AlN:Cr thin films synthesized by pulsed laser deposition: Studies by X-ray diffraction and spectroscopic ellipsometry

The structure and optical properties of AlN thin films doped with Cr atoms were studied by X-ray diffractometry, Fourier transform infrared spectroscopy and spectroscopic ellipsometry analyses. The films were synthesized by pulsed laser deposition from an AlN:Cr (10% Cr) target onto Si(1 0 0) wafers in vacuum at residual pressure of 10⁻³ Pa or in nitrogen at a dynamic pressure of 0.1 Pa. The study of the XRD patterns revealed that both phases co-existed in the synthesized films and that the amorphous one was prevalent. Two different amorphous matrices, i.e. two types of chemical bond arrangements, were found in films deposited at 0.1 Pa N₂. By difference, deposition in vacuum resulted in the coexistence of hexagonal and cubic crystallites embedded into an amorphous matrix. The introduction of Cr atoms into the AlN lattice causes a broadening of the IR spectrum along with the shift toward higher wavenumbers of the characteristic Al-N bands at 2351 cm⁻¹ and 665 cm⁻¹, respectively. This was related to the generation of a compressive stress inside films. In comparison to the optical constants of pure AlN films, the synthesized AlN:Cr films exhibited a smaller refractive index and showed a weak absorption throughout the 300-800 nm spectral region, characteristic to amorphous AlN structure.     

PLD of Fe3O4 thin films: Influence of background gas on surface morphology and magnetic properties

Ablation of Fe₃O₄ targets has been performed using a pulsed UV laser (KrF, λ = 248 nm, 30 ns pulse duration) onto Si(100) substrates, in reactive atmospheres of O₂ and/or Ar, with different oxygen partial pressures. The as-deposited films were characterised by atomic force microscopy (AFM), X-ray diffraction (XRD), conversion electron Mössbauer spectroscopy (CEMS) and extraction magnetometry, in order to optimise the deposition conditions in the low temperature range. The results show that a background mixture of oxygen and argon improves the Fe:O ratio in the films as long as the oxygen partial pressure is maintained in the 10⁻² Pa range. Thin films of almost stoichiometric single phase polycrystalline magnetite, Fe_2.99O₄, have been obtained at 483 K and working pressure of 7.8 × 10⁻² Pa, with a high-field magnetization of ∼490 emu/cm³ and Verwey transition temperature of 112 K, close to the values reported in the literature for bulk magnetite.     

Nd:YAG laser synthesis of nanostructural V2O5 from vanadium oxide sols: Morphological and structural characterizations

Vanadium oxide thin films were prepared by sol-gel method, then subjected to Nd:YAG laser (CW, 1064 nm) radiation. The characteristics of the films were changed by varying the intensity of the laser radiation. The nanocrystalline films were characterized by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM) and scanning electron microscopy (SEM). XRD revealed that above 102 W/cm² the original xerogel structure disappears and above 129 W/cm² the films become totally polycrystalline with an orthorhombic structure. From TEM observations, we can see that due to laser radiation, the originally fibrillar-like particles disappear and irregular shaped, layer structured V₂O₅ particles are created. From XPS spectra we can conclude that due to laser radiation the O/V ratio increased with higher intensities.     

Structural and optical properties of Er, Yb co-doped Y2O3 thin films

Thin Er³⁺, Yb³⁺ co-doped Y₂O₃ films were grown on (1 0 0) YAG substrates by pulsed laser deposition. Ceramic targets having different active ion concentration were used for ablation. The influence of the rare-earth content and oxygen pressure applied during the deposition on the structural, morphological and optical properties of the films were investigated. The films deposited at the lower pressure, 1 Pa, and at 1/10 Er to Yb doping ratio are highly textured along the (1 1 1) direction of the Y₂O₃ cubic phase. In addition to the crystalline structure, these films possess smoother surface compared to those prepared at the higher pressure, 10 Pa. All other films are polycrystalline, consisting of cubic and monoclinic phases of Y₂O₃. The rougher surface of the films produced at the higher-pressure leads to higher scattering losses and different behavior of the reflectivity spectra. Optical anisotropy in the films of less than 0.004 was measured regardless of the monoclinic structure obtained. Waveguide losses of about 1 dB/cm at 633 nm were obtained for the films produced at the lower oxygen pressure.     

Pulsed Nd:YAG laser depositions of ITO and DLC films for OLED applications

Indium-tin oxide (ITO) films deposited on heated and non-heated glass substrates by a pulsed Nd:YAG laser at 355 nm and ∼2.5 J/cm² were used in the fabrication of simple organic light-emitting diodes (OLEDs), ITO/(PVK + Alq₃ + TPD)/Al. The ITO was deposited on heated glass substrates which possessed resistivity as low as ∼3 × 10⁻⁴ Ω cm, optical transmission as high as ∼92% and carrier concentration of about ∼5 × 10²⁰ cm⁻³, were comparable to the commercial ITO. Substrate heating transformed the ITO microstructure from amorphous to polycrystalline, as revealed by the XRD spectrum. While the polycrystalline ITO produced higher OLED brightness, it was still lower than that on the commercial ITO due to surface roughness. A DLC layer of ∼1.5 nm deposited on this ITO at laser fluence of >12.5 J/cm² improved its device brightness by suppressing the surface roughness effect.     

XRD and XPS analysis of laser treated vanadium oxide thin films

In this work, we present X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD) analysis of laser treated vanadium oxide sols. The films were also observed by transmission electron microscopy (TEM) and scanning electron microscopy (SEM) to reveal how the original xerogel structure changes into irregular shaped, layer structured V₂O₅ due to the laser radiation. XRD revealed that above 102 W/cm² the original xerogel structure disappears and above 129 W/cm² the films become totally polycrystalline with an orthorhombic structure. XPS spectra showed O/V ratio increment by using higher laser intensities.     

Morphological and structural characterizations of CrSi2 nanometric films deposited by laser ablation

The structure and morphology of chromium disilicide (CrSi₂) nanometric films grown on 〈1 0 0〉 silicon substrates both at room temperature (RT) and at 740 K by pulsed laser ablation are reported. A pure CrSi₂ crystal target was ablated with a KrF excimer laser in vacuum (∼3 × 10⁻⁵ Pa). Morphological and structural properties of the deposited films were investigated using Rutherford backscattering spectrometry (RBS), grazing incidence X-ray diffraction (GID), X-ray reflectivity (XRR), scanning (SEM) and transmission electron microscopy (TEM). From RBS analysis, the films’ thickness resulted of ∼40 nm. This value is in agreement with the value obtained from XRR and TEM analysis (∼42 and ∼38 nm, respectively). The films’ composition, as inferred from Rutherford Universal Manipulation Program simulation of experimental spectra, is close to stoichiometric CrSi₂. GID analysis showed that the film deposited at 740 K is composed only by the CrSi₂ phase. The RT deposited sample is amorphous, while GID and TEM analyses evidenced that the film deposited at 740 K is poorly crystallised. The RT deposited film exhibited a metallic behaviour, while that one deposited at 740 K showed a semiconductor behaviour down to 227 K.     

Magnetoresistance of magnetite thin films grown by pulsed laser deposition on GaAs(1 0 0) and Al2O3(0 0 0 1)

Magnetotransport properties of magnetite thin films deposited on gallium arsenide and sapphire substrates at growth temperatures between 473 and 673 K are presented. The films were grown by UV pulsed laser ablation in reactive atmospheres of O₂ and Ar, at working pressure of 8 × 10⁻² Pa. Film stoichiometry was determined in the range from Fe_2.95O₄ to Fe_2.97O₄. Randomly oriented polycrystalline thin films were grown on GaAs(1 0 0) while for the Al₂O₃(0 0 0 1) substrates the films developed a (1 1 1) preferred orientation. Interfacial Fe³⁺ diffusion was found for both substrates affecting the magnetic behaviour. The temperature dependence of the resistance and magnetoresistance of the films were measured for fields up to 6 T. Negative magnetoresistance values of ∼5% at room temperature and ∼10% at 90 K were obtained for the as-deposited magnetite films either on GaAs(1 0 0) or Al₂O₃(0 0 0 1).     

Room temperature growth and properties of ZnO films by pulsed laser deposition

ZnO thin films were prepared by pulsed laser deposition at room temperature on glass substrates with oxygen pressures of 10-30 Pa. The structural, electrical, and optical properties of ZnO films were studied in detail. ZnO films had an acceptable crystal quality with high c-axis orientation and smooth surface. The resistivity was in the 10² Ω cm order for ZnO films, with the electron concentration of 10¹⁶-10¹⁷ cm⁻³. All the films showed a high visible transmittance ∼90% and a high UV absorption about 90-100%. The UV emission ∼390 nm was observed in the photoluminescence spectra. The oxygen pressures in the 10-30 Pa range were suitable for room temperature growth of high-quality ZnO films.     

Influence of the deposition pressure on the properties of transparent conducting zirconium-doped zinc oxide films prepared by RF magnetron sputtering

Transparent and conducting zirconium-doped zinc oxide films with high transparency and relatively low resistivity have been successfully prepared by RF magnetron sputtering at room temperature. The deposition pressure was varied from 0.6 to 2.5 Pa. A transformation from a relatively compact structure to individual grains was observed with the increase of deposition pressure. As the deposition pressure increases, the resistivity increases sharply due to both, the decrease of hall mobility and carrier concentration. The lowest resistivity achieved was 2.07 × 10⁻³ Ω cm at a deposition pressure of 0.6 Pa with a hall mobility of 16 cm² V⁻¹ s⁻¹ and a carrier concentration of 1.95 × 10²⁰ cm⁻³. The films are polycrystalline with a hexagonal structure and a preferred orientation along the c-axis. All the films present a high transmittance of above 90% in the visible range. The optical band gap decreases from 3.35 to 3.20 eV as the deposition pressure increases from 0.6 to 2.5 Pa.     

Formation of TiN-Ir particle films using pulsed-laser deposition and their electrolytic properties in producing hypochlorous acid

Using sintered TiN and TiN-Ir (Ir contents: 5.9-14.2 at.%) targets, pulsed-laser deposition (PLD) was carried out to produce thin films composed of nanoparticles and particulates in the presence of nitrogen gas. The size (2-100 nm) of the produced crystalline TiN nanoparticles increased as nitrogen pressure was increased in the range from 1.33 to 1.33 × 10² Pa. At a pressure of 1.33 × 10³ Pa, amorphous TiN nanoparticles combined in the form of chains. Large Ir particulates with diameters of up to 2 μm were particularly prominent in TiN-Ir films. Size distributions of the Ir particulates were dependent on ablation laser wavelength; that is, the diameter decreased at laser wavelength shortened. The TiN-Ir films with different Ir contents and morphologies on Ti substrates were evaluated as electrolysis electrodes for water disinfection. The highest current efficiency was 0.45%, which is comparable to that of conventional Ti-Pt electrodes, for a chloride-ion concentration of 9 mg dm⁻³.     

Electrical characteristics of insulating aluminum nitride MIS nanostructures

Capacitance-voltage measurements of high quality PECVD and MBE grown aluminum nitride (AlN) thin films have been performed. The prepared films have shown polycrystalline (0 0 2)-preferential orientation, and were deposited on p-type Si (1 0 0) substrates with Pt forming the metal gate in a metal-insulator-semiconductor (MIS) configuration. The structure, crystallinity, texture and insulating properties have been found to depend on film thickness and were substantially influenced by the increase of the thickness. C-V measurements of the epitaxial and PECVD films were carried out and their insulating characteristics with increasing thickness (200-1000 nm) were investigated. The epitaxial films exhibited no hysteresis in capacitance behaviour, owing to better crystalline quality over the PECVD grown ones. Capacitance curves versus bias voltage have also been acquired at different temperatures; 10 K, 30 K and 50 K for deposited polycrystalline AlN films of (0 0 2) orientation. We have found that the defects trapped in the Pt/AlN/Si structure played a key role in dominating the overall behaviour of the C-V measurement curves. The trapped charges at the interface between the AlN insulating film and Si substrate caused the capacitance characteristics to shift to negative voltages, and the estimated charge density was of the order of 10¹⁰ and 10⁸ cm⁻² eV⁻¹ for the PECVD and epitaxial samples respectively. The I-V measurements referred to space-charge conduction mechanism, and the deduced leakage current was found to be of the order of 10⁻⁹ A at 200 nm film thickness.     

Low-temperature deposition of transparent conducting ZnO:Zr films on PET substrates by DC magnetron sputtering

Transparent conducting zirconium-doped zinc oxide (ZnO:Zr) films were firstly deposited on polyethylene terephthalate (PET) substrates with ZnO buffer layers by DC magnetron sputtering at room temperature. Dependence of physical properties of ZnO:Zr films on deposition pressure was systematically studied. All the deposited films were polycrystalline and (1 0 0) oriented. When deposition pressure increases from 1 to 2.5 Pa, the crystallinity of the films improves and the resistivity decreases. While deposition pressure increases from 2.5 to 3.5 Pa, the crystallinity of the films deteriorates and the resistivity increases. The lowest resistivity of 1.8 × 10⁻³ Ω cm was obtained for the films deposited at the optimum deposition pressure of 2.5 Pa. All the films present a high transmittance of above 86% in the wavelength range of the visible spectrum.     

Preparation of transparent conductive TiO2:Nb thin films by pulsed laser deposition

This study investigated the optical and electrical properties of Nb-doped TiO₂ thin films prepared by pulsed laser deposition (PLD). The PLD conditions were optimized to fabricate Nb-doped TiO₂ thin films with an improved electrical conductivity and crystalline structure. XRD analyses revealed that the deposition at room temperature in 0.92 Pa O₂ was suitable to produce anatase-type TiO₂. A Nb-doped TiO₂ thin film attained a resistivity as low as 6.7 × 10⁻⁴ Ω cm after annealing at 350 °C in vacuum (<10⁻⁵ Pa), thereby maintaining the transmittance as high as 60% in the UV-vis region.     

Evolution of surface morphology of NiO thin films under swift heavy ion irradiation

NiO nanoparticle thin films grown on Si substrates were irradiated by 107 MeV Ag⁸⁺ ions. The films were characterized by glancing angle X-ray diffraction and atomic force microscopy. Ag ion irradiation was found to influence the shape and size of the nanoparticles. The pristine NiO film consisted of uniform size (∼100 nm along major axis and ∼55 nm along minor axis) elliptical particles, which changed to also of uniform size (∼63 nm) circular shape particles on irradiation at a fluence of 3 × 10¹³ ions cm⁻². Comparison of XRD line width analysis and AFM data revealed that the particles in the pristine films are single crystalline, which turn to polycrystalline on irradiation with 107 MeV Ag ions.     

Effect of oxygen pressure on structure and properties of Bi1.5Zn1.0Nb1.5O7 pyrochlore thin films prepared by pulsed laser deposition

The Bi₂O₃-ZnO-Nb₂O₅ (BZN) cubic pyrochlore thin films were prepared on Pt/TiO₂/SiO₂/Si(1 0 0) substrates by using pulsed laser deposition process. The oxygen pressure was varied in the range of 5-50 Pa to investigate its effect on the structure and dielectric properties of BZN thin films. It is found that oxygen pressure during deposition plays an important role on structure and other properties of BZN films. The BZN films deposited at temperature of 650 °C and at O₂ pressure of 5 Pa have an amorphous BZN and Nb₂O₅ phases but exhibits a cubic pyrochlore structure with a preferential (2 2 2) orientation when the oxygen pressure increases to 10 Pa. Dielectric constant and loss tangent of the films deposited at 10 Pa are 185 and 0.0008 at 10 kHz, respectively. The dielectric tunability is about 10% at a dc bias field of 0.9 MV/cm.     

Atomic force microscopic characterization of films grown by inverse pulsed laser deposition

Carbon nitride films have been deposited by KrF excimer laser ablation of a rotating graphite target in 5 Pa nitrogen ambient in an inverse pulsed laser deposition configuration, where the backward motion of the ablated species is utilised for film growth on substrates lying in the target plane. Topometric AFM scans of the films, exhibiting elliptical thickness distribution, have been recorded along the axes of symmetry of the deposition area. High resolution AFM scans revealed the existence of disk-like, or somewhat elongated rice-like features of 5-10 nm average thickness and ∼100 nm largest dimension, densely packed over the whole, approximately 14 × 10 cm² deposition area. The RMS roughness of the film decreased from 9 nm near to the laser spot down to 2 nm in the outer regions. Even the highest RMS value obtained for IPLD films was less than half of the typical, 25 nm roughness measured on simultaneously deposited PLD films.     

Electrical, structural, and optical properties of ITO thin films prepared at room temperature by pulsed laser deposition

Indium tin oxide (ITO) thin films were prepared by pulsed laser deposition (PLD) on glass substrate at room temperature. Structural, optical, and electrical properties of these films were analyzed in order to investigate its dependence on oxygen pressure, and rapid thermal annealing (RTA) temperature. High quality ITO films with a low resistivity of 3.3 × 10⁻⁴ Ω cm and a transparency above 90% were able to be formed at an oxygen pressure of 2.0 Pa and an RTA temperature of 400 °C. A four-point probe method, X-ray diffraction (XRD), atomic force microscopy (AFM), and UV-NIR grating spectrometer are used to investigate the properties of ITO films.     

Sputter deposition of high transparent TiO2−xNx/TiO2/ZnO layers on glass for development of photocatalytic self-cleaning application

In this study, TiO_2−xN_x/TiO₂ double layers thin film was deposited on ZnO (80 nm thickness)/soda-lime glass substrate by a dc reactive magnetron sputtering. The TiO₂ film was deposited under different total gas pressures of 1 Pa, 2 Pa, and 4 Pa with constant oxygen flow rate of 0.8 sccm. Then, the deposition was continued with various nitrogen flow rates of 0.4, 0.8, and 1.2 sccm in constant total gas pressure of 4 Pa. Post annealing was performed on as-deposited films at various annealing temperatures of 400, 500, and 600 °C in air atmosphere to achieve films crystallinity. The structure and morphology of deposited films were evaluated by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), and atomic force microscopy (AFM). The chemical composition of top layer doped by nitrogen was evaluated by X-ray photoelectron spectroscopy (XPS). Photocatalytic activity of samples was measured by degradation of Methylene Blue (MB) dye. The optical transmittance of the multilayer film was also measured using ultraviolet-visible light (UV-vis) spectrophotometer. The results showed that by nitrogen doping of a fraction (∼1/5) of TiO₂ film thickness, the optical transmittance of TiO_2−xN_x/TiO₂ film was compared with TiO₂ thin film. Deposited films showed also good photocatalytic and hydrophilicity activity at visible light.     

Influence of substrate crystallography on the room temperature synthesis of AlN thin films by reactive sputtering

A pulsed DC reactive ion beam sputtering system has been used to synthesize aluminium nitride (AlN) thin films at room temperature by reactive sputtering. After systematic study of the processing variables, high-quality polycrystalline films with preferred c-axis orientation have been grown successfully on silicon and Au/Si substrates with an Al target under a N₂/(N₂ + Ar) gas flow ratio of 55%, 2 mTorr processing pressure and keeping the temperature of the substrate holder at room temperature. The crystalline quality of the AlN layer as well as the influence of the substrate crystallography on the AlN orientation has been characterized by high-resolution X-ray diffraction (HR-XRD). Best ω-FWHM (Full Width at Half Maximum) values of the (0 0 0 2) reflection rocking curve in the 1 μm thick AlN layers are 1.3°. Atomic Force Microscopy (AFM) measurements have been used to study the surface morphology of the AlN layer and Transmission Electron Microscopy (TEM) measurements to investigate the AlN/substrate interaction. AlN grew off-axis from the Si substrate but on-axis to the surface normal. When the AlN thin film is deposited on top of an Au layer, it grows along the [0 0 0 1] direction but showing a two-domain structure with two in-plane orientations rotated 30° between them.