Growth and characterisation of GaN with reduced dislocation density

Two GaN MOVPE growth methods to reduce the threading dislocation (TD) density have been explored. The combined effects of (1) in situ SiN_x masking of the sapphire substrate and (2) starting the epitaxial growth at low V-to-III ratio on the GaN film quality were studied by atomic force microscopy, transmission electron microscopy and high-resolution X-ray diffraction. It was found that the annealing condition of the low-temperature nucleation layer after in situ SiN_x masking is critical in order to decrease the density of nucleation sites and hence increase the average grain size to about 5 μm. However, the coalescence of large grains with vertical side facets results in the formation of dense bundles of TDs at the grain boundaries combined with large numbers of basal-plane dislocation loops throughout the film. The formation of these dislocations can be prevented by starting the epilayer growth at low V-to-III ratio, resulting in the formation of grains with inclined side facets. The interaction of the TDs with the inclined side facets causes the dislocations to bend 90 as the grains grow in size and coalesce. GaN films with dislocation densities as low as 1×10⁸ cm⁻², giving full-width at half-maximum values of 180 and 220 arcsec for respectively (002) and (302) omega scans, were achieved by the combination of in situ masking and low V–III ratio epilayer growth. Hall carrier mobility values in excess of 900 cm² V ⁻¹ s⁻¹ were deduced for Si-doped layers.     

Dependences of structural and electrical properties on thickness of polycrystalline Ga-doped ZnO thin films prepared by reactive plasma deposition

Polycrystalline Ga-doped (Ga content: 4 wt%) ZnO (GZO) thin films were deposited on glass substrates at 200 C by a reactive plasma deposition with DC arc discharge technique. The dependences of structural and electrical properties of GZO films on thickness, ranging from 30 to 560 nm, were investigated. Carrier concentration, n, and Hall mobility, μ, increases with increasing film thickness below 100 nm, and then the n remains nearly constant and the μ gradually increases until the thickness reaches 560 nm. The resistivity obtained of the order of 10⁻⁴ Ω cm for these films decreases with increasing film thickness: The highest resistivity achieved is 4.4×10⁻⁴ Ω cm with n of 7.6×10²⁰ cm⁻³ and μ of 18.5 cm²/V s for GZO films with a thickness of 30 nm and the lowest one is 1.8×10⁻⁴ Ω cm with n of 1.1×10²¹ cm⁻³ and μ of 31.7 cm²/V s for the GZO film with a thickness of 560 nm. X-ray diffraction pattern for all the films shows a hexagonal wurtzite structure with its strongly preferred orientation along the c-axis. Full width at half maximum of the (002) preferred orientation diffraction peak of the films decreases with increasing film thickness below 100 nm.     

AlGaN/GaN HEMTs grown on silicon (001) substrates by molecular beam epitaxy

We report the realization of an AlGaN/GaN HEMT on silicon (001) substrate with noticeably better transport and electrical characteristics than previously reported. The heterostructure has been grown by molecular beam epitaxy. The 2D electron gas formed at the AlGaN/GaN interface exhibits a sheet carrier density of 8×10¹² cm⁻² and a Hall mobility of 1800 cm²/V s at room temperature. High electron mobility transistors with a gate length of 4 μm have been processed and DC characteristics have been achieved. A maximum drain current of more than 500 mA/mm and a transconductance g_m of 120 mS/mm have been obtained. These results are promising and open the way for making efficient AlGaN/GaN HEMT devices on Si(001).     

Properties of Si-doped GaN and AlGaN/GaN heterostructures grown by RF-MBE on high resistivity Fe-doped GaN

Silicon-doped GaN epilayers and AlGaN/GaN heterostructures were developed by nitrogen plasma-assisted molecular beam epitaxy on high resistivity iron-doped GaN (0001) templates and their properties were investigated by atomic force microscopy, x-ray diffraction and Hall effect measurements. In the case of high electron mobility transistors heterostructures, the AlN mole fraction and the thickness of the AlGaN barrier employed were in the range of from 0.17 to 0.36 and from 7.5 to 30 nm, respectively. All structures were capped with a 2 nm GaN layer.Despite the absence of Ga droplets formation on the surface, growth of both GaN and AlGaN by RF-MBE on the GaN (0001) surfaces followed a step-flow growth mode resulting in low surface roughness and very abrupt heterointerfaces, as revealed by XRD. Reciprocal space maps around the reciprocal space point reveal that the AlGaN barriers are fully coherent with the GaN layer.GaN layers, n-doped with silicon in the range from 10¹⁵ to 10¹⁹ cm⁻³ exhibited state of the art electrical properties, consistent with a low unintentional background doping level and low compensation ratio. The carrier concentration versus silicon cell temperatures followed an Arhenius behaviour in the whole investigated doping range. The degenerate 2DEG, at the AlGaN/GaN heteroiterfaces, exhibited high Hall mobilities reaching 1860 cm²/V s at 300 K and 10 220 cm²/V s at 77 K for a sheet carrier density of 9.6E12 cm⁻².The two dimensional degenerate electron gas concentration in the GaN capped AlGaN/GaN structures was also calculated by self-consistent solving the Schrödinger–Poisson equations. Comparison with the experimental measured values reveals a Fermi level pinning of the GaN (0001) surface at about 0.8 eV below the GaN conduction band.     

High-quality InAlN/GaN heterostructures grown by metal–organic vapor phase epitaxy

We fabricated high-quality InAlN/GaN heterostructures by metal–organic vapor phase epitaxy (MOVPE). X-ray diffraction measurements revealed that InAlN/GaN heterostructures grown under optimal conditions have flat surfaces and abrupt heterointerfaces. Electron mobility from 1200 to 2000 cm²/V s was obtained at room temperature. To our knowledge, this mobility is the highest ever reported for InAlN/GaN heterostructures. We also investigated the relationship between the Al composition and sheet electron density (N_s) for the first time. N_s increased from 1.0×10¹² to 2.7×10¹³ cm⁻² when the Al composition increased from 0.78 to 0.89.     

In-plane gate transistors in AlxGa1−xN/GaN heterostructures written by focused ion beams

Focused ion beam implantation of gallium and dysprosium was used to locally insulate the near-surface two-dimensional electron gas of Al_xGa_1−xN/GaN heterostructures. The threshold dose for insulation was determined to be 2×10¹⁰ cm⁻¹ for 90 keV Ga⁺ and 1×10⁹ cm⁻¹ for 200 keV Dy²⁺ at 4.2 K. This offers a tool not only for inter-device insulation but also for direct device fabrication. Making use of “open-T” like insulating line patterns, in-plane gate transistors have been fabricated by focused ion beam implantation. An exemplar with a geometrical channel width of 1.5 μm shows a conductance of 32 μS at 0 V gate voltage and a transconductance of around 4 μS, which is only slightly dependent on the gate voltage.     

Large area SiC substrates and epitaxial layers for high power semiconductor devices — An industrial perspective

We review the progress in the industrial production of SiC substrates and epitaxial layers for high power semiconductor devices. Optimization of SiC bulk growth by the sublimation method has resulted in the commercial release of 100 mm n-type 4H-SiC wafers and the demonstration of micropipe densities as low as 0.7 cm⁻² over a full 100 mm diameter. Modelling results link the formation of basal plane dislocations in SiC crystals to thermoelastic stress during growth. A warm-wall planetary SiC-VPE reactor has been optimized up to a 8×100 mm configuration for the growth of uniform 0.01–80-micron thick, specular, device-quality SiC epitaxial layers with low background doping concentrations of <1×10¹⁴ cm⁻³, and intentional p- and n-type doping from 1×10¹⁵ to >1×10¹⁹ cm⁻³. We address the observed degradation of the forward characteristics of bipolar SiC PiN diodes [H. Lendenmann, F. Dahlquist, J.P. Bergmann, H. Bleichner, C. Hallin, Mater. Sci. Forum 389–393 (2002) 1259], and discuss the underlying mechanism due to stacking fault formation in the epitaxial layers. A process for the growth of the epitaxial layers with a basal plane dislocation density <10 cm⁻² is demonstrated to eliminate the formation of these stacking faults during device operation [J.J. Sumakeris, M. Das, H.McD. Hobgood, S.G. Müller, M.J. Paisley, S. Ha, M. Skowronski, J.W. Palmour, C.H. Carter Jr., Mater. Sci. Forum 457–460 (2004) 1113].     

Characterization of nitrogen-doped ZnO thin films grown by plasma-assisted pulsed laser deposition on sapphire substrates

The crystalline, optical and electrical properties of N-doped ZnO thin films were measured using X-ray diffraction, photoluminescence and Hall effect apparatus, respectively. The samples were grown using pulsed laser deposition on sapphire substrates coated priorly with ZnO buffer layers. For the purpose of acceptor doping, an electron cyclotron resonance (ECR) plasma source operated as a low-energy ion source was used for nitrogen incorporation in the samples. The X-ray diffraction analyses indicated some deterioration of the ZnO thin film with nitrogen incorporation. Temperature-dependent Van der Pauw measurements showed consistent p-type behavior over the measured temperature range of 200–450 K, with typical room temperature hole concentrations and mobilities of 5×10¹⁵ cm⁻³ and 7 cm²/V s, respectively. Low temperature photoluminescence spectra consisted of a broad emission band centered around 3.2 eV. This emission is characterized by the absence of the green deep-defect band and the presence of a band around 3.32 eV.     

Structural properties of 10 μm thick InN grown on sapphire (0001)

The structural properties of a 10 μm thick In-face InN film, grown on Al₂O₃ (0001) by radio-frequency plasma-assisted molecular beam epitaxy, were investigated by transmission electron microscopy and high resolution x-ray diffraction. Electron microscopy revealed the presence of threading dislocations of edge, screw and mixed type, and the absence of planar defects. The dislocation density near the InN/sapphire interface was 1.55×10¹⁰ cm⁻², 4.82×10⁸ cm⁻² and 1.69×10⁹ cm⁻² for the edge, screw and mixed dislocation types, respectively. Towards the free surface of InN, the density of edge and mixed type dislocations decreased to 4.35×10⁹ cm⁻² and 1.20×10⁹ cm⁻², respectively, while the density of screw dislocations remained constant. Using x-ray diffraction, dislocations with screw component were found to be 1.2×10⁹ cm⁻², in good agreement with the electron microscopy results. Comparing electron microscopy results with x-ray diffraction ones, it is suggested that pure edge dislocations are neither completely randomly distributed nor completely piled up in grain boundaries within the InN film.     

Characterization of InN epilayers grown on Si(1 1 1) substrates at various temperatures by MBE

InN films have been grown by plasma-assisted molecular beam epitaxy (PAMBE) and characterized by various technologies. It was found that the structural, optical and electrical properties can be drastically improved by raising growth temperature from 440 to 525 °C. Grainy morphology was found in the grain size was found in atomic force microscope images. The large grain size was about 360 nm for a film grown at 525 °C. These films exhibited Wurtzite structure with a c/a ratio ranging from 1.59 to 1.609. The dislocation densities estimated by X-ray diffraction techniques closely agreed with those analyzed by plan-view transmission electron microscopy. Photoluminescence (PL) studies confirmed near band-to-band transitions and the narrowest low-temperature PL peak width was found to be 24 meV at 0.666 eV. Carrier concentrations decreased from 1.44×10¹⁹ to 1.66×10¹⁸ cm⁻³ and Hall mobility increased from 226 to 946 cm² V⁻¹ s⁻¹ as the growth temperature is progressively increased from 440 to 525 °C. Raman spectra also indicated improved crystal quality as the growth temperature was raised.     

Correlation between structural and electrical properties of InN thin films prepared by molecular beam epitaxy

The strain-relaxation phenomena and the formation of a dislocation network in 2H-InN epilayers during molecular beam epitaxy are reported. The proposed growth model emphasizes the dominant role of the coalescence process in the formation of a dislocation network in 2H-InN. Edge type threading dislocations and dislocations of mixed character have been found to be the dominating defects in wurtzite InN layers. It is demonstrated that these dislocations are active suppliers of electrons and an exponential decay of their density with the thickness implies a corresponding decay in the carrier density. Room temperature mobility in excess of 1500 cm² V ⁻¹ s⁻¹ was obtained for 800 nm thick InN layers with dislocation densities of 3×10⁹ cm⁻².     

Electrical characterisation of phosphorus-doped ZnO thin films grown by pulsed laser deposition

Phosphorus-doped ZnO films were grown by pulsed laser deposition using a ZnO:P₂O₅-doped target as the phosphorus source with the aim of producing p-type ZnO material. ZnO:P layers (with phosphorus concentrations of between 0.01 to 1 wt%) were grown on a pure ZnO buffer layer. The electrical properties of the films were characterised from temperature dependent Hall-effect measurements. The samples typically showed weak n-type conduction in the dark, with a resistivity of 70 Ω cm, a Hall mobility of μ_n0.5 cm² V ⁻¹ s⁻¹ and a carrier concentration of n3×10¹⁷ cm⁻³ at room temperature. After exposure to an incandescent light source, the samples underwent a change in conduction from n- to p-type, with an increase in mobility and decrease in concentration for temperatures below 300 K.     

Structural and optical characterisation of InN layers grown by MOCVD

In the following, we report investigations of the dependencies of the structural, optical and electrical characteristics of InN thin films grown by MOCVD on the growth temperature. The layer thicknesses range from 70 to 400 nm. Their carrier concentrations range from 7×10¹⁸ to 4×10¹⁹ cm⁻³. Hall mobility values from 150 to 1300 cm²/V/s were determined in these films. The variation of the growth temperature and V/III ratio brought about different growth modes and rates. Using TEM, in addition to measuring layer thickness, we also determined the growth mode along with the structural quality of the InN layers. The surface roughness was obtained from AFM measurements. The layer crystalline quality was also investigated by means of X-ray diffraction in the rocking mode. Photoluminescence measurements performed at room temperature and at 7 K gave emission at around 0.7 eV.     

MBE growth of nitride-based photovoltaic intersubband detectors

In this work, we present the plasma-assisted molecular-beam epitaxial growth of quantum well infrared photodetector (QWIP) structures, including the Si-doped GaN/AlN short-period superlattice of the active region, conductive AlGaN claddings and integration of the final device. The growth of Si-doped GaN/AlN multiple quantum well (QW) structures is optimized by controlling substrate temperature, metal excess and growth interruptions. Structural characterization confirms a reduction of the interface roughness to the monolayer scale. P-polarized intersubband absorption peaks covering the 1.33–1.91 μm wavelength range are measured on samples with QW thickness varying from 1 to 2.5 nm. The absorption exhibits Lorentzian shape with a line width around 100 meV in QWs doped 5×10¹⁹ cm⁻³. To prevent partial depletion of the QWs owing to the internal electric field, we have developed highly-conductive Si-doped AlGaN cladding layers using In as a surfactant during growth. Complete ISB photodetectors with 40 periods of 1 nm-thick Si-doped GaN QWs with 2 nm-thick AlN barriers have been grown on conductive AlGaN claddings, the Al mole fraction of the cladding matching the average Al content of the active region. Temperature-dependent photovoltage measurements reveal a narrow (90 meV) detection peak at 1.39 μm.     

Carrier concentration and shallow electron states in In-doped hydrothermally grown ZnO

Single-crystal ZnO has been hydrothermally grown with additional In₂O₃ in the solution. Schottky barrier contacts have been deposited by electron beam evaporation of Pd onto the face. Capacitance–voltage measurements have been performed to reveal the carrier concentration as a function of the In₂O₃ content in the solution, and secondary-ion mass spectrometry was used to measure the resulting In concentration in the samples. For an In₂O₃ content of 2×10¹⁹ cm⁻³, the average free electron concentration increased to 5×10¹⁸ cm⁻³ compared to 4×10¹⁷ cm⁻³ for the non-doped material. An increase of the In₂O₃ content to 4×10¹⁹ cm⁻³ leads to a measured carrier concentration of approximately 1×10¹⁹ cm⁻³; however, only up to a quarter of the incorporated In became electrically active. From thermal admittance spectroscopy measurements two prominent electronic levels are found, and compared with to the non-doped material case, the freeze-out of the shallow doping in the In-doped samples takes place at lower temperatures (below 80 K).     

Free-to-bound radiative recombination in highly conducting InN epitaxial layers

We present a theoretical simulation of near-band-edge emission spectra of highly conducting n-InN assuming the model of ‘free-to-bound’ radiative recombination (FBRR) of degenerate electrons from the conduction band with nonequilibrium holes located in the valence band tails. We also study experimental photoluminescence (PL) spectra of highly conducting InN epitaxial layers grown by MBE and MOVPE with electron concentrations in the range (7.7×10¹⁷–6×10¹⁸) cm⁻³ and find that the energy positions and shape of the spectra depend on the impurity concentration. By modeling the experimental PL spectra of the InN layers we show that spectra can be nicely interpreted in the framework of the FBRR model with specific peculiarities for different doping levels. Analyzing simultaneously the shape and energy position of the InN emission spectra we determine the fundamental bandgap energy of InN to vary between E_g=692 meV for effective mass m_n0=0.042m₀ and E_g=710 meV for m_n0=0.1m₀.     

Bi-induced vibrational modes in GaAsBi

We have studied GaAs_1−xBi_x (up to x3%) using Raman scattering with two different polarization configurations. Two Bi-induced phonon modes are observed at 186 cm⁻¹ and 214 cm⁻¹ with increasing Raman intensity as the Bi concentration increases. By comparing Raman selection rules for the observed Bi-induced phonon modes with those for the substitutional N vibrational mode (GaN mode) in GaAsN, the phonon mode at 214 cm⁻¹ is identified as originating from substitutional Bi at the As site in GaAsBi.     

Extended X-ray absorption fine structure studies of thulium doped GaN epilayers

The local structure of Tm³⁺ ions incorporated into GaN epilayers was studied by means of Extended X-ray Absorption Fine Structure. The samples were doped either in situ during growth by Molecular Beam Epitaxy or by ion implantation of layers grown by Metal Organic Chemical Vapour Deposition. The implantation was done at ion energy of 300 keV and different nominal fluences of 3×10¹⁵, 4×10¹⁵ cm⁻² and 5×10¹⁵ cm⁻². The concentration of Tm in the samples studied was measured by Wavelength Dispersive X-ray analysis. For the in situ doped sample with concentration of 0.5%, and for all of the implanted samples, Tm was found on the Ga site in GaN. The ion implanted sample and an in situ doped sample with a similar concentration of Tm showed the same local structure, which suggests that the lattice site occupied by Tm does not depend on the doping method. When the average Tm concentration for in situ doped samples is increased to 1.2% and 2.0%, Tm is found to occupy the Ga substitutional site and the presence of a substantial number of Tm ions in the second coordination sphere indicates dopant clustering in the films. The formation of pure TmN clusters was found in an in situ doped sample with a dopant concentration of 3.4%.     

The structure of crystallographic damage in GaN formed during rare earth ion implantation with and without an ultrathin AlN capping layer

The crystallographic nature of the damage created in GaN implanted by rare earth ions at 300 keV and room temperature has been investigated by transmission electron microscopy versus the fluence, from 7×10¹³ to 2×10¹⁶ at/cm², using Er, Eu or Tm ions. The density of point defect clusters was seen to increase with the fluence. From about 3×10¹⁵ at/cm², a highly disordered ‘nanocrystalline layer’ (NL) appears on the GaN surface. Its structure exhibits a mixture of voids and misoriented nanocrystallites. Basal stacking faults (BSFs) of I₁, E and I₂ types have been noticed from the lowest fluence, they are I₁ in the majority. Their density increases and saturates when the NL is observed. Many prismatic stacking faults (PSFs) with Drum atomic configuration have been identified. The I₁ BSFs are shown to propagate easily through GaN by folding from basal to prismatic planes thanks to the PSFs.When implanting through a 10 nm AlN cap, the NL threshold goes up to about 3×10¹⁶ at/cm². The AlN cap plays a protective role against the dissociation of the GaN up to the highest fluences. The flat surface after implantation and the absence of SFs in the AlN cap indicate its high resistance to the damage formation.     

Ni–Al ohmic contact to p-type 4H-SiC

Investigations on Ni/Al alloys to form ohmic contacts to p-type 4H-SiC are presented in this paper. Different ratios of Ni/Al were examined. Rapid thermal annealing was performed in argon atmosphere at 400 C for 1 min, followed by an annealing at 1000 C for 2 min. In order to extract the specific contact resistance, TLM test structures were fabricated. A specific contact resistance of 3×10⁻⁵ Ω cm² was obtained reproducibly on Al²⁺ implanted p-type layers, having a doping concentration of 1×10¹⁹ cm⁻³. The lowest specific contact resistance value measured amounts to 8×10⁻⁶ Ω cm².