Effects of post-thermal annealing temperature on the optical and structural properties of gold particles on silicon suboxide films

In this work, silicon suboxide (SiO_x) thin films were deposited using a RF magnetron sputtering system. A thin layer of gold (Au) with a thickness of about 10 nm was sputtered onto the surface of the deposited SiO_x films prior to the thermal annealing process at 400 °C, 600 °C, 800 °C and 1000 °C. The optical and structural properties of the samples were studied using scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR) and optical transmission and reflection spectroscopy. SEM analyses demonstrated that the samples annealed at different temperatures produced different Au particle sizes and shapes. SiO_x nanowires were found in the sample annealed at 1000 °C. Au particles induce the crystallinity of SiO_x thin films in the post-thermal annealing process at different temperatures. These annealed samples produced silicon nanocrystallites with sizes of less than 4 nm, and the Au nanocrystallite sizes were in the range of 7-23 nm. With increased annealing temperature, the bond angle of the Si-O bond increased and the optical energy gap of the thin films decreased. The appearance of broad surface plasmon resonance absorption peaks in the region of 590-740 nm was observed due to the inclusion of Au particles in the samples. The results show that the position and intensity of the surface plasmon resonance peaks can be greatly influenced by the size, shape and distribution of Au particles.     

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.     

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.     

Effect of Co layer thickness on structural and magnetic properties of C/Co/C films

Granular C/Co/C films have been prepared by magnetron sputtering from C and Co onto glass substrates at room temperature and subsequent in situ annealing. It has been found that the structure and magnetic properties of the C/Co/C films depend strongly on the Co layer thickness. Vibrating sample magnetometer measurements indicate that the in-plane coercivities reach maximum in 20 nm Co thickness of both as-deposited and annealed films. The squareness ratio of annealed films was more than 0.8. X-ray diffraction shows that majority Co nanograins are formed as the hexagonal-close-packed (HCP) structure in 20 nm Co thickness with annealing at 400 °C. Scanning probe microscope was used to scan surface morphology and magnetic domain structures. The values of the surface roughness were lower than 0.6 nm in all annealed samples. The average magnetic cluster size was estimated to be about 10 nm in annealed 20 nm Co thickness films.     

Characterization of AgInS2 thin films prepared by vacuum evaporation

We characterized AgInS₂ thin films prepared by vacuum evaporation. In the case of thin films annealed at 400 °C, diffraction peaks were observed only for the chalcopyrite AgInS₂ phase. The chemical composition of the thin films annealed at 400 °C was 26.5 at% Ag, 23.8 at% In, and 49.7 at% S. PL spectra of the AgInS₂ thin films at 10.7 K showed peaks at 1.70, 1.80, and 1.83 eV. The PL peak at1.80 eV was attributed to sulfur deficiency.     

Effects of annealing temperature and method on structural and optical properties of TiO2 films prepared by RF magnetron sputtering at room temperature

TiO₂ thin film was deposited on non-heated Si(1 0 0) substrate by RF magnetron sputtering. The as-deposited films were annealed by a conventional thermal annealing (CTA) and rapid thermal annealing (RTA) at 700 and 800 °C, and the effects of annealing temperature and method on optical properties of studied films were investigated by measuring the optical band gaps and FT-IR spectra. And we also compared the XRD patterns of the studied samples. The as-deposited film showed a mixed structure of anatase and brookite. Only rutile structures were found in samples annealed above 800 °C by CTA, while there are no special peaks except the weak brookite B(2 3 2) peak for the sample annealed at (or above) 800 °C by RTA. FT-IR spectra show the broad peaks due to Ti-O vibration mode in the range of 590-620 cm⁻¹ for the as-deposited film as well as samples annealed by both annealing methods at 700 °C. The studied samples all had the peaks from Si-O vibration mode, which seemed to be due to the reaction between TiO₂ and Si substrate, and the intensities of these peaks increased with increasing of annealing temperature. The optical band gap of the as-deposited film was 3.29 eV but it varied from 3.39 to 3.43 eV as the annealing temperature increased from 700 to 800 °C in the samples annealed by CTA. However, it varied from 3.38 to 3.32 eV as the annealing temperature increased from 700 to 800 °C by RTA.     

Influence of annealing temperature on the structural, optical and mechanical properties of ALD-derived ZnO thin films

ZnO thin films grown on Si(1 1 1) substrates by using atomic layer deposition (ALD) were annealed at the temperatures ranging from 300 to 500 °C. The X-ray diffraction (XRD) results show that the annealed ZnO thin films are highly (0 0 2)-oriented, indicating a well ordered microstructure. The film surface examined by the atomic force microscopy (AFM), however, indicated that the roughness increases with increasing annealing temperature. The photoluminescence (PL) spectrum showed that the intensity of UV emission was strongest for films annealed at 500 °C. The mechanical properties of the resultant ZnO thin films investigated by nanoindentation reveal that the hardness decreases from 9.2 GPa to 7.2 GPa for films annealed at 300 °C and 500 °C, respectively. On the other hand, the Young's modulus for the former is 168.6 GPa as compared to a value of 139.5 GPa for the latter. Moreover, the relationship between the hardness and film grain size appear to follow closely with the Hall-Petch equation.     

Microstructural and surface property variations due to the amorphous region formed by thermal annealing in Al-doped ZnO thin films grown on n-Si (1 0 0) substrates

X-ray diffraction (XRD) patterns revealed that the as-grown and annealed Al-doped ZnO (AZO) films grown on the n-Si (1 0 0) substrates were polycrystalline. Transmission electron microscopy (TEM) images showed that bright-contrast regions existed in the grain boundary, and high-resolution TEM (HRTEM) images showed that the bright-contrast regions with an amorphous phase were embedded in the ZnO grains. While the surface roughness of the AZO film annealed at 800 °C became smoother, those of the AZO films annealed at 900 and 1000 °C became rougher. XRD patterns, TEM images, selected-area electron diffraction patterns, HRTEM images, and atomic force microscopy (AFM) images showed that the crystallinity in the AZO thin films grown on the n-Si (1 0 0) substrates was enhanced resulting from the release in the strain energy for the AZO thin films due to thermal annealing at 800 °C. XRD patterns and AFM images show that the crystallinity of the AZO thin films annealed at 1000 °C deteriorated due to the formation of the amorphous phase in the ZnO thin films.     

Formation of gold nanoparticles in heat-treated reactive co-sputtered Au-SiO2 thin films

In this work, formation of gold nanoparticles in radio frequency (RF) reactive magnetron co-sputtered Au-SiO₂ thin films post annealed at different temperatures in Ar + H₂ atmosphere has been investigated. Optical, surface topography, chemical state and crystalline properties of the prepared films were analyzed by using UV-visible spectrophotometry, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and X-ray diffractometry (XRD) techniques, respectively. Optical absorption spectrum of the Au-SiO₂ thin films annealed at 800 °C showed one surface plasmon resonance (SPR) absorption peak located at 520 nm relating to gold nanoparticles. According to XPS analysis, it was found that the gold nanoparticles had a tendency to accumulate on surface of the heat-treated films in the metallic state. AFM images showed that the nanoparticles were uniformly distributed on the film surface with grain size of about 30 nm. Using XRD analysis average crystalline size of the Au particles was estimated to about 20 nm.     

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.     

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.     

The effect of heat treatment on the physical properties of sol-gel derived ZnO thin films

Zinc oxide (ZnO) thin films were deposited on microscope glass substrates by sol-gel spin coating method. Zinc acetate (ZnAc) dehydrate was used as the starting salt material source. A homogeneous and stable solution was prepared by dissolving ZnAc in the solution of monoethanolamine (MEA). ZnO thin films were obtained after preheating the spin coated thin films at 250 °C for 5 min after each coating. The films, after the deposition of the eighth layer, were annealed in air at temperatures of 300 °C, 400 °C and 500 °C for 1 h. The effect of thermal annealing in air on the physical properties of the sol-gel derived ZnO thin films are studied. The powder and its thin film were characterized by X-ray diffractometer (XRD) method. XRD analysis revealed that the annealed ZnO thin films consist of single phase ZnO with wurtzite structure (JCPDS 36-1451) and show the c-axis grain orientation. Increasing annealing temperature increased the c-axis orientation and the crystallite size of the film. The annealed films are highly transparent with average transmission exceeding 80% in the visible range (400-700 nm). The measured optical band gap values of the ZnO thin films were between 3.26 eV and 3.28 eV, which were in the range of band gap values of intrinsic ZnO (3.2-3.3 eV). SEM analysis of annealed thin films has shown a completely different surface morphology behavior.     

Effects of post-annealing on structural, optical and electrical properties of Al-doped ZnO thin films

Aluminum-doped zinc oxide (AZO) films were deposited at 400 °C by radio-frequency magnetron sputtering using a compound AZO target. The effects of annealing atmospheres as well as hydrogen annealing temperatures on the structural, optical and electrical properties of the AZO films were investigated. It was found that the electrical resistivity varied depending on the atmospheres while annealing in air, nitrogen and hydrogen at 300 °C, respectively. Comparing with that for the un-annealed films, the resistivity of the films annealed in hydrogen decreased from 9.8 × 10⁻⁴ Ω cm to 3.5 × 10⁻⁴ Ω cm, while that of the films annealed in air and nitrogen increased. The variations in electrical properties are ascribed to both the changes in the concentration of oxygen vacancies and adsorbed oxygen at the grain boundaries. These results were clarified by the comparatively XPS analyzing about the states of oxygen on the surface of the AZO films. There was great increase in electrical resistivity due to the damage of the surfaces, when AZO films were annealed in hydrogen with a temperature higher than 500 °C, but high average optical transmittance of 80-90% in the range of 390-1100 nm were still obtained.     

Structural characterization of supported nanocrystalline ZnO thin films prepared by dip-coating

Nanocrystalline ZnO thin films prepared by the sol-gel dip-coating technique were characterized by grazing incidence X-ray diffraction (GIXD), atomic force microscopy (AFM), X-ray reflectivity (XR) and grazing incidence small-angle X-ray scattering (GISAXS). The structures of several thin films subjected to (i) isochronous annealing at 350, 450 and 550 °C, and (ii) isothermal annealing at 450 °C during different time periods, were characterized. The studied thin films are composed of ZnO nanocrystals as revealed by analysing several GIXD patterns, from which their average sizes were determined. Thin film thickness and roughness were determined from quantitative analyses of AFM images and XR patterns. The analysis of XR patterns also yielded the average density of the studied films. Our GISAXS study indicates that the studied ZnO thin films contain nanopores with an ellipsoidal shape, and flattened along the direction normal to the substrate surface. The thin film annealed at the highest temperature, T = 550 °C, exhibits higher density and lower thickness and nanoporosity volume fraction, than those annealed at 350 and 450 °C. These results indicate that thermal annealing at the highest temperature (550 °C) induces a noticeable compaction effect on the structure of the studied thin films.     

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.     

Oxidation of a cesium-covered Ni (1 1 0) surface studied by metastable-induced electron spectroscopy

An initial stage of oxidation of a cesium-covered Ni (1 1 0) surface has been studied by metastable-induced electron spectroscopy (MIES) and low-energy electron diffraction (LEED). The MIES brought spectra with Cs 6s induced peak (P_6s), Cs 5p (P_5p), O 2p induced peak (P_ox) and a structure related to the substrate Ni 3d states (P_3d). The work function change Δφ showed an oscillatory behavior in the progress of surface oxidation. The process is divided into three stages: (i) at low O₂ exposures, Δφ > 0 with unchanging P_5p and P_6s; (ii) at moderate exposures, Δφ < 0 with a drastic decrease in the P_6s intensity; (iii) at higher exposures, Δφ > 0 with shifts of peaks P_5p and P_ox to higher energies, together with an appearance of peak P_3d. A three-step model of initial oxidation of alkali-covered Ni (1 1 0) surfaces is presented.     

Effect of annealing on thermal stability and morphology of pulsed laser deposited Ir thin films

Iridium (Ir) thin films, deposited on Si (1 0 0) substrate by pulsed laser deposition (PLD) technique using Ir target in a vacuum atmosphere, were annealed in air ambient and the thermal stability was investigated. The crystal structure and surface morphology of Ir thin films before and after being annealed were studied by X-ray diffraction, Raman scattering, scanning electron microscope, and atomic force microscopy. The results showed that single-phase Ir thin films with (1 1 1) preferred orientation could be deposited on Si (1 0 0) substrate at 300 °C and it remained stable below 600 °C, which showed a promising bottom electrode of integrated ferroelectric capacitors. Ir thin films got oxidized to IrO₂ at temperatures from 650 to 800 °C.     

Microstructural and surface characterization of thin gold films on n-Ge (1 1 1)

Thin gold films were fabricated by vacuum resistive deposition on the n-Ge (1 1 1) wafers. The films were annealed between 300 and 600 °C. These resulting thin films were then characterised using scanning electron microscopy (field emission and back-scattering modes), Rutherford back scattering spectroscopy and time of flight secondary ion mass spectroscopy (TOF-SIMS). For temperatures below the eutectic temperature the distribution of both the gold and the germanium on the surface are uniform. Above the eutectic temperature, the formation of gold rich islands on the surface of the Germanium were observed. These changes in the microstructure were found to correspond to changes in the electrical characteristics of the diodes.     

Influence of annealing temperature on the properties of ZnO thin films deposited by thermal evaporation

ZnO thin films were deposited by thermal evaporation of a ZnO powder. The as-deposited films are dark brown, rich zinc and present a low transmittance. Then, these films were annealed in air atmosphere at different temperatures between 100 and 400 °C. Their microstructure and composition were studied using XRD and RBS measurements respectively. By increasing the temperature, it was found that film oxidation starts at 250 °C. XRD peaks related to ZnO appear and peaks related to Zn decrease. At 300 °C, zinc was totally oxidised and the films became totally transparent. The electrical conductivity measurement that were carried out in function of the annealing temperature showed the transition from highly conductive Zn thin film to a lower conductive ZnO thin film. The optical gap (E_g) was deduced from the UV-vis transmittance, and its variation was linked to the formation of ZnO.     

Effect of deposition temperature on the microstructure and surface morphology of c-axis oriented AlN films deposited on sapphire substrate by RF reactive magnetron sputtering

In this paper, c-axis oriented AlN films were prepared on sapphire substrate by RF reactive magnetron sputtering at various deposition temperatures (30–700 °C). The influences of deposition temperature on the chemical composition, crystalline structure and surface morphology of the AlN films were systematically investigated. The as-deposited films were characterized by X-ray photoelectron spectroscopy (XPS), two-dimensional X-ray diffraction (2D-XRD) and atomic force microscopy (AFM). The experimental results show that it can be successfully grown for high-purity and near-stoichiometric (Al/N = 1.12:1) AlN films except for the segregation of a few oxygen impurities exist in the form of Al–O bonding. The chemical composition of as-deposited films is almost independent of substrate temperature in the range of 30–700 °C. However, the crystalline structure and surface morphology of the deposited AlN films are strongly influenced by the deposition temperature. The optimum deposition temperature is 300 °C, giving a good compromise between crystalline structure and surface morphology to grow AlN films.