Influence of annealing temperature on structural and optical properties of ZnO: In thin films prepared by ultrasonic spray technique

Transparent conducting indium doped zinc oxide was deposited on glass substrate by ultrasonic spray method. The In doped ZnO samples with indium concentration of 3 wt.% were deposited at 300, 350 and 400 °C with 2 min of deposition time. The effects of substrate temperature and annealing temperature on the structural, electrical and optical properties were examined. The DRX analyses indicated that In doped ZnO films have polycrystalline nature and hexagonal wurtzite structure with (0 0 2) preferential orientation and the maximum average crystallite size of ZnO: In before and annealed at 500 °C were 45.78 and 55.47 nm at a substrate temperature of 350 °C. The crystallinity of the thin films increased by increasing the substrate temperature up 350 °C, the crystallinity improved after annealing temperature at 500 °C. The film annealed at 500 °C and deposited at 350 °C show lower absorption within the visible wavelength region. The band gap energy increased from E_g = 3.25 to 3.36 eV for without annealing and annealed films at 500 °C, respectively, indicating that the increase in the transition tail width. This is due to the increase in the electrical conductivity of the films after annealing temperature.     

Structural characterizations of Co2MnSi/MgO/Co2MnSi magnetic tunnel junctions by transmission electron microscopy

We have investigated the structure of Co₂MnSi/MgO/Co₂MnSi magnetic tunneling junctions with different tunnel magnetoresistance values depending on the in situ annealing temperatures just after the deposition of the upper Co₂MnSi electrodes. The nano-beam diffraction patterns indicated that the degree of order of the upper Co₂MnSi electrode annealed at 550 °C was higher than that of an electrode annealed at 400 °C. Moreover, the degree of the L2₁ order of the upper Co₂MnSi electrode annealed at 550 °C was even lower than that of the lower Co₂MnSi electrode annealed at an almost equal temperature of 600 °C. Atomic-scale observation using a high-angle annular dark-field (HAADF) method distinctly showed the existence of the L2₁-ordered regions in the B2-ordered matrix in the upper Co₂MnSi electrode annealed at 400 °C.     

Effect of high magnetic field annealing on the microstructure and magnetic properties of Co-Fe layered double hydroxide

The effects of high magnetic field (10 T) on the products obtained by calcination of Co-Fe LDH precursors at different temperatures were investigated. The XRD results indicated that Fe^III substituted for Co^III in Co₃O₄ to yield Co^IICo^IIIFe^IIIO₄ under the calcination of Co-Fe LDH precursors at 400 °C. The products obtained by magnetic field annealing at 400 °C had a porous plate-like morphology, whereas the products without magnetic field annealing were composed of nanoparticles. It was seen that CoFe₂O₄ phase could be formed at low temperature (about 500 °C) under the magnetic field annealing. The grain size of products obtained by magnetic field annealing at 800 °C was larger than that of zero magnetic field. It was found that the saturation magnetization was significantly enhanced after magnetic field annealing, especially at lower temperature (≤600 °C). The possible reason for the effects on the microstructure and magnetic properties of products obtained by magnetic field annealing was discussed.     

Crystallization and electrochemical performance of La0.6Sr0.4Co0.2Fe0.8O3 − δ-Ce0.8Gd0.2O1.9 thin film cathodes processed by single solution spray pyrolysis

La_0.6Sr_0.4Co_0.2Fe_0.8O_3 − δ-Ce_0.8Gd_0.2O_1.9 (LSCF-CGO) thin films obtained by spray pyrolysis of a single precursor solution were investigated by XRD, TEM and impedance spectroscopy at annealing temperatures ranging from 500 to 900 °C. Films annealed at 600 °C contained a mixture of amorphous regions and crystalline regions composed of fine crystallites (< 5 nm). Annealing above 600 °C increased the ratio of crystalline to amorphous material, led to the segregation of the films into distinct LSCF and CGO phases, and promoted grain growth. The electrical behavior of the films depended on annealing temperature. At testing temperatures of 400 °C and below, the polarization resistance of films with lower annealing temperatures was larger than the polarization resistance of films with higher annealing temperatures. However, at testing temperatures of 500 °C and above the polarization resistance of films with lower annealing temperatures was equal to or lower than the polarization resistance of films with higher annealing temperatures. This was reflected by the activation energy that decreased with increasing annealing temperature. The varying electrical behavior may be related to microstructural changes that caused bulk diffusion to be the rate-limiting step in films with lower annealing temperatures and oxygen dissociation to be the rate-limiting step in films with higher annealing temperatures.     

Crystallization of amorphous Co2MnSi thin film

Amorphous Co₂MnSi thin film was deposited using radio-frequency sputtering. The amorphous film crystallized into a single-phased L2₁ structure at 500 °C, which was highly disordered. The structure was meta-stable as the crystallized film decomposed upon further heating. Increasing the annealing temperature to 600 °C precipitated fcc Co together with Co₂MnSi. Magnetic measurements showed that the as-deposited amorphous film was paramagnetic, exhibiting a spin glass state below 44 K. The phase transition at 500 °C produced a ferromagnetic Co₂MnSi thin film whose saturation magnetic moment was considerably lower than reported values due to the disordered structure of the crystallized film.     

Investigation of thermal annealing effects on microstructural and optical properties of HfO2 thin films

In the present paper, we investigate the effect of thermal annealing on optical and microstructural properties of HfO₂ thin films (from 20 to 190 nm) obtained by plasma ion assisted deposition (PIAD). After deposition, the HfO₂ films were annealed in N₂ ambient for 3 h at 300, 350, 450, 500 and 750 °C. Several characterisation techniques including X-ray reflectometry (XRR), X-ray diffraction (XRD), spectroscopic ellipsometry (SE), UV Raman and FTIR were used for the physical characterisation of the as-deposited and annealed HfO₂ thin films. The results indicate that as-deposited PIAD HfO₂ films are mainly amorphous and a transition to a crystalline phase occurs at a temperature higher than 450 °C depending on the layer thickness. The crystalline grains consist of cubic and monoclinic phases already classified in literature but this work provides the first evidence of amorphous-cubic phase transition at a temperature as low as 500 °C. According to SE, XRR and FTIR results, an increase in the interfacial layer thickness can be observed only for high temperature annealing. The SE results show that the amorphous phase of HfO₂ (in 20 nm thick samples) has an optical bandgap of 5.51 eV. Following its transition to a crystalline phase upon annealing at 750 °C, the optical bandgap increases to 5.85 eV.     

Effects of annealing temperature on structure and magnetic properties of amorphous Fe61Co27P12 nanowire arrays

Arrays of Fe₆₁Co₂₇P₁₂ nanowire with an aspect ratio about 70 were prepared in anodic aluminum oxide templates by electrodeposition. The influences of annealing temperature on structure and magnetic properties of Fe₆₁Co₂₇P₁₂ nanowires were studied. When the specimens were annealed below 400 °C, there are no obvious changes in structure except relaxation. With the annealing temperature increasing from 400 to 600 °C, the Fe-Co phase is detected by X-ray diffraction and Mössbauer spectra. The crystalline fraction and hyperfine field can be derived from Mössbauer spectra. The room temperature magnetic hysteresis loops show that the coercivity and squareness of the nanowire arrays in parallel to the wire axis increase with the increasing of annealing temperature, which mainly attributes to the strengthening of anisotropy.     

Annealing effects on structural, optical and electrical properties of e-beam evaporated CuIn0.5Ga0.5Te2 thin films

CuIn_0.5Ga_0.5Te₂ (CIGT) thin films have been prepared by e-beam evaporation from a single crystal powder synthesized by direct reaction of constituent elements in a stoichiometric proportion. Post-depositional annealing has been carried out at 300 and 350 °C. The compositions of the films were determined by energy dispersive X-ray analysis (EDXA) and it was found that there was a remarkable fluctuation in atomic percentage of the constituent elements following to the post-depositional annealing. X-ray diffraction analysis (XRD) has shown that as-grown films were amorphous in nature and turned into polycrystalline structure following to the annealing at 300 °C. The main peaks of CuIn_0.5Ga_0.5Te₂ and some minor peaks belonged to a binary phase Cu₂Te appeared after annealing at 300 °C, whereas for the films annealed at 350 °C single phase of the CuIn_0.5Ga_0.5Te₂ chalcopyrite structure was observed with the preferred orientation along the (1 1 2) plane. The effect of annealing on and near surface regions has been studied using X-ray photoelectron spectroscopy (XPS). The results indicated that there was a considerable variation in surface composition following to the annealing process. The transmission and reflection measurements have been carried out in the wavelength range of 200-1100 nm. The absorption coefficients of the films were found to be in the order of 10⁴ cm⁻¹ and optical band gaps were determined as 1.39, 1.43 and 1.47 eV for as-grown and films annealed at 300 and 350 °C, respectively. The temperature dependent conductivity and photoconductivity measurements have been performed in the temperature range of −73 to 157 °C and the room temperature resistivities were found to be around 3.4 × 10⁷ and 9.6 × 10⁶ (Ω cm) for the as-grown and annealed films at 350 °C, respectively.     

Structure and magnetic properties of nanocrystalline cobalt ferrite powders synthesized using organic acid precursor method

Nanocrystalline octahedra of cobalt ferrite CoFe₂O₄ powders were synthesized using the organic acid precursor route. The effect of the calcination temperature, Fe³⁺/Co²⁺ molar ratio, calcination time and type of organic acid (oxalic, benzoic and tartaric acids) on the formation, crystallite size, microstructure and magnetic properties was studied systematically. The Fe³⁺/Co²⁺ molar ratio was varied from 2 to 1.739 while the annealing temperature was controlled from 400 to 1000 °C for various periods from 0.5 to 2 h. The resulting powders were investigated using X-ray diffraction (XRD) analysis, Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and vibrating sample magnetometer (VSM). XRD results indicate that a well crystallized, single spinel cobalt ferrite phase was formed for the precursors annealed at 600-800 °C for 2 h, using oxalic and tartaric acids as precursors for Fe³⁺/Co²⁺ molar ratio 1.818. The crystallite size of as-formed powders was in the range of 38.0-92.6 nm at different operating conditions. The calcination temperature and Fe³⁺/Co²⁺ molar ratio have a significant effect on the microstructure of the produced cobalt ferrite. The microstructure of the produced powders was found to be octahedra-shaped. The crystalline, pure cobalt ferrite powders with magnetic properties having a maximum saturation magnetization (76.1 emu/g) was achieved for the single phase at Fe³⁺/Co²⁺ molar ratio 1.818 and annealing temperature of 600 °C for 2 h using tartaric acid precursor.     

Growth, structural and optical transport properties of nanocrystal Zn1−xCdS thin films deposited by solution growth technique (SGT) for photosensor applications

Solution Growth Technique (SGT) has been used for deposition of Zn_1−xCdS nanocrystalline thin films. Various parameters such as solution pH (10.4), deposition time, concentration of ions, composition and deposition and annealing temperatures have been optimized for the development of device grade thin film. In order to achieve uniformity and adhesiveness of thin film on glass substrate, 5 ml triethanolamine (TEA) have been added in deposition solution. The as-deposited films have been annealed in Rapid Thermal Annealing (RTA) system at various temperature ranges from 100 to 500 °C in air. The changes in structural formation and optical transport phenomena have been studied with annealing temperatures and composition value (x). As-deposited films have two phases of ZnS and CdS, which were confirmed by X-ray diffraction studies; further the X-ray analysis of annealed (380 °C) films indicates that the films have nanocrystalline size (150 nm) and crystal structure depends on the films stoichiometry and annealing temperatures. The Zn_0.4CdS films annealed at 380 °C in air for 5 min have hexagonal structure where as films annealed at 500 °C have represented the oxide phase with hexagonal structure. Optical properties of the films were studied in the wavelength range 350-1000 nm. The optical band gap (E_g=2.94-2.30 eV) decreases with the composition (x) value. The effect of air rapid annealing on the photoresponse has also been observed on Zn_1−xCdS nanocrystal thin films. The Zn_1−xCdS thin film has higher photosensitivity at higher annealing temperatures (380-500 °C), and films also have mixed Zn_1−xCdS/Zn_1−xCdSO phase with larger grain size than the as-deposited and films annealed up to 380 °C. The present results are well agreed with the results of other studies.     

Structural and magnetic properties of RF sputtered FePt/Fe multilayers

Series of [FePt(4min)/Fe(t_Fe)]₁₀ multilayers have been prepared by RF magnetron sputtering and post-annealing in order to optimize their magnetic properties by structural designs. The structure, surface morphology, composition and magnetic properties of the deposited films have been characterized by X-ray diffractometer (XRD), Rutherford backscattering (RBS), scanning electron microscope (SEM), energy dispersive X-ray spectroscope (EDX) and vibrating sample magnetometer (VSM). It is found that after annealing at temperatures above 500 °C, FePt phase undergoes a phase transition from disordered FCC to ordered FCT structure, and becomes a hard magnetic phase. X-ray diffraction studies on the series of [FePt/Fe]_n multilayer with varying Fe layer thickness annealed at 500 and 600 °C show that lattice constants change with Fe layer thickness and annealing temperature. Both lattice constants a and c are smaller than those of standard ones, and lattice constant a decreases as Fe layer deposition time increases. Only a slight increase in grain size was observed as Fe layer decreased in samples annealed at 500 °C. However, the increase in grain size is large in samples annealed at 600 °C. The coercivities of [FePt/Fe]_n multilayers decrease with Fe layer deposition time, and the energy product (BH)_max reaches a maximum in the samples with Fe layer deposition time of 3 min. Comparison of magnetic properties with structure showed an almost linear relationship between the lattice constant a and the coercivities of the FePt phase.     

Thermal stability of Ag films in air prepared by thermal evaporation

The thermal stability of silver films in air has been studied. Pure Ag films, 250 nm in thickness, were prepared on glass substrates by thermal evaporation process, and subsequently annealed in air for 1 h at temperatures between 200 and 400 °C. The structure and morphology of the samples were investigated by X-ray diffraction, Raman spectra and atomic force microscopy. It is found that the crystallization enhances for the annealed films, and film surface becomes oxidized when annealing temperature is higher than 350 °C. The electrical and optical properties of the films were studied by van der Pauw method and spectrophotometer, respectively. Reflectance drops sharply as Ag films are annealed at temperatures above 250 °C. Film annealed at 250 °C has the maximum surface roughness and the minimum reflectance at 600 nm optical wavelength. Film annealed at 200 °C has the minimum resistivity, and resistivity increases with the increasing of the annealing temperature when temperature is above 200 °C. The results show that both oxidization on film surface and agglomeration of silver film result in infinite of electrical resistivity as the annealing temperature is above 350 °C.     

Influence of temperature annealing on optical properties of SrTiO3/BaTiO3 multilayered films on indium tin oxide

We have prepared SrTiO₃/BaTiO₃ thin films with multilayered structures deposited on indium tin oxide (ITO) coated glass by a sol-gel deposition and heating at 300-650 °C. The optical properties were obtained by UV-vis spectroscopy. The films show a high transmittance (approximately 85%) in the visible region. The optical band gap of the films is tunable in the 3.64-4.19 eV range by varying the annealing temperature. An abrupt decrease towards the bulk band gap value is observed at annealing temperatures above 600 °C. The multilayered film annealed at 650 ° C exhibited the maximum refractive index of 2.09-1.91 in the 450-750 nm wavelength range. The XRD and AFM results indicate that the films annealed above 600 ° C are substantially more crystalline than the films prepared at lower temperatures which were used to change their optical band gap and complex refractive index to an extent that depended on the annealing temperature.     

Magnetic,structural and electrical properties of ordered and disordered Co50Fe50 films

Co₅₀Fe₅₀ films with thickness varying from 100 to 500 Å were deposited on a glass substrate by sputtering process, respectively. Two kinds of CoFe films were studied: one was the as-deposited film, and the other the annealed film. The annealing procedure was to keep the films at 400 °C for 5 h in a vacuum of 5×10⁻⁶ mbar. From the X-ray study, we find that the as-deposited film prefers the CoFe(1 1 0) orientation. Moreover, the body-centered cubic (bcc) CoFe(1 1 0) line is split into two peaks: one corresponding to the ordered body-centered tetragonal (bct) phase, and the other, the disordered bcc phase. After annealing, the peak intensity of the ordered bct phase becomes much stronger, while that of the disordered bcc phase disappears. The annealing has also caused the ordered CoFe(2 0 0) line to appear. When the amount of the ordered bct phase in Co₅₀Fe₅₀ is increased, the saturation magnetization (M_s) and coercivity (H_c) become larger, but the electrical resistivity (ρ) decreases. From the temperature coefficient of resistance (TCR) measurement, we learn that the bct grains in the CoFe film start to grow at temperature 82 °C.     

Effects of rapid thermal annealing on structural, magnetic and optical properties of Ni-doped ZnO thin films

XPS depth profiles were used to investigate the effects of rapid thermal annealing under varying conditions on the structural, magnetic and optical properties of Ni-doped ZnO thin films. Oxidization of metallic Ni from its metallic state to two-valence oxidation state occurred in the film annealed in air at 600 °C, while reduction of Ni²⁺ from its two-valence oxidation state to metallic state occurred in the film annealed in Ar at 600 and 800 °C. In addition, there appeared to be significant diffusion of Ni from the bottom to the top surface of the film during annealing in Ar at 800 °C. Both as-deposited and annealed thin films displayed obvious room temperature ferromagnetism (RTFM) which was from metallic Ni, Ni²⁺ or both with two distinct mechanisms. Furthermore, a significant improvement in saturation magnetization (M_s) in the films was observed after annealing in air (M_s = 0.036 μ_B/Ni) or Ar (M_s = 0.033 μ_B/Ni) at 600 °C compared to that in as-deposited film (M_s = 0.017 μ_B/Ni). An even higher M_s value was observed in the film annealed in Ar at 800 °C (M_s = 0.055 μ_B/Ni) compared to that at 600 °C mainly due to the diffusion of Ni. The ultraviolet emission of the Ni-doped ZnO thin film was restored during annealing in Ar at 800 °C, which was also attributed to the diffusion of Ni.     

Comparative study on the effect of annealing treatments on RTL mechanism in natural quartz from different origins

The behaviour of trap centres and luminescence centres has been investigated for fired and unfired natural quartz from bricks and sediments irradiated at 100 Gy and annealed at different temperatures in the range 350-700 °C. The annealing treatment affects thermoluminescence (TL) glow curve as various changes were observed. The higher sensitization occurred for an annealing in the region 550-600 °C. At this annealing temperature, it has been observed the emergence of two peaks arising at 96 and 180 °C. At lower annealing temperatures, these peaks are overlapped by the peaks localized at 90 and 195 °C, respectively. Concerning the fired quartz, the higher sensitization occurred for an annealing in the region 500-550 °C for peak temperature around 200 °C and an unusual desensitization for the peak temperature around 100 °C. The behaviour of the two types of quartz is analyzed regarding to their kinetic parameters and luminescence emission and compared to literature data.     

Investigation of p-type behavior in Ag-doped ZnO thin films by E-beam evaporation

Ag-doped ZnO (ZnO:Ag) thin films were grown on glass substrates by E-beam evaporation technique. The structural, electrical and optical properties of the films were investigated as a function of annealing temperature. The films were subjected to post annealing at different temperatures in the range of 350-650 °C in an air ambient. All the as grown and annealed films at temperature of 350 °C showed p-type conduction. The films lost p-type conduction after post annealing treatment temperature of above 350 °C, suggesting a narrow post annealing temperature window for the fabrication of p-type ZnO:Ag films. ZnO:Ag film annealed at 350 °C revealed lowest resistivity of 7.25 × 10⁻² Ω cm with hole concentration and mobility of 5.09 × 10¹⁹ cm⁻³ and 1.69 cm²/V s, respectively. Observation of a free-to-neutral-acceptor (e,A^o) and donor-acceptor-pair (DAP) emissions in the low temperature photoluminescence measurement confirms p-type conduction in the ZnO:Ag films.     

High temperature annealing effect on structural and magnetic properties of Ti/Ni multilayers

High temperature annealing effect on structural and magnetic properties of Ti/Ni multilayer (ML) up to 600 °C have been studied and reported in this paper. Ti/Ni multilayer samples having constant layer thicknesses of 50 Å each are deposited on float glass and Si(1 1 1) substrates using electron-beam evaporation technique under ultra-high vacuum (UHV) conditions at room temperatures. The micro-structural parameters and their evolution with temperature for as-deposited as well as annealed multilayer samples up to 600 °C in a step of 100 °C for 1 h are determined by using X-ray diffraction (XRD) and grazing incidence X-ray reflectivity techniques. The X-ray diffraction pattern recorded at 300 °C annealed multilayer sample shows interesting structural transformation (from crystalline to amorphous) because of the solid-state reaction (SSR) and subsequent re-crystallization at higher temperatures of annealing, particularly at ≥400 °C due to the formation of TiNi₃ and Ti₂Ni alloy phases. Sample quality and surface morphology are examined by using atomic force microscopy (AFM) technique for both as-deposited as well as annealed multilayer samples. In addition to this, a temperature dependent dc resistivity measurement is also used to study the structural transformation and subsequent alloy phase formation due to annealing treatment. The corresponding magnetization behavior of multilayer samples after each stage of annealing has been investigated by using Magneto-Optical Kerr Effect (MOKE) technique and results are interpreted in terms of observed micro-structural changes.     

Unidirectional variation of lattice constants of Al-N-codoped ZnO films by RF magnetron sputtering

Al-N-codoped ZnO films were fabricated by RF magnetron sputtering in the ambient of N₂ and O₂ on silicon (1 0 0) and homo-buffer layer, subsequently, annealed in O₂ at low pressure. X-ray diffraction (XRD) spectra show that as-grown and 600 °C annealed films grown by codoping method are prolonged along crystal c-axis. However, they are not prolonged in (0 0 1) plane vertical to c-axis. The films annealed at 800 °C are not prolonged in any directions. Codoping makes ZnO films unidirectional variation. X-ray photoelectron spectroscopy (XPS) shows that Al content hardly varies and N escapes with increasing annealing temperature from 600 °C to 800 °C.     

Influence of deposition temperature on the structural and morphological properties of Be3N2 thin films grown by reactive laser ablation

Be₃N₂ thin films have been grown on Si(1 1 1) substrates using the pulsed laser deposition method at different substrate temperatures: room temperature (RT), 200 °C, 400 °C, 600 °C and 700 °C. Additionally, two samples were deposited at RT and were annealed after deposition in situ at 600 °C and 700 °C. In order to obtain the stoichiometry of the samples, they have been characterized in situ by X-ray photoelectron (XPS) and reflection electron energy loss spectroscopy (REELS). The influence of the substrate temperature on the morphological and structural properties of the films was investigated using scanning electron microscopy (SEM), atomic force microscopy (AFM) and X-ray diffraction (XRD). The results show that all prepared films presented the Be₃N₂ stoichiometry. Formation of whiskers with diameters of 100-200 nm appears at the surface of the films prepared with a substrate temperature of 600 °C or 700 °C. However, the samples grown at RT and annealed at 600 °C or 700 °C do not show whiskers on the surface. The average root mean square (RMS) roughness and the average grain size of the samples grown with respect the substrate temperature is presented. The films grown with a substrate temperature between the room temperature to 400 °C, and the sample annealed in situ at 600 °C were amorphous; while the αBe₃N₂ phase was presented on the samples with a substrate temperature of 600 °C, 700 °C and that deposited with the substrate at RT and annealed in situ at 700 °C.