition of our films with XRD and confirm that we cover the full range of 0 < x < 1 with vacuum ultraviolet transmittance measurements showing that the bandgaps of our films shift from α-Ga2O3 to α-Al2O3. We show that the film composition can be controlled directly by the relative ratios of the Ga2O and Al fluxes. Our films have high structural quality as revealed by the full width at half maximum (FWHM) of rocking curves of the α-(AlxGa1-x)2O3 films ranging from 11 - 15 arcseconds; these FWHMs are identical to the underlying sapphire substrates. The surfaces of the films are also smooth with RMS roughnesses measured by atomic force microscopy ranging from 0.3 - 1.1 nm on α-(AlxGa1-x)2O3 films with thicknesses in the 17.8 - 47.8 nm range. We also show our progress with growing α-(AlxGa1-x)2O3 films over 100 nm thick and with doping using a SiO2 source. View Supplemental Document (pdf)
9:30 AM EG+BG+MD-WeM-5 Structural, Electrical, and Thermal Characterization of CIS-MOCVD β-Ga2O3 Epitaxial Buffer Layers
Hannah Masten (Naval Research Laboratory); Gustavo Alvarez (Cornell University); Corey Halverson (Washington State University); Michael Liao, James Spencer Lundh (Naval Research Laboratory); Fikadu Alema, Andrei Osinsky (Agnitron Technology); Alan Jacobs (Naval Research Laboratory); Marc Weber (Washington State University); Zhiting Tian (Cornell University); Karl Hobart, Marko Tadjer (Naval Research Laboratory)

Epitaxial growth of β-Ga2O3 using metalorganic chemical vapor deposition (MOCVD) has seen great advancements demonstrating high-quality films with low point defect concentrations and high mobility with low doping concentrations [1]. Here, we investigate the impact of buffer layer thickness for these MOCVD epitaxial films on electrical characteristics, thermal conductivity, and defect concentrations.

MOCVD films were grown on Novel Crystal Technology’s Fe-doped (010) β-Ga2O3 substrates using Agnitron Technology’s Agilis close-injection showerhead MOCVD (CIS-MOCVD). The unintentionally doped (UID) buffer layer thickness was varied on the 3 samples: A-300, B-500, and C-1000 nm. The UID layers were followed by a 10 nm thick n+ (~1019 cm-3) Ga2O3 layer for improved channel conductivity. A 100 nm highly n+ layer was selectively regrown following ref. [2]. Ohmic contacts were formed in the regrown areas with an annealed 20/200 nm Ti/Au metal stack (470 °C, 1 min., N2). Mesa isolation was formed with an etch of ~170 nm. Transmission line measurements (TLM) showed sample C had the lowest specific contact resistance of 2.25 × 10-6Ω·cm2 and sample A had the highest of 1.99 × 10-4Ω·cm2. Room temperature Hall effect measurement showed similar mobility for B and C of 115-116 cm2/V·s, while sample A showed a much lower mobility of 71 cm2/V·s. Samples B and C, both showed high open-gated source-drain current (ID) (>0.05 A/mm at VDS= 5 V) and low isolation (mesa-mesa) current (Iiso) of < 0.1 µA/mm at VDS= 10 V. Sample A (300 nm thick buffer layer), showed 10X lower open-gated ID and a high Iiso of ~3 mA/mm at VDS= 10 V. Higher Iiso for samples with thin buffer layers, such as sample A, have been frequently attributed to a peak in Si concentration at the epilayer/substrate interface observed in secondary-ion mass spectroscopy [1]. Here, we offer further insight on this effect via frequency-domain thermoreflectance (FDTR) and positron annihilation spectroscopy (PAS). Preliminary FDTR data showed decreasing thermal conductivity for thicker epilayers. PAS data fitted with a 3-layer model consistently showed higher density of Ga-related vacancies in the epilayers compared to each substrate. More detailed measurements, including XRD and device-level FDTR, will be performed. This preliminary data suggested that MOCVD Ga2O3 was affected by both unintentional impurities and point defects in addition to the known issue of interfacial Si accumulation. [1] A. Waseem, et al., Physica Status Solidi (A), p. 2200616, 2022. [2] Z. Xia, et al.,IEEE EDL, 39(4), 568–571, 2018.

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9:45 AM EG+BG+MD-WeM-6 Electrical and Optical Properties of Melt-Grown Mn Doped β-Ga2O3
Benjamin Dutton, Cassandra Remple, Jani Jesenovec (Washington State University); Joel Varley, Lars Voss (Lawrence Livermore National Laboratory); Matthew McCluskey, John McCloy (Washington State University)
Several acceptor dopants have been explored in β-Ga2O3 to produce semi-insulating substrates and epitaxial films. Fe and Mg make up the majority of research thus far, however, other transition metals provide potential alternatives for optimized performance. β-Ga2O3 bulk single crystals were grown by the Czochralski and vertical gradient freeze methods with a nominal dopant concentration of 0.25 at.% Mn. Ultraviolet-visible-near infrared spectroscopy and photoluminescence revealed polarization and orientation dependent optical absorptions and a unique orange luminescence. All samples were electrically insulating, indicative of acceptor doping on the order of 109 – 1011 ohm∙cm at room temperature. Actual dopant concentrations of the intentionally doped transition metal and background impurities were determined via glow discharge mass spectrometry, indicating the macro-scale segregation behavior. Laser-ablation inductively-coupled plasma mass spectrometry along with photoluminescence mapping revealed micro-scale segregation of impurity ions. Density functional theory calculations were carried out to elucidate likely site-occupancy and the acceptor level of Mn in the band gap.
10:00 AM EG+BG+MD-WeM-7 Mg and Zn Counter doping of Homoepitaxial β-Ga2O3 Grown by Molecular Beam Epitaxy
Stephen Schaefer, Kingsley Egbo, Steve Harvey, Andriy Zakutayev, Brooks Tellekamp (National Renewable Energy Laboratory)

Gallium oxide has attracted attention as a candidate material for high-power diodes and transistors owing to its wide bandgap and high breakdown voltage. Homoepitaxial β-Ga2O3 has been successfully grown by plasma-assisted molecular beam epitaxy, however it is well-documented that unintentional Si donors at the epitaxial interface lead to the formation of an undesirable parasitic conducting channel. Mg and Zn are deep acceptor levels in β-Ga2O3 and Mg counterdoping by MBE has been shown to compensate unintentional donor impurities. However counterdoping with other elements such as Zn remains sparsely investigated.

We report on Mg and Zn counterdoping in homoepitaxial β-Ga2O3 grown by MBE on (010) Fe-doped (semi-insulating) and (001) Sn-doped (n-type) wafers. A valved cracker source is used for Mg while Zn is evaporated from a conventional effusion cell. Mg- and Zn-doped stacks are measured by secondary ion mass spectroscopy to calibrate the cell temperatures and valve positions to the dopant incorporation. A typical Ga2O3 growth temperature is 600 °C and growth rates are 0.47 – 0.70 Å/s. β-Ga2O3 samples composed of a ~2 nm Mg- or Zn-doped layer and a 300 nm unintentionally doped layer are grown with dopant fluxes ranging from 3.8×10-9 to 2.0×10-8 torr. Counterdoped samples grown on (001) Sn-doped and (010) Fe-doped wafers are processed into vertical and lateral Schottky devices, respectively. In both devices the Ohmic contact is formed by stable 5 nm Ti / 100 nm Au annealed under N2 at 550 °C while the Schottky contact is formed by 30 nm Ni / 100 nm Au. The Schottky devices are characterized by capacitance-voltage (C-V) measurements at 20 kHz.

We find that the C-V characteristics of the vertical Schottky devices grown on (001) Sn-doped Ga2O3 show a reduction in residual capacitance and corresponding increase in depletion width at high reverse bias voltage for the Mg-counterdoped sample compared to an undoped control sample grown under identical conditions. Additionally, the I-V characteristic of the Mg doped device exhibits lower reverse leakage current. These findings are mirrored in lateral Schottky devices grown on (010) Fe-doped Ga2O3 where counterdoping with 1.0×10-8 torr Zn flux results in approximately ~2× reduction of capacitance and effective carrier concentration while counterdoping with the same Mg flux results in ~5× reduction. The C-V results suggest that Mg and Zn effectively compensate unintentional donors in Ga2O3. Experiments including an annealing study of Mg and Zn diffusion in β-Ga2O3 are expected to yield insight to the controllability of counterdoping in Ga2O3. View Supplemental Document (pdf)
10:15 AM EG+BG+MD-WeM-8 Optimizing Si Implantation and Annealing in β-Ga2O3
Katie Gann, Naomi Pieczulewski (Cornell University); Thaddeus Asel (Air Force Research Laboratory); Cameron Gorsak (Cornell University); Karen Heinselman (national renewable Energy Laboratory); Kathleen Smith, Jonathan McCandless (Cornell University); Brent Noesges (Air Force Research Lab); Grace Xing, Debdeep Jena, Hari Nair, David Muller, Michael Thompson (Cornell University)

Optimizing the thermal anneal of Si implanted β-Ga2O3 is critical for low resistance contacts and selective area doping in advanced device structures. We report the impact of annealing time, temperature, and ambient on the activation of ion-implanted Si in β-Ga2O3 at concentrations from 5×1018 to 1×1020 cm-3, and in β-(AlxGa1-x)2O3 (x≤15%) at 5×1019 cm-3. Nearly full activation (>90%) and high mobilities (>70 cm2/V-s) are achieved in β-Ga2O3 with contact resistances below 0.16 Ω-mm. In β-(AlxGa1-x)2O3, initial results are promising with moderate activation (50%) and high mobility (60 cm2/V-s).

UID β-Ga2O3 films were grown by plasma assisted MBE on Fe-doped (010) β-Ga2O3 substrates; comparable β-(AlxGa1-x)2O3 films were grown by MOCVD. Si was implanted at multiple energies to yield 65 or 100 nm box profiles with concentrations of 5×1018, 5×1019, or 1×1020 cm-3. To understand damage accumulation, low and high temperature implants were also studied. Anneals were performed in a UHV-compatible quartz furnace at 1 bar with well-controlled gas ambients.

To maintain β-Ga2O3 stability, PO2 must be greater than 10-9 bar (based on annealing in vacuum or forming gas). For 5×1019 cm-3 Si, full activation is achieved for PO2<10-4 bar while 5×1018 cm-3 tolerates ~10-2 bar. Water vapor is critical even at 1 ppm; at 25 ppm active carriers are reduced by 10x. Optimal results were obtained with H2O below 10 ppb. Based on recovery with subsequent “dry” anneals, we propose an OH-mediated defect compensating Si dopants.

Lattice recovery (mobility) occurs for T > 900 °C, with carriers and mobility increasing with temperature to 1050 °C. However, SIMS shows substantial Si diffusion above 1000 °C with 950 °C the optimal anneal temperature. Activation at 950 °C is maximized between 5 and 20 minutes with shorter times exhibiting slightly lower mobilities while longer times result in carrier deactivation; this “over-annealing” behavior occurs at all temperatures and becomes more significant at high concentrations. Room temperature implants to 1×1020 cm-3 are shown to fully activate under these optimal conditions.

To understand lattice damage recovery, implants at varying temperatures were characterized by XRD, Rutherford Backscattering Channeling (RBS/C), and STEM. XRD showed no second phases under any conditions. RBS/C and STEM showed only partial amorphization with remnant aligned β-Ga2O3. We propose a model to explain the efficient activation based on 3D lattice recovery in the absence of full amorphization.

View Supplemental Document (pdf)
10:30 AM BREAK
Session Abstract Book
(331KB, Aug 7, 2023)
Time Period WeM Sessions | Abstract Timeline | Topic EG Sessions | Time Periods | Topics | GOX 2023 Schedule