Improved morphology for epitaxial growth on 4° off-axis 4H-SiC substrates

A process optimization of the growth of silicon carbide (SiC) epilayers on 4° off-axis 4H-SiC substrates is reported. Process parameters such as growth temperature, C/Si ratio and temperature ramp-up conditions are optimized for the standard non-chlorinated growth in order to grow smooth epilayers without step bunching and triangular defects. The growth of 6-μm-thick n-type-doped epitaxial layers on 75-mm-diameter wafers is demonstrated as well as that of 20-μm-thick layer. The optimized process was then transferred to a chloride-based process and a growth rate of 28 μm/h was achieved without morphology degradation. A low growth temperature and a low C/Si ratio are the key parameters to reduce both the step bunching and the formation of triangular defects.     

Bulk GaN crystals grown by HVPE

We succeeded in preparing very thick c-plane bulk gallium nitride (GaN) crystals grown by hydride vapor phase epitaxy. Growth of the bulk GaN crystals was performed on templates with 3 μm GaN layer grown by metal organic chemical vapor deposition on (0 0 0 1) sapphire substrates. Colorless freestanding bulk GaN crystals were obtained through self-separation processes. The crystal's diameter and thickness were about 52 and 5.8 mm, respectively. No surface pits were observed within an area of 46 mm diameter of the bulk GaN crystal. The dislocation density decreased with growth direction (from N-face side to Ga-face side) and ranged from 5.1×10⁶ cm⁻² near the N-face surface to 1.2×10⁶ cm⁻² near the Ga-face. A major impurity was Si, and other impurities (O, C, Cl, H, Fe, Ni and Cr) were near or below the detection limits by SIMS measurements.     

MOVPE growth of InN buffer layers on sapphire

We report on the MOCVD growth of InN buffer layers on sapphire substrate for InN growth. The approach used assumes that an optimized InN buffer layer has to exhibit at least the same crystalline quality and sapphire surface coverage than the GaN buffer layers allowing to grow high crystalline quality GaN on sapphire. The buffer layers were characterized by AFM and GID measurements. Sapphire nitridation was investigated: it has a strong influence on in-plane crystalline quality. Two kinds of buffer layers were optimized according to the GaN buffer layer specifications: one of them only presented In droplets at its surface. It was shown that the small amount of In droplets increases the adatoms mobility of the main layer overgrown, leading to a 25% decrease of its in-plane mosaicity, compared to InN films directly grown on sapphire. To achieve a same improvement on InN buffer layer free of In droplets, the InN main layer growth temperature had to be increased from 550 °C. to 600 °C.     

Growth characteristics of AlN on sapphire substrates by modified migration-enhanced epitaxy

We investigated the effect of growth parameters for obtaining high-quality AlN grown directly on sapphire substrates by a hybridized method, derived from simultaneous source supply and conventional migration-enhanced epitaxy. At an optimal growth temperature of 1200 °C, AlN was atomically smooth and pit-free, while below and above 1200 °C, AlN was rough and with pits, respectively. Surface morphologies also depended on the V/III ratio. Rough surfaces became atomically smooth but then pits appeared, as the V/III ratio increased. The crystallinity revealed by X-ray diffraction changed accordingly. The 600-nm-thick AlN grown under the optimal conditions showed X-ray line widths of as narrow as ∼43 and ∼250 arcsec for (0 0 0 2) and (1 0 1¯ 2) diffractions, respectively.     

Improved hot-wall MOCVD growth of highly uniform AlGaN/GaN/HEMT structures

The inherent advantages of the hot-wall metal organic chemical vapor deposition (MOCVD) reactor (low temperature gradients, less bowing of the wafer during growth, efficient precursor cracking) compared to a cold-wall reactor make it easier to obtain uniform growth. However, arcing may occur in the growth chamber during growth, which deteriorates the properties of the grown material. By inserting insulating pyrolytic BN (PBN) stripes in the growth chamber we have completely eliminated this problem. Using this novel approach we have grown highly uniform, advanced high electron mobility transistor (HEMT) structures on 4″ semi-insulating (SI) SiC substrates with gas-foil rotation of the substrate. The nonuniformities of sheet resistance and epilayer thickness are typically less than 3% over the wafer. The room temperature hall mobility of the 2DEG is well above 2000 cm²/V s and the sheet resistance about 270 Ω/sqr.     

Fabrication of a GaN lateral polarity junction by metalorganic chemical vapor deposition

A fabrication process for growth of GaN lateral polarity junctions consisting of Ga-polar and N-polar domains grown simultaneously side-by-side on c-plane sapphire was developed using the polarity control scheme. An ammonia-annealing step following deposition and patterning of a thin low-temperature AlN nucleation layer played a crucial role in avoiding mixed-polarity growth of the remaining AlN nucleation layer, as well as in nitriding the bare sapphire surface to facilitate growth of N-polar GaN. The achievement of both polar domains, free from inversion domains within a contiguous domain, led to Ga-polar domain exhibiting featureless morphology with highly resistive characteristics, while N-polar domains exhibited hexagonally faceted morphology and were highly conductive.     

Defect reduction of laterally regrown GaN on GaN/patterned sapphire substrates

Structural properties of GaN epilayers on wet-etched protruding and recess-patterned sapphire substrates (PSSs) have been investigated in detail using high-resolution double-crystal X-ray diffraction (DCXRD) and etch-pit density methods. The DCXRD results reveal various dislocation configurations on both types of PSSs. The etch pits of GaN on the recess PSS exhibit a regular distribution, i.e. less etch pits or threading dislocation density (TDD) onto the recess area than those onto the sapphire mesas. On the contrary, an irregular distribution is observed for the etch pits of GaN on the protruding PSS. A higher crystal quality of the GaN epilayer grown onto the recess PSS can be achieved as compared with that onto the protruding PSS. These data reflect that the GaN epilayer on the recess PSS could be a better template for the second epitaxial lateral overgrowth (ELOG) of GaN. As a result, the GaN epilayers after the ELOG process display the TDDs of around ∼10⁶ cm⁻².     

Alternative precursors for MOVPE growth of InN and GaN at low temperature

We report on the use of dimethylhydrazine (DMHy) and tertiarybuthylhydrazine (TBHy), as alternative nitrogen precursor for GaN low-temperature growth, as well as to improve the InN growth rate. Lowering the GaN growth temperature, would allow growing InN/GaN heterostructures by MOVPE, without damaging the InN layers. Increasing the low InN MOVPE growth rate is of major importance to grow reasonably thick InN layers. In this respect, triethylindium (TEIn) was also used as an alternative to trimethylindium (TMIn).     

Mg segregation in a (1 1¯ 0 1) GaN grown on a 7° off-axis (0 0 1) Si substrate by MOVPE

Redistribution behavior of magnesium (Mg) in the N-terminated (1 1¯ 0 1) gallium nitride (GaN) has been investigated. A nominally undoped GaN layer was grown on a heavily Mg-doped GaN template by metalorganic vapor-phase epitaxy (MOVPE). Mg dopant profiles were measured by secondary ion mass spectrometry (SIMS) analysis. A slow decay of the Mg concentration was observed in the nominally undoped GaN layer due to the surface segregation. The calculated decay lengths of the (1 1¯ 0 1) GaN are ∼75–85 nm/decade. These values are shorter than the decay length determined in the sample grown on the Ga-terminated (0 0 0 1) GaN. This result indicates that Mg exhibited weak surface segregation in the (1 1¯ 0 1) GaN as compared to the (0 0 0 1) GaN. The weak surface segregation is in agreement with the high efficiency of Mg incorporation on the (1 1¯ 0 1) face. The high density of hydrogen was obtained in the (1 1¯ 0 1) GaN, which might enhance the Mg incorporation.     

Homoepitaxy on bulk ammonothermal GaN

In this work results of extensive characterization of homoepitaxial layers grown on truly bulk ammonothermal gallium nitride (GaN) substrates are presented. The 2-μm-thick layers were deposited using metalorganic chemical vapor deposition. The photoluminescence (PL) and reflectance results show very intensive, perfectly resolved excitonic structure in range of band-edge emission of gallium nitride. This structure consists of both lines related to free excitons emission and very narrow lines (full-width at half-maximum (FWHM) value of the order of 0.3 meV) related with excitons bound to neutral acceptor and different neutral donors. In high excitation condition the biexciton emission was observed. The luminescence is uniform in the whole sample surface range. High PL homogeneity corresponds with structural and microscopic measurements performed on these layers. It proves that ammonothermal GaN substrates with perfect crystalline properties enable to grow excellent quality, strain-free homoepitaxial layers.     

Theoretical investigation on the decomposition process of GaN(0 0 0 1) surface under a hydrogen atmosphere

The activation energies for Ga and N desorption from a GaN surface were calculated using the density functional theory to understand the detailed decomposition process of the hydrogen terminated GaN(0 0 0 1) Ga and N surfaces under a hydrogen atmosphere. It was found that the Ga atoms on the hydrogen terminated GaN(0 0 0 1) Ga surface desorbed as GaH molecules from the surface while the N atoms on the hydrogen terminated GaN(0 0 0 1) N surface desorbed as NH₃ molecules from the surface. The desorption energies of GaH and NH₃ on the hydrogen terminated surface were more consistent with the previous experimental values than those on the ideal surface. These results suggest that the initial surface structure of the GaN(0 0 0 1) surface is terminated with hydrogen.     

N-face GaN growth on c-plane sapphire by metalorganic chemical vapor deposition

In this work, we report the growth of smooth, high-quality N-face GaN on c-plane sapphire by metalorganic chemical vapor deposition. It is found that the nitridation temperature of sapphire has a critical effect on the surface morphology of N-face GaN. Sapphire after a severe nitridation gives rise to a high density of hexagonal hillocks during N-face GaN growth. Smooth N-face GaN has been grown on appropriately nitridized sapphire. The N-polarity of the GaN film has been confirmed with no inversion domain by convergent beam electron diffraction. Controlled growth interruption is carried out to study the nucleation evolution during N-face GaN growth, which is found distinctly different from the two-step growth of Ga-face GaN. Atomically smooth N-face GaN has been achieved with comparable structural quality to Ga-face GaN.     

Acceptor incorporation in SiC epilayers grown at high growth rate with chloride-based CVD

A systematic p-type doping study has been performed on 4H- and 6H-silicon carbide (SiC) epilayers grown at high growth rate using chloride-based chemical vapor deposition. The effect of temperature, pressure, growth rate, C/Si-, Cl/Si-ratios and dopant flow on the incorporation of the acceptor atoms aluminum and boron has been studied. The C/Si-ratio on the aluminum incorporation has similar behavior to what has been reported for the standard non-chlorinated low growth rate process, while no clear effect of C/Si-ratio was observed for the boron incorporation. A higher Cl/Si-ratio seems to lead to lower the aluminum and boron incorporation either due to more effective silicon supply at high Cl/Si-ratio or due to removal of dopant atoms from the surface by chlorine. The doping concentration is stable to the variations in silicon molar fraction, growth pressure and growth temperature for the aluminum-doped layers. Also p-type doping with gallium was tested.     

Molecular beam epitaxial growth of hexagonal boron nitride on Ni(1 1 1) substrate

We demonstrate hexagonal boron nitride (h-BN) epitaxial growth on Ni(1 1 1) substrate by molecular beam epitaxy (MBE) at 890 °C. Elemental boron evaporated by an electron-beam gun and active nitrogen generated by a radio-frequency (RF) plasma source were used as the group-III and -V sources, respectively. Reflection high-energy electron diffraction revealed a streaky (1×1) pattern, indicative of an atomically flat surface in the ongoing growth. Correspondingly, atomic force microscopy images exhibit atomically smooth surface of the resulting h-BN film. X-ray diffraction characterization confirmed the crystallinity of the epitaxial film to be h-BN, and its X-ray rocking curve has a full-width at half-maximum of 0.61°, which is the narrowest ever reported for h-BN thin film. The epitaxial alignments between the h-BN film and the Ni substrate were determined to be [0 0 0 1]_h−BN∥[1 1 1]_Ni, [1 1 2¯ 0]_h−BN∥[1¯ 1 0]_Ni, and [1 1¯ 0 0]_h−BN∥[1¯ 1¯ 2]_Ni.     

One-sidewall-seeded epitaxial lateral overgrowth of a-plane GaN by metalorganic vapor-phase epitaxy

The selective regrowth of GaN during sidewall-seeded epitaxial lateral overgrowth was performed. In addition to adjusting the V/III ratio, control of offset angle of the sidewall was found to be effective for realizing one-sidewall-seeded a-plane (1 1 2¯ 0) GaN on r-plane (1 1¯ 0 2) sapphire. The number of coalescence regions on the grooves was reduced, and threading-dislocation and stacking-fault densities as low as 10⁶–10⁷ cm⁻² and 10³–10⁴ cm⁻¹, respectively, were successfully realized.     

Characterizations of GaN films and AlGaN/GaN heterostructures on vicinal sapphire (0 0 0 1) substrates grown by MOCVD

GaN films and AlGaN/GaN heterostructures grown on vicinal sapphire (0 0 0 1) substrates by metalorganic chemical vapor deposition (MOCVD) are investigated. It is found that surface morphologies of GaN films depend on the vicinal angle, however, they are not sensitive to the inclination directions of the substrate. The optimized vicinal angle for obtaining excellent surface morphology is around 0.5°. This conclusion is also confirmed by characterizing the electrical property of two-dimensional electron gas (2DEG) in the AlGaN/GaN heterostructure.     

Fabrication of freestanding m-plane GaN wafer by using the HVPE technique on an aluminum carbide buffer layer on an m-plane sapphire substrate

A freestanding m-plane GaN wafer is fabricated by using the hydride vapor-phase epitaxy (HVPE) technique on an aluminum carbide buffer layer on an m-plane sapphire substrate. X-ray pole-figure measurements show a clear m-plane orientation of the GaN surface. The full-width at half-maximum (FWHM) of GaN (1 1¯ 0 0) X-ray rocking curve (XRC) with the scattering vector along the [1 1 2¯ 0] direction is approximately 800 arcsec; this indicates good crystallinity. On the other hand, the FWHM for the case in which the scattering vector is oriented along the [0 0 0 1] direction is broad; this suggests the influence of structural defects along this direction. In fact, basal plane stacking faults (BSF) with a density of approximately 3×10⁵ cm⁻¹ is observed by transmission electron microscopy (TEM). The preparation of a 45-mm-diameter m-plane GaN wafer due to spontaneous separation of the GaN layer from the sapphire substrate is demonstrated.     

Effect of an applied electric current in epitaxial growth of GaAs layer on patterned GaAs substrate

Selective epitaxial growth of a GaAs layer on SiN_x masked Si-doped semi-insulating (1 0 0) GaAs substrate was performed by current-controlled liquid-phase epitaxy (CCLPE) in the conventional liquid-phase epitaxy. Experiments were carried out with and without the application of electric current. Surface morphology of (1 0 0) facet of the grown layer and the vertical and lateral growth rates were significantly improved under applied electric current. A thick layer of about 330 μm was achieved at relatively low growth time of 6 h with a current density of 20 Acm⁻². The epitaxial growth is realized by both electromigration of the solute and supercooling under a constant rate of furnace cooling. The dislocation density of the grown layer was significantly reduced, compared with that of the substrate (4×10⁴ cm²).     

Growth of InN films and nanostructures by MOVPE

Since a few years, a lot of research efforts have been devoted to InN, the least known of the semiconducting group-III nitrides. Most of the samples available today have been grown using the molecular beam epitaxy technique, and fewer using the metal organic vapor phase epitaxy (MOVPE) method. Whatever the method, the growth of InN is extremely challenging, in particular due to the fact that no lattice matched substrate is available.     

Growth of InxGa1−xN quantum dots by nitridation of nano-alloyed droplet method using MOCVD

In_xGa_1−xN quantum dots (QDs) were grown on GaN/sapphire (0 0 0 1) substrates by employing nitridation of nano-alloyed droplet (NNAD) method using metal-organic chemical vapor deposition (MOCVD). In+Ga alloy droplets were initially formed by flowing the precursors TMIn and TMGa. Density of the In+Ga alloy droplets was increased with increasing precursors flow rate; however, the droplet size was scarcely changed in the range of about 100–200 nm. Two cases of In_xGa_1−xN QDs growth were investigated by varying the nitridation time and the growth temperature. It was observed that the In_xGa_1−xN QDs size can be easily changed by controlling the nitridation process at the temperature between 680 and 700 °C for the time of 5–30 min. Self-assembled In_xGa_1−xN QDs were successfully grown by employing NNAD method.