Effects of annealing temperature on structural,optical, and electrical properties of antimony-doped tin oxide thin films

Antimony-doped tin oxide (ATO) films, approximately 320 nm in thickness, have been prepared by electron beam evaporation onto glass substrates. The films were annealed at temperatures between 400°C and 550°C in air and their structure and surface morphologies were observed by X-ray diffraction (XRD) and atomic force microscopy (AFM) after the different annealing treatments. XRD patterns of the ATO thin films as-deposited and annealed at 400°C showed that they were amorphous, but annealing beyond 400°C caused the films to become polycrystalline with tetragonal structure and orientated in the (1 1 0) direction. The grain size in the annealed films, obtained from the XRD analysis, was in the range 146–256 Å and this increased with the annealing temperature. The dislocation density, cell volume and strain were found to decrease gradually with increasing annealing temperature. Photoluminescence spectra revealed an intensive blue/violet peak at 420 nm, which increased gradually in height with annealing. It is suggested that an increase in the population of Sb⁺⁵ ions might be the reason for the enhancement of the blue/violet emission. The optical properties of the films were also investigated in the UV-visible-NIR region (300–1000 nm). The optical constants, namely the refractive index n and the extinction coefficient k in the visible region were calculated. The optical energy band gap, as determined by the dependence of the absorption coefficient on the photon energy at short wavelengths, was found to increase from 3.59 to 3.76 eV with annealing temperature.     

Morphological and magnetic response of copper-substituted nickel ferrite nanoparticles

Ferrite nanoparticles are interesting materials owing to their unique physical and chemical properties. The metal-doped ferrites have well-defined structures and magnetic response, such as high permeability for a specific frequency range. In this study, copper-substituted nickel ferrite (Ni_1?xCu_xFe₂O₄) nanoparticles with a compositional range of 0?≤?x?≤?0.3 were synthesised through a co-precipitation technique. Metal chlorides were used as precursors and NaOH as a precipitating agent for the growth of ferrite nanoparticles. To minimise the internal stresses and maximise the magnetic response, ferrite nanoparticles were annealed in a furnace at 700°C for 6 h. The structural and magnetic response of Ni_1?xCu_xFe₂O₄ ferrite with different values of x were investigated using Scanning Electron Microscopy (SEM), Fourier Transform Infrared spectroscopy (FT-IR), Vibrating Sample Magnetometer (VSM) and X-ray Diffraction (XRD) techniques. XRD analysis confirmed the formation of cubic spinel structure of single phase for all the compositions. The lattice constant decreased with increase in the value of x. FT-IR study showed two main metal oxygen bonds in the range 500–700 cm^?1 confirming the formation of a single-phase cubic inverse structure of Cu-substituted Ni ferrite. VSM results revealed the formation of ferrimagnetic nanoparticles. The optical and magnetic response of the ferrite nanoparticles changed with Cu content.     

Hydrothermal growth of ZnO nanoparticles under different conditions

In this study, a simple low-temperature hydrothermal method was used to synthesize ZnO nanoparticles. The structural, morphological and optical characterizations of the nanoparticles were evaluated with regard to the zinc content. To achieve this, the molar ratios of the precursors were changed from 0.05 to 0.1 M. The structural and morphological analyses showed that all samples had a polycrystalline hexangular wurtzite crystal structure and the shape of the ZnO nanoparticles changed with increasing zinc content. A possible growth mechanism of the ZnO nanoparticles is explained in terms of the zinc content. Optical measurement revealed that the shape of the nanoparticles affects the position of the band-edge emission as well as the shape of the luminescence spectrum.     

An explanation for the low-temperature H evolution peak in hydrogenated amorphous silicon films deposited 'on the edge of crystallinity'

The puzzling existence of a sharp low-temperature (T = 400°C) H evolution peak in compact hydrogenated amorphous silicon (a-Si : H) films deposited 'on the edge of crystallinity' is examined. From infrared absorption and X-ray diffraction (XRD) measurements, we show that none of the standard methods used to explain the existence of this peak in a-Si : H materials is applicable to the present films. From the Si-H wag-mode peak frequency, we postulate the existence of very small Si crystallites contained within the amorphous matrix. While the crystallite volume fraction is too small to be detected by XRD in the as-grown films, crystallization is observed for this material at anneal temperatures as low as 500°C. It is proposed that these crystallites catalyse the crystallization of the remainder of the amorphous matrix upon moderate annealing, enabling H surface desorption and H₂ out-diffusion to the sample surface along newly formed grain boundaries at low anneal temperatures.     

In situ measurement of GaN film photoluminescence under plasma etching

This work focuses on an improved method that enables us to measure in situ GaN film photoluminescence (PL) under Ar or N₂ plasma etching. Although the background signal is large and increases with bias voltage, the GaN PL can be obtained after subtraction of this background from the total luminescence. Moreover, after plasma etching, the intensities of the near-band-edge and the yellow luminescence decrease significantly. It is suggested that this behaviour is strongly related to the heavy plasma-induced damage, which includes non-radiative defects and deep-level defects, such as Ga vacancies and/or C impurities.     

Synthesis and characterizations of NiTiO3 nanoparticles prepared by the sol–gel process

Nanocrystalline nickel titanate (NiTiO₃) composite powders were prepared by the sol–gel process combined with a surfactant-assisted template method. The resulting powders were calcined at different temperatures ranging from 150°C to 750°C for 2 h in air. The results revealed that a pure hexagonal phase of NiTiO₃ could be obtained at the low temperature of 750°C. The phase evolution of NiTiO₃ was investigated by X-ray diffraction patterns, Fourier-transform infrared spectroscopy, and X-ray photoelectron spectroscopy. Particle size and morphology were studied by transmission electron microscopy.     

Nucleation of misfit dislocations in strained-layer InGaAs on GaAs

Abstract

Austenitic 316L stainless steel alloys annealed at 550°C for 100 h present a few ferrite precipitates surrounded by a new interfacial phase, here called the I-phase, that develops at the level of the austenite/ferrite interface. The I-phase presents the typical patterns of an icosahedral quasicrystal with a primitive hypercubic lattice of parameter A = 0.63 nm. The marked orientation relationships between the I-phase and the ferrite precipitates strongly suggest that this phase results from a decomposition of the ferrite and not of the austenite. The I-phase is metastable and transforms eventually after annealing at 700°C to the stable crystalline σ-phase.     

Enhanced grain growth in yttria-doped zirconia thin film structures synthesized under photon irradiation

Enhanced grain growth in ultra-thin yttria-doped zirconia (YDZ) films synthesized under ultraviolet (UV) irradiation is reported. The mean grain size in UV-synthesized 7.5 mol% YDZ films nearly 56 nm thick increased to 85 nm upon annealing in an oxygen-rich ambient at 900°C for 1 h, while in thermally grown YDZ they grew only to ～15 nm under identical annealing conditions. In situ electron microscopy kinetic studies reveal an enhanced kinetic constant and self-limiting grain growth behaviour in the UV-synthesized oxide films. The difference between UV and thermally grown films was not significant in undoped films when compared to the case of 7.5 mol% YDZ.     

Tuning the structure of MoO3 nanoplates via MoS2 oxidation

Orthorhombic phase MoO₃ (α-MoO₃) nanoplates were synthesized by oxidizing MoS₂ nanoplates in air at 300?°C, while α-MoO₃ microplates were achieved by directly evaporating MoO₃ powders at 800?°C. Much thinner α-MoO₃ nanoplates were characterized by scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy and micro Raman spectroscopy. This experiment may provide a pathway to the formation of α-MoO₃ nanoplates.     

Improvement in mechanical properties of commercially pure titanium through reverse rolling

Commercially pure (cp) titanium plates were subjected to 90% reduction in thickness through UDR (unidirectional rolling) and RR (reverse rolling) in the cold-rolling route. These rolled plates were then annealed at 600 °C for 20 min. The plates processed through UDR and RR exhibited similar values of ductility, but the plates subjected to RR exhibiting a significant increase in their strength compared to those rolled through UDR. However, on annealing the yield strength of the RR plate was reduced slightly while its ductility improved. Relative growths of dislocation density in the samples appeared to be responsible for such differences in the mechanical properties of the samples.     

Light emission from ferroelectric barium titanate nanocrystals

Thin laminates (thickness δ = 20–45 nm) of barium titanate, BaTiO₃ (BT), have been synthesised by the sol–gel method followed by heating of the amorphous precursor powder in air. An orthorhombic BT polymorph forms along with a tetragonal phase (t-BT) after 2 h of heating the precursor at 600°C, as evidenced by a well-defined X-ray diffraction pattern. The average crystallite size D ～ 21 nm compares the δ-value obtained from the scanning electron micrograph. On heating at temperatures as high as 750°C, the structure remains mostly t-BT (D ? 44 nm), which emits violet–blue–green light at a wavelength of 380–580 nm with a maximum at around 422 nm. The emission extends to wavelengths shorter than ～300 nm owing to a quantum-size effect in smaller crystals processed at lower temperatures. Electron paramagnetic resonance (EPR), which occurs at a g-value of 1.995 (linewidth ΔH = 1.12 mT) in a sample heated at 400°C, shows an order of magnitude of lower intensity at g = 1.993 (ΔH = 3.69 mT) on annealing out the paramagnetic defects at 600°C in air. No EPR signal arises in t-BT free from such defects in larger crystals.     

Coarsening behaviour of gamma prime precipitates and concurrent transitions in the interface width in Ni-14 at.% Al-7 at.% Cr

Coupling atom probe tomography and transmission electron microscopy, the temporal evolution of γ′ precipitate morphology and size distribution and compositional width of the γ/γ′ interface, have been tracked in a model Ni-14Al-7Cr (at.%) alloy, during isothermal annealing at 800?°C subsequent to rapid quenching. During the initial annealing period, coalescence-dominated growth and coarsening of γ′ precipitates are accompanied by a gradual decrease in the interface width, eventually leading to classical LSW coarsening with a constant interface width at extended annealing time periods.     

Effects of ball milling and annealing of an alloy in the Al-Fe-Cu system: Implications for phase equilibria

An icosahedral quasicrystalline alloy in the Al-Fe-Cu system has been mechanically milled in a high-energy ball mill (Szegvari attritor) for 1, 3, 6 and 10 h. Samples were characterized by X-ray diffraction and transmission electron microscopy. The evolution of nanosize crystallites of the disordered B2 phase (bcc; a = 0.29 nm), coexisting with either the parent icosahedral phase or an amorphous phase, occurs during milling. Isothermal heat treatment of milled powder at various temperatures (200, 500, 600, 700, 800 and 850°C) leads in all cases, except at 200°C, to the transformation from disordered B2 and amorphous phases to an ordered B2 phase with a high degree of long-range ordering. The maximum degree of superlattice ordering was found after isothermal treatment at 800^oC. The implications of these results are discussed with reference to phase equilibria existing between crystalline and quasicrystalline phases in the Al-Fe-Cu system.     

Post-irradiation annealing behaviour of oxide dispersion strengthened Fe-Cr alloys studied by nanoindentation

ABSTRACT

To study the nature of irradiation-induced nanofeatures in oxide dispersion strengthened (ODS) Fe-Cr alloys, post-irradiation isochronal thermal annealing up to 600°C was performed for ODS Fe-9%Cr and Fe-14%Cr alloys ion-irradiated at 300°C and 500°C. Nanoindentation indicated hardening for all as-irradiated alloys and complete hardness recovery upon post-irradiation annealing. Cross-sectional TEM indicated an irradiation-induced defect band near peak damage mainly consisting of dislocation loops. Candidate mechanisms of recovery were critically evaluated. Shrinkage of loops via capture of thermal vacancies was found to correctly reflect the annealing behaviour of ODS Fe-9Cr irradiated at 300°C.     

Experimental and simulated grain boundary groove profiles in tungsten

Grain-boundary grooving has been studied on polished surfaces of polycrystalline tungsten annealed at 1350°C. Atomic force microscopy images were taken in the same area for each groove after different annealing times. Secondary oscillations next to the main groove maxima (predicted for grooving by surface diffusion) were observed, to our knowledge for the first time. The agreement between experimental and calculated groove profiles (using the surface diffusion model of Mullins (1957, J. appl. Phys., 28, 333)) improved when grain-boundary fluxes were introduced.     

Recrystallization of amorphous ion-implanted silicon carbide after thermal annealing

Single crystals of 6H–SiC were implanted at room temperature with 4-MeV Au ions to a fluence of 10^15?cm^?2. Raman spectra showed that full amorphization was achieved. The recrystallization process was studied by micro-Raman spectrometry after isochronal thermal annealing between 700 and 1500°C. The spectra permitted the evolution upon annealing of Si–C bonds, and also of Si–Si and C–C bonds, to be followed. Amorphous phase relaxation takes place below 700°C; then recrystallization of the 6H polytype sets in at 700°C. At 900°C crystallites with different crystalline states are formed. Moreover, Raman spectra provide evidence of graphitic nanocluster formation at 1500°C.     

Recrystallization in a low-density low-alloy Fe–Mn–Al–C duplex-phase alloy

The recrystallization behaviour of a cold-rolled, low-density, low-alloy duplex-phase alloy (Fe–6.57Al–3.34Mn–0.18C, wt.%) has been studied. Temperature-resolved X-ray diffraction and dilatometry showed that the alloy recrystallizes at 850?°C during continuous heating. However, electron back-scattered diffraction investigations using Kernel average misorientation revealed that during annealing ferrite recrystallizes at lower temperatures while austenite remains strained up to 1200?°C. This study underlines the complexity of recrystallization of a microstructure comprising of constituents with high and low stacking fault energy.     

Tailoring the crack-tip microstructure: a novel approach

This investigation demonstrates a way to innovatively modify the ferritic microstructure at a local scale, particularly at the failure prone area such as Charpy V-notch (CVN) root. Tensile pre-strain (PS) up to 6% and 12% were employed before annealing (An) the samples at 650°C for 15?minutes. Ferrite grain size increased sharply and gradually (along the distance ahead of the notch root) within the microstructurally modified region in 6–12% pre-strained and annealed samples, respectively. The critical strain which promotes strain-induced boundary migration (SIBM), was found to be 0.1 which resulted in abnormally coarse ferrite grains.     

Kinetic study of static recrystallization in an Fe–Al–O ultra-fine-grained nanocomposite

A nearly abrupt coarsening of grains is observed in a newly developed Fe–Al–O ultra-fine-grained nanocomposite with a significant volume fraction (4%) of alumina nano-precipitates. The microstructure of the alloy was analysed in different states (as-received and annealed) by means of scanning electron microscopy, transmission electron microscopy (TEM) and hardness. The initial grain size 150–200 nm increases up to 50 μm during annealing 1000 °C/8 h and thereafter demonstrates saturation. A linear correlation between volume fraction of coarse grains and hardness was found. It was identified by TEM that alumina nano-precipitates stabilize the dislocation microstructure against recovery very effectively and the grain coarsening is due to fast growth of very few dislocation free grains. Thus, the observed grain coarsening has the attributes of static recrystallization.     

Microstructural features of phase transformation in a binary Pd–Si metallic glass

Glassy ribbons of Pd–Si alloys were prepared by a combination of melt spinning and flux treatment. The crystallization behaviour of a Pd₈₁Si₁₉ glassy alloy was studied through isothermal annealing at temperatures ranging lower than the glass-transition temperature T _g to around the onset of crystallization. The evolution of microstructures arising from isothermal annealing was investigated by X-ray diffraction (XRD) and (high-resolution) transmission electron microscopy ((HR)TEM). XRD spectra showed that, after the sample was annealed at a sub-T _g temperature, its first diffraction peak was split into two overlapping broad peaks. TEM analysis revealed the formation of a spherical, particle-like glassy phase embedded in the glassy matrix together with a finely connected network morphology within both. Combining these observations with compositional analysis suggested that phase separation had taken place during sub-T _g annealing. When the glassy alloy was annealed at temperatures higher than T _g, nanocrystalline structures, composed of Pd₃Si and Pd phases plus a Pd₉Si₂ phase with a lamellar structure, was formed.