Investigation of the thermal diffusion during the formation of a quasicrystalline phase in thin Al-Pd-Re films

The layer mixing during the formation of the Al₇₀Pd₂₀Re₁₀ icosahedral quasicrystalline phase in thin (55 nm) Al-Pd-Re layered film systems subjected to vacuum annealing has been studied. It is shown that a combined layer of Pd and Al atoms (with the Al₃Pd₂ phase dominating) is formed in the first stage (at 350°C), while the rhenium layer remains invariable. In the second annealing stage (at 450°C), the β′-AlPd phase is formed and the Re layer is diffused. In the third stage (700°C), Pd and Re atoms are uniformly distributed throughout the film with the formation of a quasicrystalline phase.     

Ionenstrahlgestäubte GaAs-Schichten auf verschiedenen einkristalline Substraten

Thin GaAs-films have been deposited on spinel, (111)-Si, and (100)-GaAs by ion beam sputtering. The beam system operated with argon ions at a vacuum of 5…︁8 · 10⁻⁶ torr in the chamber. Undoped polycrystalline GaAs was used as target material. The film proporties were investigated by electron optical methods (RHEED respective by C/Pt replica). Substrate temperatures were varied between 180 and 590 °C, and deposition rates were adjusted between 1…︁3 Å/s. Within a relative narrow temperature range epitaxial layers of good quality were obtained; the optimum values being 540 °C in case of GaAs/Si or 400…︁450 °C for GaAs/GaAs. Films deposited at higher temperatures showed extended defects induced by gallium excess because of dissociation.     

Rapid Thermal Diffusion of Zinc in GaAs

Rapid thermal diffusion of zinc into semi-insulating GaAs from spin-on silica films was investigated for various temperatures and heating rates with halogen lamps as the heat source. Dependent on the heating rate two types of SIMS profiles were observed. The degree of electrical activation of zinc was different as measured by the Hall effect. In some cases at high zinc concentrations, a ZnGa₂O₄ film on the GaAs surface was formed.     

Growth mechanisms in GaAs-VPE at low deposition temperature

The VPE growth of GaAs in the system GaAs AsCl₃ with either H₂ or He as the Carrier gas was studied in the range of low deposition temperatures. Down to about 670 °C the growth in the H₂-system is limited by the kinetics of chlorine desorption by molecular hydrogen. The increase in growth rate at lower temperatures results from the onset of GaCl₃-desorption (disproportionation mechanism). The addition of NH₃ to the vapour phase enhances this effect. Below about 700 °C the growth rate in the GaAs AsCl₃ H₂ NH₃ system becomes comparable to that in the GaAs AsCl₃ He-system, where the GaCl₃ desorption mechanism is the only possible growth mechanism.     

Structural investigation and electronic band transitions of nanostructured TiO2 thin films

Titanium dioxide (TiO₂) thin film was deposited on n‐Si (100) substrate by reactive DC magnetron sputtering system at 250 °C temperature. The deposited film was thermally treated for 3 h in the range of 400‐1000 °C by conventional thermal annealing (CTA) in air atmosphere. The effects of the annealing temperature on the structural and morphological properties of the films were investigated by X‐ray diffraction (XRD) and atomic force microscopy (AFM), respectively. XRD measurements show that the rutile phase is the dominant crystalline phase for the film annealed at 800 °C. According to AFM results, the increased grain sizes indicate that the annealing improves the crystalline quality of the TiO₂ film. In addition, the formation of the interfacial SiO₂ layer between TiO₂ film and Si substrate was evaluated by the transmittance spectra obtained with FTIR spectrometer. The electronic band transitions of as‐deposited and annealed films were also studied by using photoluminescence (PL) spectroscopy at room temperature. The results show that the dislocation density and microstrain in the film were decreased by increasing annealing temperature for both anatase and rutile phases. (© 2011 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

The transition layers in AlGaAs/GaAs and InGaAsP/GaAs heterostructures grown by LPE

AlGaAs/GaAs and InGaAsP/GaAs heterostructues were grown by liquid phase epitaxy (T_o = 800–770 °C), the transition layers (TLs) were measured with Auger profiling. The Auger profiling of the InGaAsP/GaAs heterostructures after a long heating (1–6 hours, 770 °C) has been made too. The analysis of the experimental data led to the conclusion that the fundamental values of the TL in above mentioned systems are about 10 and 1 to 2 nm, correspondingly. This difference between the minimum widths of the TL in AlGaAs/GaAs and InGaAsP/GaAs system is connected with the different speed of solid state diffusional processes which occur at the initial stpeps of liquid – solid contact.     

HigHighly strained InGaAs/GaAs quantum wells emitting beyond 1.2 µm

Highly strained In_xGa_1–xAs quantum wells (QWs) with GaAs barriers emitting around 1.2 µm are grown on GaAs substrates by metal organic vapour phase epitaxy (MOVPE) at low growth temperatures using conventional precursors. The effects of growth temperature, V/III ratio and growth rate on QW composition and luminescence properties are studied. The variation of indium incorporation with V/III ratio at a growth temperature of 510 °C is found to be opposite to the results reported for 700 °C. By an appropriate choice of the growth parameters, we could extend the room temperature photoluminescence (PL) wavelength of InGaAs/GaAs QWs up to about 1.24 µm which corresponds to an average indium content of 41% in the QW. The results of the growth study were applied to broad area laser diodes emitting at 1193 nm with low threshold current densities. (© 2005 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

On the growth of Au on clean and contaminated GaAs(001) surfaces

Auger analysis and transmission electron microscope (TEM) analysis have been used to determine the influence of contamination on the structural properties of Au films grown on different chemically treated (001)GaAs surfaces. The Au films were evaporated on to the (001)GaAs surfaces at 320°C in a vacuum of 10^-8 Torr after an initial bake-out of 500°C for 1 h. The results revealed that carbon contamination of the surfaces resulted in completely polycrystalline Au overgrowth while clean surfaces resulted in perfectly alligned epitaxial Au overgrowths. The epitaxial relationship is given by (100)_Au 6(100)_GaAs and <100 > _Au6 <100 > _GaAs which is equivalent to a misfit of 32.24%.     

Irradiation plus annealing-induced 1.20 eV emission band in p-type GaAs

The effect of 2.2 MeV electron irradiation and subsequent annealings on the luminescence of tellurium-compensated p-type GaAs crystals is studied and analyzed. A comparatively strong emission band peaked at hv_m near 1.20 eV (induced by radiative electron recombination in Te_AsV_Ga pairs) appears in irradiated annealed (at T ≧ 250 °C) compensated p-type GaAs. The data obtained testify about the following: a) electron irradiation of GaAs creates stable (at T ≦ 200 °C) defects not only in the arsenic sublattice of GaAs, but in its gallium sublattice too; b) radiation plus annealing (r.p.a.)-induced Te_AsV_Ga pairs are characterized by a rather high (compared to that for grown-in Te_As V_Ga pairs) probability of electron radiative transitions in them. The electrical characterization of the r.p. a.-induced 1.20 eV radiative centres (Te_AsV_Ga pairs) is given.     

Spray pyrolysis deposition and characterization of highly (100) oriented magnesium oxide thin films

Transparent dielectric thin films of MgO has been deposited on quartz substrates at different temperatures between 400 and 600°C by a pneumatic spray pyrolysis technique using Mg(CH₃COO)₂·4H₂O as a single molecular precursor. The thermal behavior of the precursor magnesium acetate is described in the results of thermogravimetry analysis (TGA) and differential thermal analysis (DTA). The prepared films are reproducible, adherent to the substrate, pinhole free and uniform. Amongst the different spray process parameters, the substrate temperature effect has been optimized for obtaining single crystalline and transparent MgO thin films. The films crystallize in a cubic structure and X‐ray diffraction measurements have shown that the polycrystalline MgO films prepared at 500°C with (100) and (110) orientations are changed to (100) preferred orientation at 600°C. The MgO phase formation was also confirmed with the recorded Fourier Transform Infrared (FTIR) results. The films deposited at 600°C exhibited highest optical transmittivity (>80%) and the direct band gap energy was found to vary from 4.50 to 5.25 eV with a rise in substrate temperature from 500 to 600°C. The measured sheet resistance and the resistivity of the film prepared at 600°C were respectively 10¹³Ω/□ and 2.06x10⁷Ω cm. The surface morphology of the prepared MgO thin films was examined by atomic force microscopy. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

Synthesis on large area and uniform nanosheet morphology of polycrystalline cobalt oxide Co3O4 obtained from oxidation of Co films in a pure oxygen atmosphere

Large area and uniform nanosheets Co₃O₄ have been fabricated by thermal annealing of cobalt thin film under the DC magnetron sputtering method. The synthesis is based on controlling the simple thermal oxidative formation of precursor Co films. The Co films were heated at 300, 400, and 500 °C for two hours in a pure oxygen atmosphere. At 300 °C, CoO and Co₃O₄ phases appear to survive together. An amount of pure polycrystalline Co₃O₄ nanosheets were observed at 400 °C. The structural and morphological properties of the nanosheets Co₃O₄ were characterized by means of transmission electron microscopy (TEM) and Raman spectroscopy.     

Untersuchung der Volumenstruktur dünner Bi1–xSbx-Schichten

The cross-sectional structure of evaporated Bi_1–xSb_x film has been investigated using electron microscopy and a replica technique. The conditions of film formation were varied by using different hydrocarbon partial pressures. After formation the films were annealed at 150°C. The cross-sectional structure is supposed to be columnary. This is in good agreement with the 〈00.1〉 texture. Grain coarsing during annealing is mainly influenced by the hydrocarbon concentration of the film. The upper part of the film shares most of the hydrocarbons. The correlation between surface- and cross-sectional structure disappeares by formation of an oxid layer.     

Investigations on the HCl gas-phase etching of differently doped and oriented gaas crystals

The influence of the orientation and dopant on the dissolution of GaAs surfaces in H₂–HCl gas mixtures has been investigated. For this purpose the etch rates, temperature regions of different etching behaviour and the corresponding activation energies were determined for temperatures ranging from 540 °C to 945 °C. The etch rate anisotropy is correlated with the three existing temperature regions of different dissolution mechanisms. The orientation-dependent transition temperatures are influenced by the dopant and can be related to the thermodynamic data of the dopant.     

Surface Chemical Bonding States and Ferroelectricity of Pb(Zr0.52Ti0.48)O3 Thin Films

The surface chemical bonding states and the ferroelectric properties of sol‐gel deposited lead zirconate titanate [Pb(Zr_0.52Ti_0.48)O₃, PZT] thin films coated on (111)Pt/Ti/SiO₂/Si substrates were investigated. X‐ray photoelectron spectroscopy (XPS) was used to determine the oxidation state of the surface and the chemical composition as a function of depth in ferroelectric PZT thin layers. Values for the dielectric constant and dissipation factor at 1 kHz for the 300 nm‐thick film were 1214 and 0.014 for the film annealed at 520 °C, and 881 and 0.015 for a film annealed at 670 °C. Measured values for the remanent polarization (P_r) and coercive field (E_c), from polarization‐electric field (P‐E) hysteresis loops biased at 10 V at a frequency of 100 Hz, were 16.7, 14.4 μC/cm² and 60, 41.7 kV/cm for 520 °C and 670 °C. The leakage current density (J) was 72 and 96 nA/cm² at an applied field of 100 kV/cm. It was found that the bonding states of lead and oxygen in the surface regions could be correlated with the ferroelectric properties of the integrated thin layers.     

Ferroelectric PbTiO3 Powders and Thin Films Derived from Sol-Gel Processing

Lead titanate powders and thin films were prepared by the sol-gel process of metal alkoxide solutions and solvents. From DSC measurements, phase transition temperature of crystallized PbTiO₃ powders was obtained at about 484 °C. From XRD investigation, it was confirmed that the tetragonal phase of polycrystalline PbTiO₃ thin films is formed by coating of concentrated solution on all of the substrates we used after heat treatment above 500 °C. It was found by SEM and ellipsometric analysis that the thin film coated with 0.25 M concentrated solutions once had an average thickness of about 720 Å. Surfaces of thin films were crack-free, uniform, and its average grain size investigated by SEM was 0.6–0.8 μm. Band gap energy of PbTiO₃ thin film coated on the Al₂O₃ (2243) substrate was 3.45 eV, which is assumed to be due to the direct band to band transition. Dielectric constant (ϵ) and dielectric loss (tan δ) of PbTiO₃ thin film amounted to 60–70 and 0.01–0.02 in the region of 10 kHz ∼ 1 MHz at room temperature, respectively, and transition temperature was 486 °C at 1 MHz. From the hysteresis loop of PbTiO₃ thin film, spontaneous polarization of 12 μC/cm² and coercive filed of 45 kV/cm were obtained.     

Influence of arsenic flow on the crystal structure of epitaxial GaAs grown at low temperatures on GaAs (100) and (111)<Emphasis Type="Italic">A</Emphasis> substrates

The influence of arsenic flow in a growth chamber on the crystal structure of GaAs grown by molecular-beam epitaxy at a temperature of 240°C on GaAs (100) and (111)A substrates has been investigated. The flow ratio γ of arsenic As4 and gallium was varied in the range from 16 to 50. GaAs films were either undoped, or homogeneously doped with silicon, or contained three equidistantly spaced silicon δ-layers. The structural quality of the annealed samples has been investigated by transmission electron microscopy. It is established for the first time that silicon δ-layers in “low-temperature” GaAs serve as formation centers of arsenic precipitates. Their average size, concentration, and spatial distribution are estimated. The dependence of the film structural quality on γ is analyzed. Regions 100–150 nm in size have been revealed in some samples and identified (by X-ray microanalysis) as pores. It is found that, in the entire range of γ under consideration, GaAs films on (111)A substrates have a poorer structural quality and become polycrystalline beginning with a thickness of 150–200 nm.     

New gaseous impurity and its effect on the purity of LPE GaAs

The present work describes a new gaseous impurity source of GaAs grown by the conventional liquid phase epitaxy. A large quantity of impurity gas of mass number 16 was detected in the LPE atmosphere even when H₂O vapour and O₂ residual gas were exhausted almost completely. The impurity gas was only detected in the presence of H₂ and a graphite boat at high temperature, and above 850°C this was exaggerated. From comparison of the mass-spectrum of standard gas, the impurity gas was identified as methane. An amount of 130 ppm of methane in H₂ resulted in a carrier concentration of LPE GaAs higher than 10¹⁶ cm^-3.     

Edge misfit dislocations in the GeSi/Si(001) pair: Conditions and specific features of high-quantity generation

Dislocation structure of Ge_xSi_1?x films (x=0.4?0.8) grown by molecular-beam epitaxy on Si(001) substrates was studied by means of transmission electron microscopy. It was found that the density of edge MDs formed at the early stage of plastic strain relaxation in the films could exceed the density of 60° MDs. In our previous publications, a predominant mechanism underlying the early formation of edge misfit dislocations (MD) in Ge_xSi_1?x/Si films with x>0.4 was identified; this mechanism involves the following processes. A 60° glissile MD provokes nucleation of a complementary 60° MD gliding on a mirror-like tilted plane (111). A new edge MD forms as a result of interaction of the two complementary 60° MDs, and the length of the newly formed edge MD can then be increased following the motion of the “arms” of the complementary 60° MDs. Based on this scenario of the edge MD generation process, we have calculated the critical thickness of insertion of an edge MD into GeSi layers of different compositions using the force balance model. The obtained values were found to be more than twice lower than the similar values for 60° MDs. This result suggests that a promising strategy towards obtaining dislocation arrays dominated by 90° dislocations in MBE-grown Ge_xSi_1?x/Si films can be implemented through preliminary growth on the substrate of a thin, slightly relaxed buffer layer with 60° MDs present in this layer. The dislocated buffer layer, acting as a source of threading dislocations, promotes the strain relaxation in the main growing film through nucleation of edge MDs in the film/buffer interface. It was shown that in the presence of threading dislocations penetrating from the relaxed buffer into the film nucleation of edge MDs in the stressed film can be initiated even if the film thickness remains small in comparison with the critical thickness for insertion of 60° MDs. Examples of such unusual MD generation processes are found in the literature.     

Synthesis of zinc oxide crystals with different shapes from zincate aqueous solutions stabilized with triethanolamine

ZnO crystals were synthesized from basic aqueous solutions including zincate ions stabilized with triethanolamine (N(C₂H₄OH)₃, teaH₃) by heating at 60°C. The influence of the basicity of the solutions on the morphology of the ZnO crystals was examined. The aqueous solutions were prepared using ZnSO₄·7H₂O, N(CH₃)₄OH (TMAOH), and teaH₃ as a zinc source, a base, and a stabilizer, respectively, at a zinc concentration of 0.2 M at a teaH₃ / Zn molar ratio of 4. Clear solutions were obtained at a molar ratio of TMAOH / Zn ≥ 3.0. When the clear solutions, in which glass or polyester substrates were placed, were heated at 60°C, agglomerates of ZnO crystals were deposited on the substrates in the TMAOH / Zn range from 3.0 to 3.6. With increasing the TMAOH / Zn ratio, the shape of the resulting ZnO crystals changed from a short asymmetric column with a hexagonal flat edge and a rounded one, through a rocket‐like shape formed by intergrowth, to a hexagonal rod. Although no films of ZnO were formed, ZnO crystals with different shapes were synthesized. When the glass substrates pre‐coated with a ZnO thin film by a sol‐gel method were used, highly oriented, dense ZnO films were formed. The films consisted of rod‐like crystals aligned normal to the substrate surface. (© 2007 WILEY‐VCH Verlag GmbH & Co. KGaA, Weinheim)     

On the Influence of Short R.T. preageing on the formation of the η′-phase in an Al-Zn(4.5 at.%)-Mg(2.5 at.%) alloy

The influence of short R.T. preageing (1 min) after quenching from 480 °C into RT-water on the formation of the η′-phase in an Al-Zn(4.5)-Mg(2.5) alloys has been investigated by means of TEM, XSAS, resistivity, and hardness measurements in the ageing temperature range between T_a = 120 °C comparing samples directly quenched (DQ) to T_a and those quenched into RT-water, kept there for 1 min, and subsequently stored in an oil-bath of T_a (IQ). At T_a ≦ 170 °C both heat treatments result in finely distributed precipitates of the η′-phase accompanied by a fairly high hardness value. But at T_a ≧ 180 °C the DQ leads only to few coarse heterogeneously formed η′- and η-precipitates, whilst the IQ yields qualitatively the same precipitation structure as already described at T_a ≦ 170 °C even till 280 °C. These results are interpreted assuming that. A1) the limitation temperature of homogeneous formation of η′ is located at about T_h = 175°c and A2) during the pre-ageing at RT “nucleation sites” are formed as already suggested by RYUM, which are able to act as sites for heterogeneous formation of η′ even at T_a > T_h. Hints are obtained that the formation of these “nucleation sites” is not so strongly governed by the quenched-in excess vacancies as discussed in the literature.