Boris N. Feigelson

Multicycle rapid thermal annealing optimization of Mg-implanted GaN: Evolution of surface, optical, and structural properties

The first step of a multi-cycle rapid thermal annealing process was systematically studied. The surface, structure, and optical properties of Mg implanted GaN thin films annealed at temperatures ranging from 900 to 1200 °C were investigated by Raman spectroscopy, photoluminescence, UV-visible spectroscopy, atomic force microscopy, and Nomarski microscopy. The GaN thin films are capped with two layers of in-situ metal organic chemical vapor deposition -grown AlN and annealed in 24 bar of N2 overpressure to avoid GaN decomposition. The crystal quality of the GaN improves with increasing annealing temperature as confirmed by UV-visible spectroscopy and the full widths at half maximums of the E2 and A1 (LO) Raman modes. The crystal quality of films annealed above 1100 °C exceeds the quality of the as-grown films. At 1200 °C, Mg is optically activated, which is determined by photoluminescence measurements. However, at 1200 °C, the GaN begins to decompose as evidenced by pit formation on the surface of the samp...

Characterization of a selective AlN wet etchant

The effects of a selective AlN wet etchant, AZ400K, on the morphology and chemical composition of capped and uncapped GaN surfaces were investigated. After etching an uncapped GaN thin film at 80 °C for 8 h, the surface morphology was unchanged. After an annealing pulse of 1500 °C was applied, AlN-encapsulated GaN surfaces exhibited morphology change due to surface rearrangement. No reaction occurred between the GaN and AlN, preventing the complete removal of AlN. AZ400K was found to completely etch AlN without damaging the underlying GaN film, thus enabling plasma-free processing of power and optoelectronic devices.

Defect reduction in MBE-grown AlN by multicycle rapid thermal annealing

Multicycle rapid thermal annealing (MRTA) is shown to reduce the defect density of molecular beam epitaxially grown AlN films. No damage to the AlN surface occurred after performing the MRTA process at 1520°C. However, the individual grain structure was altered, with the emergence of step edges. This change in grain structure and diffusion of AlN resulted in an improvement in the crystalline structure. The Raman E2 linewidth decreased, confirming an improvement in crystal quality. The optical band edge of the AlN maintained the expected value of 6.2 eV throughout MRTA annealing, and the band edge sharpened after MRTA annealing at increased temperatures, providing further evidence of crystalline improvement. X-ray diffraction shows a substantial improvement in the (002) and (102) rocking curve FWHM for both the 1400 and 1520°C MRTA annealing conditions compared to the as-grown films, indicating that the screw and edge type dislocation densities decreased. Overall, the MRTA post-growth annealing of AlN lowers defect density, and thus will be a key step to improving optoelectronic and power electronic devices.

Electron Backscatter Diffraction Study of Hexagonal Boron Nitride Growth on Cu Single-Crystal Substrates

Hexagonal boron nitride (h-BN) is an important material for the development of new 2D heterostructures. To enable this development, the relationship between crystal growth and the substrate orientation must be explored and understood. In this study, we simultaneously grew h-BN on different orientations of Cu substrates to establish the impact of substrate structure on the growth habit of thin h-BN layers. The substrates studied were a polycrystalline Cu foil, Cu(100), Cu(110), and Cu(111). Fourier transform grazing-incidence infrared reflection absorption spectroscopy (FT-IRRAS) was used to identify h-BN on copper substrates. X-ray photoelectron spectroscopy (XPS) was used to determine the effective thickness of the h-BN. Scanning electron microscopy (SEM) and electron backscatter diffraction (EBSD) were used to measure the morphology of the films and postgrowth crystal structure of the Cu substrates, respectively. Combining the SEM and EBSD images allowed for the correlation between h-BN film coverage and the crystal structure of Cu. It was found that the growth rate was inversely proportional to the surface free energy of the Cu surface, with Cu(111) having the most h-BN surface coverage. The Cu foil predominately crystallized with a (100) surface orientation, and likewise had a film coverage very close to the Cu(100).

Efficient Incorporation of Mg in Solution Grown GaN Crystals

Detailed spectrometry and optical spectroscopy studies carried out on GaN crystals grown in solution detect and identify Mg as the dominant shallow acceptor. Selective etching of crystals with higher Mg levels than that of the donor concentration background indicates that Mg acceptors incorporate preferentially in the N-polar face. Electrical transport measurements verified an efficient incorporation and activation of the Mg acceptors. These results suggest that this growth method has the potential to produce p-type doped epitaxial layers or p-type substrates characterized by high hole concentration and low defect density.

Comparison of AlN encapsulants for high-temperature GaN annealing

Four different capping structures for high-temperature annealing of GaN were studied. The studied caps included a two-layer MOCVD-deposited cap and three different MOCVD + sputtered layer capping structures. After an annealing pulse of 1500 °C, the MOCVD cap surface roughened due to decomposition of the underlying GaN. GaN decomposition was evident via observation of thermal decomposition pits after etching of the AlN caps. It was found that the combination of an MOCVD cap with a sputtered cap greatly reduced the amount of GaN decomposition as the density of thermal etch pits decreased by 99.4%.

Below the Hall–Petch Limit in Nanocrystalline Ceramics

Reducing the grain size of metals and ceramics can significantly increase strength and hardness, a phenomenon described by the Hall-Petch relationship. The many studies on the Hall-Petch relationship in metals reveal that when the grain size is reduced to tens of nanometers, this relationship breaks down. However, experimental data for nanocrystalline ceramics are scarce, and the existence of a breakdown is controversial. Here we show the Hall-Petch breakdown in nanocrystalline ceramics by performing indentation studies on fully dense nanocrystalline ceramics fabricated with grain sizes ranging from 3.6 to 37.5 nm. A maximum hardness occurs at a grain size of 18.4 nm, and a negative (or inverse) Hall-Petch relationship reduces the hardness as the grain size is decreased to around 5 nm. At the smallest grain sizes, the hardness plateaus and becomes insensitive to grain size change. Strain rate studies show that the primary mechanism behind the breakdown, negative, and plateau behavior is not diffusion-based. We find that a decrease in density and an increase in dissipative energy below the breakdown correlate with increasing grain boundary volume fraction as the grain size is reduced. The behavior below the breakdown is consistent with structural changes, such as increasing triple-junction volume fraction. Grain- and indent-size-dependent fracture behavior further supports local structural changes that corroborate current theories of nanocrack formation at triple junctions. The synergistic grain size dependencies of hardness, elasticity, energy dissipation, and nanostructure of nanocrystalline ceramics point to an opportunity to use the grain size to tune the strength and dissipative properties.

Growth per cycle of alumina atomic layer deposition on nano- and micro-powders

Core–shell powders consisting of a tungsten particle core and thin alumina shell have been synthesized using atomic layer deposition in a rotary reactor. Standard atomic layer deposition of trimethylaluminum/water at 150 °C utilizing a microdosing technique was performed on four different batches of powder with different average particle sizes. The particle size of the powders studied ranges from ∼25 to 1500 nm. The high mass-thickness contrast between alumina and tungsten in transmission electron microscopy images demonstrates that the particle core/shell interface is abrupt. This allows for the uncomplicated measurement of alumina thickness and therefore the accurate determination of growth per cycle. In agreement with prior works, the highest growth per cycle of ∼2 A/cycle occurred on the batch of powder with the smallest average particle size and the growth per cycle decreased with increasing average particle size of a powder batch. However, the growth per cycle of the alumina film on an individual pa...

Single n-GaN microwire / p-Silicon thin film heterojunction light-emitting diode

The emission and waveguiding properties of individual GaN microwires as well as devices based on an n-GaN microwire/p-Si (100) junction were studied for relevance in optoelectronics and optical circuits. Pulsed photoluminescence of the GaN microwire excited in the transverse or longitudinal direction demonstrated gain. These n-type GaN microwires were positioned mechanically or by dielectrophoretic force onto pre-patterned electrodes on a p-type Si (100) substrate. Electroluminescence from this p-n point junction was characteristic of a heterostructure light-emitting diode. Additionally, waveguiding was observed along the length of the microwire for light originating from photoluminescence as well as from electroluminescence generated at the p-n junction.

Ga2O3 Schottky barrier and heterojunction diodes for power electronics applications

We present novel approaches for the development of Ga2O3 Schottky barrier and heterojunction diodes. Samples of β- Ga2O3 were first annealed in N2 and O2 to demonstrate the effect of annealing on the carrier concentration. Cathodoluminescence and electron spin resonance measurements were also performed. Schottky barrier diodes on asgrown and O2-annealed epitaxial Ga2O3 films were fabricated and breakdown voltages were compared. Lower reverse current and a breakdown voltage of about 857 V were measured on the O2-annealed device. Finally, we report preliminary results from the development of anisotype heterojunctions between n-type Ga2O3 with a sputtered NiO layer. Rectifying current-voltage characteristics were obtained when the NiO was deposited both at room temperature and at 450 °C.