Authors: Serguei I. Maximenko, Jaime A. Freitas, N.Y. Garces, E.R. Glaser, Mark A. Fanton
Abstract: The behavior of the D1 center in semi-insulating 4H-SiC substrates revealed by
low-temperature photoluminescence was investigated after post-growth high temperature anneals
between 1400 and 2400oC. The influence of different post-anneal cooling rates was also studied. The
optical signature of D1 was observed up to 2400oC with intensity maxima at 1700 and 2200oC. We
propose that the peak at 1700°C can be related to the formation and subsequent dissociation of SiC
native defects. It was found that changes in the post-annealing cooling rate drastically influence the
behavior of the D1 center and the concentrations of the VC, VSi, VC-VSi and VC-CSi lattice defects.
429
Authors: N.Y. Garces, E.R. Glaser, W.E. Carlos, Mark A. Fanton
Abstract: We have recently explored the nature and stability of native defects in high-purity
semi-insulating 4H-SiC bulk substrates grown by PVT and HTCVD methods after post-growth
anneal treatments up to 2400oC using electron paramagnetic resonance (EPR) and low-temperature
photoluminescence (PL) experiments. In the present study we have extended these investigations to
SI 4H-SiC subjected to the same post-growth high-temperature anneal treatments, where significantly
enhanced carrier lifetimes have been reported for such conditions, but cooled at different rates ranging
from ~2-25oC/min. Previously, the intensities of the native defects decreased monotonically with
anneals from 1200–1800oC; however, it was recently observed that several of these defects reappear
after annealing at 2100oC and above. Our results illustrate the effects of the post-growth anneal
treatments and cool-down rates on the concentrations of native defects.
389
Authors: Hun Jae Chung, Sung Wook Huh, A.Y. Polyakov, Saurav Nigam, Qiang Li, J.R. Grim, Marek Skowronski, E.R. Glaser, W.E. Carlos, Jaime A. Freitas, Mark A. Fanton
Abstract: Undoped 6H- and 4H-SiC crystals were grown by Halide Chemical Vapor Deposition
(HCVD). Concentrations of impurities were measured by various methods including
secondary-ion-mass spectrometry (SIMS). With increasing C/Si ratio, nitrogen concentration
decreased and boron concentration increased as expected for the site-competition effect. Hall-effect
measurements on 6H-SiC crystals showed that with the increase of C/Si ratio from 0.06 to 0.7, the
Fermi level was shifted from Ec-0.14 eV (nitrogen donors) to Ev+0.6 eV (B-related deep centers).
Crystals grown with C/Si > 0.36 showed high resistivities between 1053 and 1010 4cm at room
temperature. The high resistivities are attributed to close values of the nitrogen and boron
concentrations and compensation by deep defects present in low densities.
625
Authors: Howard E. Smith, Kurt G. Eyink, W.C. Mitchel, M.C. Wood, Mark A. Fanton
Abstract: A multiple data point version of the industry standard, two data point raster-changing
procedure is employed to measure low levels (< 1 x 1017 atoms/cm3) of nitrogen (N) in silicon
carbide (SiC) by SIMS (Secondary Ion Mass Spectrometry). A current-changing procedure is also
employed. Together, these are used evaluate the assumptions of the standard method, to separate
and measure the components of background signal, and to improve upon the precision and accuracy
of the standard method. The risk of poor precision in the two-point method is demonstrated, as is
the improvement provided by the multiple-point method. Results show that, in addition to the wellknown
N memory background, adsorption background can contribute significantly to the N signal.
In general, establishing the presence of adsorption gas in this way can be used to warn of the
presence of ionization background, which is not measurable per se.
617
Authors: W.E. Carlos, E.R. Glaser, N.Y. Garces, B.V. Shanabrook, Mark A. Fanton
Abstract: High temperature anneals were used to study the evolution of native defects in semiinsulating
(SI), ultrahigh purity SiC using electron paramagnetic resonance (EPR), infrared and
visible photoluminescence (PL) and COREMA (Contactless Resistivity Mapping) measurements.
In EPR we observe a defect that we tentatively identify as VC-CSi-VC. The EPR intensities of this
defect and the UD1 IRPL increase significantly with annealing in all samples.
531
Authors: Sung Wook Huh, A.Y. Polyakov, Hun Jae Chung, Saurav Nigam, Marek Skowronski, E.R. Glaser, W.E. Carlos, Mark A. Fanton, N.B. Smirnov
Abstract: Deep electron and hole traps were studied in a series of high purity 6H-SiC single crystals
grown by Halide Chemical Vapor Deposition (HCVD) method at various C/Si flow ratios and at
temperatures between 2000 oC and 2100 oC. Characterization included Low Temperature
Photoluminescence (LTPL), Deep Level Transient Spectroscopy (DLTS), Minority Carrier Transient
Spectroscopy (MCTS), and Thermal Admittance Spectroscopy (TAS) measurements. Concentrations
of all deep traps were shown to strongly decrease with increased C/Si flow ratio and with increased
growth temperature. The results indicate that the majority of deep centers in 6H-SiC crystals grown by
HCVD are due to native defects or complexes of native defects promoted by Si-rich growth
conditions. The observed growth temperature dependence of residual donor concentration and traps
density is explained by increasing the effective C/Si ratio at higher temperatures for the same nominal
ratio of C and Si flows.
497
Authors: Mark A. Fanton, Qiang Li, A.Y. Polyakov, R.L. Cavalero, R.G Ray, B.E. Weiland, Marek Skowronski
Abstract: The effects of H2 addition to the growth ambient during physical vapor transport
(PVT) growth of 6H and 4H SiC were investigated using SIMS, DLTS and Hall effect
measurements. Using this hybrid physical-chemical vapor transport (HPVT) approach, boules were
grown using Ar-H2 and He-H2 mixtures with H2 concentrations up to 50 at%. Thermodynamic
modeling suggests that addition of H2 improves the carbon transport in HPVT compared to standard
PVT. This should lead to a substantial decrease in the concentration of residual N donors and the
concentration of electron traps. This is confirmed by the experimental results. As expected, the
source transport rate increased as H2 was added to the growth environment due to increased C
transport. The background nitrogen concentration and the free electron density decreased
significantly with increasing H2 concentration. The formation of electron traps (activation energies
of 0.4 eV, 0.6-0.65 eV, 0.7 eV, 0.9 eV and 1 eV) was also strongly suppressed. These changes were
observed for H2 concentrations as low as 4 at%. The decreased N concentration improves the
ability to produce high resistivity SiC material, and for H2 concentrations as high as 10-25%, the
very first wafers cut from the seed end of the boules have a resistivity exceeding 106 cm.
103
Authors: Qiang Li, A.Y. Polyakov, Marek Skowronski, Edward Sanchez, Mark J. Loboda, Mark A. Fanton, Timothy Bogart, Rick D. Gamble, N.B. Smirnov, Yuri Makarov
Abstract: For undoped 6H-SiC boules grown by physical vapor transport the variations of resistivity,
of the type and density of deep electron and hole traps, and of the concentration of nitrogen and boron
were studied as a function of position in the cross section normal to the growth axis and along the
growth direction. It was observed that the concentrations of all deep electron and hole traps decreased
when moving from seed to tail of the boule and from the center to the edge of the wafers. Modeling of
the growth process suggests that the C/Si ratio increases in a similar fashion and could be responsible
for observed changes. We also discuss the implications of such stoichiometry changes on
compensation mechanisms rendering the crystals semi-insulating and on electrical uniformity of
SI-SiC wafers.
51
Authors: Mark A. Fanton, R.L. Cavalero, R.G Ray, B.E. Weiland, W.J. Everson, David Snyder, Rick D. Gamble, Ed Oslosky
Abstract: The effects of growth conditions, diffusion barrier coatings, and hot zone materials
on B incorporation in 6H-SiC crystals grown by physical vapor transport (PVT) were evaluated.
Development of high purity source material with a B concentration less than 1.8x1015 atoms/cm3,
was critical to the growth of boules with a B concentration less than 3.0x1016 atoms/cm3.
Application of refractory metal carbide coatings to commercial graphite to serve as boron diffusion
barriers and the use of very high purity pyrolytic graphite components ultimately led to the growth
of SiC boules with boron concentrations as low as 2.4x1015 atoms/cm3. The effect of growth
temperature and pressure were closely examined over a range from 2100°C to 2300°C and 5 to 13.5
Torr. This range of growth conditions and growth rates had no effect on B incorporation. Attempts
to alter the gas phase stoichiometry through addition of hydrogen gas to the growth environment
also had no impact on B incorporation. These results are explained by considering site competition
effects and the ability of B to diffuse through the graphite growth cell components.
47
Authors: Saurav Nigam, Hun Jae Chung, Sung Wook Huh, J.R. Grim, A.Y. Polyakov, Mark A. Fanton, B.E. Weiland, David Snyder, Marek Skowronski
Abstract: Growth rates and relative stability of 6H- and 4H-SiC have been studied as a function of
growth conditions during Halide Chemical Vapor Deposition (HCVD) process using silicon
tetrachloride, propane and hydrogen as reactants. The growth temperature ranged from 2000 to 2150
oC. Silicon carbide crystals were deposited at growth rates in the 100-300 μm/hr range in both
silicon- and carbon-supply limited regimes by adjusting flows of all three reactants. High resolution
x-ray diffraction measurements show that the growth on Si-face of 6H- and C-face of 4H-SiC
substrates resulted in single crystal 6H- and 4H-SiC polytype, respectively. The growth rate results
have been interpreted using thermodynamic equilibrium calculations.
27