An interface study of crystalline Fe/Ge multilayers grown by molecular beam epitaxy

Fe/Ge multilayers were grown on single crystal Ge(0 0 1) substrates by molecular beam epitaxy. The structural, electronic and magnetic properties of Fe/Ge have been studied. The analysis shows that Fe grows in a layer-by-layer epitaxial growth mode on Ge(0 0 1) substrates at 150 °C and no intermixing has been observed. Growth of a crystalline Ge film at 150 °C on a single crystal Fe film has been observed. At this temperature Ge films grow by means of the island growth mode according to reflection of high energy electron diffraction patterns. Fe layers of 36 nm thickness, deposited at 150 °C on Ge(0 0 1) substrates, show two magnetization reversal values indicating the growth of Fe in two different crystal orientations. 36 nm thick Fe and Ge layers grown at 150 °C in Ge/Fe/Ge/Fe/Ge(0 0 1) sequence shows ferromagnetic behavior, however, the same structure grown at 200 °C shows paramagnetic behavior.     

Migration of CrSi2 nanocrystals through nanopipes in the silicon cap

CrSi₂ nanocrystals (NC¹) were grown by reactive deposition epitaxy of Cr at 550 °C. After deposition the Cr is localized in about 20-30 nm dots on the Si surface. The NCs were covered by silicon cap grown by molecular beam epitaxy at 700 °C. The redistribution of NCs in the silicon cap was investigated by transmission electron microscopy and atomic force microscopy. The NCs are partly localized at the deposition depth, and partly migrate near the surface. A new migration mechanism of the CrSi₂ NCs is observed, they are transferred from the bulk toward the surface through nanopipes formed in the silicon cap. The redistribution of CrSi₂ NCs strongly depends on Cr deposition rate and on the cap growth temperature.     

Diamond cubic Sn-rich nanocrystals: synthesis, microstructure and optical properties

Diamond cubic Sn-rich nanocrystals were fabricated with radii less than 20 nm by post-growth annealing at T=750 °C of Sn_xGe_1-x alloys grown on Ge(001) by molecular beam epitaxy. The crystal phase of the Sn-rich nanocrystals was determined to be diamond cubic from Fourier transform analysis of high-resolution transmission electron microscopy images. Optical transmittance of these Sn_xGe_1-x/Ge (001) films demonstrated changes in optical absorption that can be attributed to absorption from the nanocrystals. The energy bandgap was measured to be 0.45 eV for nanocrystals arrays in Ge with a mean diameter of 32 nm. PACS 68.37.Lp; 78.67.Hc; 81.07.Ta; 81.16.Dn; 68.65.Hb     

Ultrathin InAs and modulated InGaAs layers in GaAs grown by MOVPE studied by photomodulated reflectance spectroscopy

Photomodulated reflectance spectroscopy (PR) and X-ray diffraction (XRD) were used for the characterization of highly strained ultrathin InAs quantum wells and modulated InGaAs layers in GaAs grown by metal-organic vapor phase epitaxy (MOVPE). Structures were grown in AIXTRON 200 reactor at 500 °C on (1 0 0) oriented GaAs substrates by sequential growth of InAs and GaAs layers. Various PR spectral features corresponding to optical transitions between ground and excited states in the layers were identified by means of simulation of electronic states in these structures using nextnano³ quantum simulator. Different models of InAs layer growth were used to explain both the XRD and PR data. Results show that the Gaussian distribution of In atoms within few monolayers gives the best fit for our MOVPE grown ultrathin InAs layers.     

Evolution of epitaxial titanium silicide nanocrystals as a function of growth method and annealing treatments

Titanium silicide grows on silicon in a form of discontinuous layers, which is the most serious obstacle to the formation of high-quality epilayers for VLSI applications. At the same time, nanometric dimensions of the epitaxial silicide islands attract interest as quantum nanostructures. However, for this purpose, nanocrystals in a self-assembled array have to be defect-free, and exhibit high shape and size uniformity. In this work titanium silicide was grown on Si(1 1 1) substrates by reactive deposition epitaxy and by solid-phase epitaxy. Since the reaction and phase-formation kinetics depend on the growth method, accordingly different lattice matching and facet energies may result in different morphological shapes of the nanocrystals. Nanocrystals from reaction in a solid-state could be characterized as highly non-uniform in both shape and size, and their evolution due to post-deposition anneals increased that non-uniformity even further. Relaxation of epitaxial mismatch strain by misfit dislocations could be inferred from a gradual reduction of the nanocrystal vertical aspect ratio and development of flat top facets out of the initially sharp conical crests, in accord with generalized Wulf-Kaishew theorem. On the other hand, the silicide nanocrystals formed by reactive deposition exhibited high uniformity and thermal stability. Significant strain relaxation, as could be judged by the nanocrystal flattening, took place only at temperatures in excess of 650 °C, followed by progressive nanocrystal coalescence. It thus could be inferred, that better titanium silicide nanocrystal arrays (in the sense of uniformity and stability) are more easily obtained by reactive deposition epitaxy than by solid-phase epitaxy. While terminal, stable C54-TiSi₂ phase, did eventually form in the epilayers in both methods, different evolution pathways were manifested by different respective morphologies and orientations even in this final state.     

Effects of carbonization and substrate temperature on the growth of 3C-SiC on Si(1 1 1) by SSMBE

The growth of 3C-SiC on Si(1 1 1) substrate was performed at different carbonization temperatures and substrate temperatures by solid-source molecular beam epitaxy (SSMBE). The properties of SiC film were analyzed with in situ reflection high energy electron diffraction (RHEED), X-ray diffraction (XRD), atomic force microscopy (AFM) and X-ray photoelectron spectroscopy (XPS). The best carbonization temperature of 810 °C was found to be optimal for the surface carbonization. The quality of SiC film grown on Si at substrate temperature of 1000 °C is best. The worse crystalline quality for the sample grown at higher temperature was attributed to the large mismatch of thermal expansion coefficient between SiC and Si which caused more dislocation when sample was cooled down to room temperature from higher substrate temperature. Furthermore, the larger size of single pit and the total area of the pits make the quality of SiC films grown at higher temperature worse. More Si atoms for the sample grown at lower temperature were responsible for the degradation of crystalline quality for the sample grown at lower temperature.     

Characterization of Si nanocrystals into SiO2 matrix

Silicon nanocrystals (nc-Si) have gained great interest due to their excellent optical and electronic properties and their applications in optoelectronics. The aim of this work is the study of growth mechanism of nc-Si into a-SiO₂ matrix from SiO/SiO₂ multilayer annealing, using non-destructive and destructive techniques. The multilayer were grown by e-beam evaporation from SiO and SiO₂ materials and annealing at temperatures up to 1100 °C in N₂ atmosphere. X-rays reflectivity (XRR) and high resolution transmission electron microscopy (HRTEM) were used for the structural characterization and spectroscopic ellipsometry in IR (FTIRSE) energy region for the study of the bonding structure. The ellipsometric results gave a clear evidence of the formation of an a-SiO₂ matrix after the annealing process. The XRR data showed that the density is being increased in the range from 25 to 1100 °C. Finally, the HRTEM characterization proved the formation of nc-Si. Using the above results, we describe the growth mechanism of nc-Si into SiO₂ matrix under N₂ atmosphere.     

Laser reflectometry in situ monitoring of InGaAs grown by atmospheric pressure metalorganic vapour phase epitaxy

InGaAs layers on undoped GaAs (0 0 1) substrates were grown by atmospheric pressure metalorganic vapour phase epitaxy (AP-MOVPE). In order to obtain films with different indium composition (x_In), the growth temperature as a growth parameter, was varied from 420 to 680 °C. Furthermore, high-resolution X-ray diffraction (HRXRD) measurements were used to quantify the change of x_In. Crystal quality has been also studied as a function of growth conditions. On the other hand, laser reflectometry (LR) at 632.8 nm wavelength, was employed to in situ monitor epitaxy. Reflectivity-time signal was enabled to evaluate structural and optical properties of samples. We have fitted experimental data to determine optical constants and growth rate of InGaAs at 632.8 nm. In addition, the fitting provided InGaAs thickness as a function of growth time. Based on ex situ characterization by scanning electronic microscopy (SEM) and HRXRD, we propose a practical method, relating the contrast of first reflectivity maximum with the X-ray diffraction peak angular difference between the substrate and epitaxial layer, to determine in situ the In solid composition in InGaAs alloys.     

Growth and annealing of zinc-blende CdSe thin films on GaAs (0 0 1) by molecular beam epitaxy

CdSe thin films have been grown on GaAs (0 0 1) substrates by molecular beam epitaxy (MBE). The effects of substrate temperature and annealing treatment on the structural properties of CdSe layers were investigated. The growth rate slightly decreases due to the accelerated desorption of Cd from CdSe surface with an increase in the temperature. The sample grown at 260 °C shows a polycrystalline structure with rough surface. As the temperature increases over 300 °C, crystalline CdSe (0 0 1) epilayers with zinc-blende structure are achieved and the structural quality is improved remarkably. The epilayer grown at 340 °C displays the narrowest full-width at half-maximum (FWHM) from (0 0 4) reflection in double-crystal X-ray rocking curve (DCXRC) and the smallest root-mean-square (RMS) roughness of 0.816 nm. Additionally, samples fabricated at 320 °C were annealed in air for 30 min to study the films’ thermal stability. X-ray diffraction (XRD) results indicate that the zinc-blende structure remains unchanged when the annealing temperature is elevated to 460 °C, meaning a good thermal stability of the cubic CdSe epilayers.     

Point-defect production in arsenic-doped silicon studied with variable-energy positrons

Silicon epilayers grown by molecular beam epitaxy and doped in-situ using low-energy implantation were examined using a variable-energy positron beam. The samples had been previously characterized using electrical measurements, ion channeling, SIMS, and electron microscopy. The positron results show that defects have been created in layers grown at 460°C and in the highly doped layers grown at 700°C. The assignment of defect structures is difficult at present, but is consistent with the formation of As clusters or Asvacancy complexes.     

Surface control of CdSe nanocrystals by UV-exposure in air and successive thermal treatment under ultra high vacuum

Colloidal CdSe nanocrystals were synthesized through a solution process. The CdSe nanocrystals coated on Si(1 0 0) wafers were UV-exposed in either an air or argon atmosphere to distinguish the effect of generated ozone from UV-radiation at 365 nm on the removal of surface capping pyridine molecules. The pyridine on the CdSe nanocrystal's surface could be effectively removed by the ozone generated during UV-exposure with an accompanying highly oxidized surface state of the CdSe nanocrystals. For the removal of surface oxides of CdSe nanocrystals, a successive thermal treatment under ultra high vacuum (UHV) was adopted. The optical energy bandgap measured by using UV-vis absorption spectroscopy showed a red shift with treatment with an increase of annealing temperature. The electronic energy structure of UHV-annealed CdSe nanocrystals film was analyzed in situ using X-ray absorption and photoelectron spectroscopy. A great resemblance was found between the values of the optical and electron energy bandgaps of effectively surface-treated CdSe nanocrystals film after UHV-annealing at 400 °C.     

Growth of ZnO thin films on c-plane Al2O3 by molecular beam epitaxy using ozone as an oxygen source

The growth of c-axis oriented ZnO thin films on c-plane Al₂O₃ via molecular beam epitaxy (MBE) using dilute ozone (O₃) as an oxygen source was investigated. Four-circle X-ray diffraction (XRD) indicates that films grown at 350 °C are epitaxial with respect to the substrate, but with a broad in-plane and out-of-plane mosaic. The films were highly conductive and n-type. Epitaxial film growth required relatively high Zn flux and O₃/O₂ pressure. The growth rate decreased rapidly as growth temperature was increased above 350 °C. The drop in growth rate with temperature reflects the low sticking coefficient of Zn at moderately high temperatures and limited ozone flux for the oxidation of the Zn metal. Characterization of the films included atomic force microscopy (AFM), X-ray diffraction, photoluminescence, and Hall measurements. These results show that molecular beam epitaxy of ZnO using ozone is rate limited by the ozone flux for growth temperatures above 350 °C.     

Four-fold magnetic anisotropy in a Co film on MgO(0 0 1)

The development of devices based on magnetic tunnel junctions has raised new interests on the structural and magnetic properties of the interface Co/MgO. In this context, we have grown ultrathin Co films (≤30 Å) by molecular-beam epitaxy on MgO(0 0 1) substrates kept at different temperatures (T_S). Their structural and magnetic properties were correlated and discussed in the context of distinct magnetic anisotropies for Co phases reported in the literature. The sample characterization has been done by reflection high energy electron diffraction, magneto-optical Kerr effect and ferromagnetic resonance. The main focus of the work is on a sample deposited at T_S=25 °C, as its particular way of growth has enabled a bct Co structure to settle on the substrate, where it is not normally obtained without specific seed layers. This sample presented the best crystallinity, softer magnetic properties and a four-fold in-plane magnetic anisotropy with Co〈1 1 0〉 easy directions. Concerning the samples prepared at T_S=200 and 500° C, they show fcc and polycrystalline structures, respectively and more intricate magnetic anisotropy patterns.     

Femtosecond pulsed laser deposition of Ge quantum dot growth on Si(1 0 0)-(2 × 1)

Ge quantum dots were grown on Si(1 0 0)-(2 × 1) by femtosecond pulsed laser deposition at various substrate temperatures using a femtosecond Ti:sapphire laser. In situ reflection high-energy electron diffraction and ex situ atomic force microscopy were used to analyze the film structure and morphology. The morphology of germanium islands on silicon was studied at different coverages. The results show that femtosecond pulsed laser deposition reduces the minimum temperature for epitaxial growth of Ge quantum dots to ∼280 °C, which is 120 °C lower than previously observed in nanosecond pulsed laser deposition and more than 200 °C lower than that reported for molecular beam epitaxy and chemical vapor deposition.     

Aerosol Synthesis of Fullerene Nanocrystals in Controlled Flow Reactor Conditions

Fullerene nanocrystals in the size range 30–300 nm were produced starting from atomized droplets of C₆₀ in toluene. The experiments were carried out under well-controlled conditions in a laminar flow reactor at temperatures of 20–600°C. Particle transformation and crystallization mechanisms of polydisperse and monodisperse (size classified) fullerene aerosol particles were studied. The results show that fullerene particles are roughly spherical having pores and voids at temperatures of 300°C and below. Particles are already crystalline and likely fine-grained at 20°C and they are polycrystalline at temperatures up to 300°C. At 400°C monodisperse particles evaporate almost completely due to their low mass concentration. Polydisperse particles are crystalline, but sometimes heavily faulted. At 500°C most of the particles are clearly faceted. In certain conditions, almost all particles are hexagonal platelets having planar defects parallel to large (111) faces. We suggest that at 500°C fullerene particles are partially vaporized forming residuals with lamellar defects such as twins and stacking faults, which promote crystal growth during synthesis. Subsequently fullerene vapor is condensed on faces with defects and hexagonal particles are grown by a re-entrant corner growth mechanism. At 600°C particles are single crystals, but they have a less distinct shape due to higher vaporization of fullerene. The final size and shape of the particles are mainly determined at the reactor outlet in the short time when the aerosol cools.     

Excimer laser assisted selective epitaxy of GaP

An ArF excimer laser has been used to achieve homoepitaxy of GaP at 500° C using trimethylgallium and tertiarybutylphosphine as the precursor gases. Dependence of epitaxial growth on several parameters is examined. The crystalline properties of the films are determined using cross-sectional transmission electron microscopy. It is found that at 500° C, in the presence of laser radiation, higher growth rate and superior crystalline properties of GaP are achieved compared to purely thermal metalorganic vapor phase epitaxy under the same conditions. Electrical properties of p-n diodes fabricated via Zn doping have also been examined.     

ZnO/cubic (Mg,Zn)O radial nanowire heterostructures

The formation and properties of radial heteroepitaxial ZnO/(Mg,Zn)O nanowires is reported in which the (Mg,Zn)O is cubic. Synthesis is achieved via a catalyst-driven molecular beam epitaxy technique. The nanowires were grown on Ag-coated Si substrates at growth temperatures ranging from T_g=300 to 500 °C, using Zn, Mg, and O₃/O₂ as the reactive flux. Structural and compositional analyses indicate that the core of the nanowire is ZnO possessing the hexagonal wurtzite structure, with the (Mg,Zn)O sheath assuming the cubic rock salt structure. Since (Mg,Zn)O has a larger band-gap energy (up to 7.8 eV) than that of ZnO (3.37 eV), these radial heterostructure nanorods provide an interesting system for quantum confinement and one-dimensional nanoscale device studies. PACS 81.05.Dz; 81.07.Vb     

Specific features and mechanisms of photoluminescence of nanostructured silicon carbide films grown on silicon in vacuum

The light-emitting properties of cubic silicon carbide films grown by vacuum vapor phase epitaxy on Si(100) and Si(111) substrates under conditions of decreased growth temperatures (T _gr ∼ 900–700°C) have been discussed. Structural investigations have revealed a nanocrystalline structure and, simultaneously, a homogeneity of the phase composition of the grown 3C-SiC films. Photoluminescence spectra of these structures under excitation of the electronic subsystem by a helium-cadmium laser (λ_excit = 325 nm) are characterized by a rather intense luminescence band with the maximum shifted toward the ultraviolet (∼3 eV) region of the spectral range. It has been found that the integral curve of photoluminescence at low temperatures of measurements is split into a set of Lorentzian components. The correlation between these components and the specific features of the crystal structure of the grown silicon carbide layers has been analyzed.     

Charging effects of ErAs islands embedded in AlGaAs heterostructures

Self-assembled ErAs islands were grown on GaAs between a two-dimensional electron gas (2DEG) and a backgate electrode by molecular-beam epitaxy. The islands have overlapping Schottky barriers that form an insulating potential barrier. A TiAu topgate was added by shadow mask evaporation. Thermal activation and charging experiments were employed to gain insight into the electronic properties of the ErAs island systems. In addition the 2DEG was characterized as a function of topgate and backgate voltage.     

Flame Temperature Effect on the Structure of SiC Nanoparticles Grown by Laser Pyrolysis

Small SiC nanoparticles (10 nm diameter) have been grown in a flow reactor by CO₂ laser pyrolysis from a C₂H₂ and SiH₄ mixture. The laser radiation is strongly absorbed by SiH₄ vibration. The energy is transferred to the reactive medium and leads to the dissociation of molecules and the subsequent growth of the nanoparticles. The reaction happens with a flame. The purpose of the experiments reported in this paper is to limit the size of the growing particles to the nanometric scale for which specific properties are expected to appear. Therefore the effects of experimental parameters on the structure and chemical composition of nanoparticles have been investigated. For a given reactive mixture and gas velocity, the flame temperature is governed by the laser power. In this study, the temperature was varied from 875°C to 1100°C. The chemical analysis of the products indicate that their composition is a function of the temperature. For the same C/Si atomic ratio in the gaseous phase, the C/Si ratio in the powder increases from 0.7 at 875°C up to 1.02 at 1100°C, indicating a growth mechanism limited by C₂H₂ dissociation. As expected, X-ray diffraction has shown an improved crystallisation with increasing temperature. Transmission electron microscopy observations have revealed the formation of 10 nm grains for all values of laser power (or flame temperature). These grains appear amorphous at low temperature, whereas they contain an increasing number of nanocrystals (2 nm diameter) when the temperature increases. These results pave the way to a better control of the structure and chemical composition of laser synthesised SiC nanoparticles in the 10 nm range.