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We have studied photoluminescence (PL) from undoped GaN films grown by HVPE technique on sapphire. Several defect-related PL bands are observed in the low-temperature PL spectrum. The concentrations of the defects responsible for these PL bands are determined from the dependence of PL intensity on excitation intensity. The RL band with a maximum at 1.8 eV is often the dominant PL band in HVPE GaN. It is caused by an unknown defect with the concentration of up to ∼1017 cm-3. The concentrations of defects responsible for other defect-related PL bands rarely exceed 1015 cm-3.
Multiwafer Planetary Reactor is a promising system for large-scale production of heterostructures for LED's based on III-group nitrides. Analysis of chemical processes occurring in the reactor allows one to get insight into specific mechanisms governing growth of nitride based heterostructures. In the present paper results of modeling analysis of MOVPE of InxGa1−xN layers in AIX-200 Reactor and AIX 2000 HT Planetary Reactor are reported. The model used for MOVPE process analysis accounts for gas flow, heat transfer, and multicomponent mass transport along with gas phase and surface chemical reactions. Results of the modeling analysis of In transport and incorporation into the solid phase are compared with experimental data. It is shown that the model predicts reasonably well the In incorporation during MOVPE of InGaN under In/(In+Ga) ratio in the gas phase less than 20%.
A quasi-thermodynamic model accounting for kinetics of molecular nitrogen evaporation is applied to simulate the growth of binary and ternary group-III nitrides using atomic group-III elements and molecular ammonia as the sources. The values of the molecular nitrogen evaporation coefficients from the surface of GaN and AlN necessary for the simulation are extracted from experiments on free evaporation of the crystals in vacuum, while for InN only estimates are available. The growth process of AlN and InN is studied by analyzing the composition of the desorbed vapor species that are thought to influence the native defect formation in group-III nitrides. Different channels of desorption from the surfaces of group-III nitrides (related either to group-III atoms or to their hydrides) are compared. Specific features of the growth processes under the metal-rich and N-rich conditions are analyzed. The developed approach is extended to study the growth of the ternary compounds GaInN and AlGaN. The growth rate of ternary compounds versus temperature shows a two-drop behavior corresponding to the rapid increase of the respective group-III atom desorption. The effect is accompanied by a corresponding stepwise change in the solid phase composition. Factors retarding the growth of ternary compounds — the miscibility gap related to internal strain accumulated in the solid phase due to the lattice mismatch of binary constituents, and the extra liquid phase formation during growth — are discussed with respect to GaInN.
A theoretical model which accounts for a physisorption precursor of molecular nitrogen is proposed for the analysis of group III-nitride growth by molecular beam epitaxy (MBE). The kinetics of nitrogen evaporation are found to be an essential factor influencing the MBE growth process of group III-nitrides. The high thermal stability of nitrides is explained to be related to the desorption kinetics resulting in a low value of the evaporation coefficient. The values of the evaporation coefficients as functions of temperature are extracted from the experimental Langmuir evaporation data of GaN and AlN. Using the revised thermodynamic properties of the group III-nitrides, and the obtained values of the evaporation coefficient, the process parameter dependent growth rate and transition to extra liquid phase formation during the GaN MBE are calculated. The theoretical results are compared to the available experimental data.
Recent studies revealed specific features of chemical processes occurring on the surface of growing group-III nitrides – extremely low sticking probability of molecular nitrogen, low sticking coefficient and incomplete decomposition of ammonia frequently used as the nitrogen precursor. These features (kinetic by nature) result in the growth process going on under conditions remarkably deviated from the gas-solid heterogeneous equilibrium. In this paper we propose a novel approach to modeling of group-III nitride growth by MOVPE taking into account these features. In the model the sticking/evaporation coefficients of N2 and NH3 extracted from independent experiments are used allowing adequate description of the kinetic effects. The model is applied to analysis of growth of binary (GaN) and ternary (InGaN) compounds in a horizontal tube reactor. The growth rate and the solid phase composition are predicted theoretically and compared with available experimental data. The modeling results reveal lower ammonia decomposition ratio on the surface of the crystal as compared to thermodynamic expectations. The developed model can be used for optimization of growth process conditions.
A database for thermodynamic properties of group-III nitrides and relevant species involved into growth of these materials is developed in this paper. Standard formation enthalpies of materials and coefficients of polynomial approximations of the reduced Gibbs free energies are collected in the tables. They allow one to determine the Gibbs free energy, enthalpy, entropy and specific heat of a species as a function of temperature. The database covers solid and gaseous group-III nitrides, elemental species, gaseous metal-organic compounds, chlorides and hydrides of group-III elements, nitrogen containing precursors and organic byproducts of various chemical reactions proceeding during growth processes. Thermodynamic properties of adducts which can be formed in the vapor phase while mixing ammonia and metal-organic compounds are presented in the database as well. Much of the data given in this paper is presented for the first time. All the data are checked for self-consistency and therefore can be used for thermodynamic calculations.
The current status of GaN crystal growth using the Sublimation Sandwich Technique is discussed in the paper. We use modeling to analyze gas dynamics in the reactor and the supply of the main gaseous species into the growth cell under growth conditions used in experiments. Important features of growth process — non-equilibrium cracking of ammonia, partial sticking of ammonia at the growing surface and kinetic limitation of GaN thermal decomposition — are taken into account in the model. Growth is carried out on sapphire and 6H-SiC substrates in ammonia atmosphere using a Ga/GaN mixture as the group-III element source. Single crystals of GaN of size 15×15 mm and up to 0.5 mm thick are normally grown with the optimized growth rates of 0.25-0.35 mm/h. The GaN crystals are characterized by photoluminescence, by the Color Cathodoluminescence Scanning Electron Microscopy technique, by differential double-crystal and triple-crystal X-ray diffractometry, and by electron paramagnetic resonance. Mechanisms of sublimation growth of GaN and physical limitations of the growth process are discussed.
Inverse modeling was applied to the optimization of a crucible design for SiC sublimation growth. We found a crucible shape providing the optimal temperature distribution in terms of the powder source stability during long-term operation and of the convex crystal shape. Considerable improvement of temperature uniformity throughout the powder charge was achieved. The results obtained show selective sensitivity of the thermal field inside the crucible to modification of the crucible design. The inverse problem approach is easy-to-adapt to various optimization criteria and seems to be especially effective in the case of multi-factor optimization.
Surface segregation and phase separation are investigated as processes limiting the indium incorporation in InGaN grown by ammonia Molecular Beam Epitaxy (MBE) and Metal- Organic Vapor Phase Epitaxy (MOVPE). It is shown that a significant concentration of indium on the growing surface may prevent the adsorption of ammonia via site blocking mechanism and result in appearance of In droplets instead of InGaN growth. Another conclusion is that the composition fluctuations in InGaN are related to coexistence of strained and relaxed InGaN islands rather than to the phase separation as commonly assumed.
Recently, an advanced technique for growing free-spreading SiC bulk crystals by sublimation has been demonstrated. This method was used to grow 6H- and 4H-SiC boules free of polycrystalline deposits on the crystal periphery, up to 35 mm in diameter with the micropipe density less than 20 cm-2 and the dislocation density about 102-103 cm-2. In this paper, we report on the numerical modeling of free-spreading crystal growth. We consider the global heat transfer in an inductively heated growth system, species transport in the growth cell and in the powder charge, and thermoelastic stress, focusing on the crystallization front dynamics, poly-SiC deposition, and powder source evolution. Special attention was given to the validation of the simulations. The computed thermal field and evolution of the powder and crystal shape were found to agree qualitatively with observations.
The analysis of In surface segregation and its impact on the composition profile and light emission spectra of the InGaN single quantum well heterostructures grown by Metalorganic Vapor Phase Epitaxy (MOVPE) is carried out by coupled solution of the Poisson and Schrödinger equations. Effective methods of controlling the composition profile, indium predeposition and temperature ramping during the cap layer growth are considered in terms of surface segregation model. General trends in spectra transformation upon the forward bias variation and their correlations with the quantum well electronic structure are discussed.
On the basis of both experimental and theoretical studies, a simple quasi-thermodynamic model of surface kinetics is suggested for Hydride Vapor Phase Epitaxy (HVPE) of GaN, working in a wide range of growth conditions. Coupled with detailed 3D modeling of species transport in a horizontal reactor, the model provides quantitative predictions for the GaN growth rate as a function of process parameters. Significance of transport effects on growth rate uniformity is demonstrated.
Bulk AlN crystal growth by Physical Vapor Transport (PVT) is studied both experimentally and numerically. This paper presents the analysis of heat and mass transport mechanisms in closed and partially open crucible geometries. The heat transfer in the growth system used at North Carolina State University (NCSU) is simulated. The computed temperature profiles are used in the analysis of mass transport in the growth cell to gain understanding of the effect of species exchange between the crucible and environment on the AlN growth rate. The model predictions are in reasonable agreement with observations.
A quantitative model of surface segregation free from adjustable parameters is suggested for the growth of ternary III-V compounds. In contrast to previous approaches, the model considers the dynamics of surface population by the three elements producing the ternary alloy. The underlying assumption is that the atoms in the adsorption layer are in equilibrium with the crystal bulk. Elastic strain arising in the epitaxial layer due to the lattice constant mismatch with the substrate is found to be one of the key factors affecting segregation. Along with growth temperature, it controls the segregation efficiency and the composition profile evolution in a growing heterostructure. The effect of the V/III ratio, growth rate and other parameters is accounted for. Here, we apply the model to analyze the InGaAs growth by molecular beam epitaxy owing to the vast experimental data available for the model verification. The theoretical predictions show a good agreement with the experimental observations
The heat and mass transport model extended to describe silicon cluster formation in the gas phase is employed for a numerical analysis of SiC CVD in a commercial vertical rotating disc reactor. The growth rate is studied as a function of precursor flow rates varied in a wide range of values. It is found that the growth rate is limited by the gas mixture depletion in silicon atoms due to homogeneous nucleation. The secondary phase formation on the growing surface is analyzed. The SiC growth window depending on the precursor flow rates is calculated, and a significant effect of the homogeneous nucleation on the window width is found. The model predicts that the Si/C ratio on the wafer can considerably differ from that at the reactor inlet.
A novel quasi-thermodynamic approach is suggested to simulate surface chemistry in III-V compound MOVPE. Blocking of free adsorption sites by methyl radicals is considered as the mechanism limiting the growth rate at low temperatures. This assumption has provided a good reproduction of experimental data on GaAs MOVPE in various types of reactor. The commercial computational fluid dynamics software CFD-ACE™ has been used to perform a detailed threedimensional modeling of AlGaAs and InGaP deposition in an AIX-200 horizontal reactor. The surface model has been incorporated into the code to obtain the growth rate and layer composition distributions over the substrate. Modeling results demonstrate a reasonable agreement with experimental data.
Global model of oxygen transport in the melt and inert gas is proposed which is based on coupled two-dimensional stationary modeling of global heat transfer, laminar flow of inert gas and turbulent flow in Si melt, and transport of dissolved oxygen in the melt and SiO vapor in the gas. The model allows to study effects of process parameters like flow rate and pressure of inert gas, and rotation of the crucible on incorporation of oxygen into Si crystal.
Thick epitaxial layers of GaN on SiC and sapphire are grown by using the sublimation sandwich method. It is shown that growth of good quality GaN crystals with the growth rates up to 0.5 mm/hour is possible using this technique. The grown layers have been separated from the seed and free standing GaN crystals up to 15 mm size were obtained.
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