Characteristics of the precursors and their thermal decomposition during the preparation of LiNbO3 thin films by the Pechini method

Lithium niobate thin films have been deposited on Pt/Ti/SiO₂/Si(100) substrates by Pechini method. Characterization of the initial precursor solutions containing citric acid (CA), niobium and lithium ions has been performed by Fourier transform infrared spectroscopy, Raman spectroscopy and carbon nuclear magnetic resonance spectroscopy. The results indicate that citric acid coordinate to niobium ions to form a niobium-CA complex through one terminal carboxyl group, the hydroxyl group and the central carboxyl group as a tridentate ligand. The thermal decomposition of the Li-Nb precursors gel powder has been studied and the results show that LiNbO₃ phase is formed directly from the thermal decomposition of the precursor gel. By heat-treatment at 600 °C for 2 h, polycrystalline LiNbO₃ thin films with smooth and crack-free surface could be achieved.     

Titanium oxide films produced on commercially pure titanium by anodic oxidation with different voltages

Titanium oxide films produced on commercially pure Ti by anodic oxidation with different voltages were analyzed. Anodic oxidation was carried out at room temperature using 1.4 M H₃PO₄ electrolyte and a platinum counter-electrode, in potentiostatic mode under the following conditions: 50 V, 100 V, 150 V, 200 V and 250 V. It was observed that porous titanium layers were formed at all voltage values but morphological differences were observed. Initially, the film was thin but with increasing voltage it broke down locally and porous regions became evident due to the dielectric breakdown. The porosity and the pore size increased with the increasing voltage. The surface morphology in samples formed with 200 V had substantially different porous structures than those formed with other voltage values. The anodic film surface displayed pores and craters formed on the relatively flat ground oxide surface. AFM images showed that higher voltages produced thicker titanium oxide films.     

Hardness of sputter deposited nanocrystalline Ni3Al thin films

Nanocrystalline thin films of nominal composition Ni-25 at.% Al have been sputter deposited from a target of the intermetallic compound Ni₃Al using different sputtering conditions. Increase in the pressure of sputtering gas resulted in a substantial reduction in the grain size of these nanocrystalline films and a consequent enhancement in their hardness. While films deposited onto heated substrates exhibited larger grain sizes as compared to those deposited on unheated substrates at the same sputtering pressure, the hardness of the former films was substantially higher. The reason for this enhanced hardness is the long-range chemical ordering in films deposited on heated substrates and the formation of L1₂-Ni₃Al, the thermodynamically stable phase for this composition.     

Ion beam deposition of α-Ta films by nitrogen addition and improvement of diffusion barrier property

Ta thin films were deposited on Si (100) substrates by an ion beam deposition method at various substrate bias voltages under Ar + N₂ atmosphere with different pressure ratios of Ar and N₂. The effects of nitrogen pressure in the plasma gas and the substrate bias voltage on the surface morphology, crystalline microstructure, electrical resistivity and diffusion barrier property were investigated. It was found that the fraction of a metastable β-phase in the Ta film deposited at the substrate bias voltage of − 50 V films decreased by adding nitrogen gas, while the α-Ta phase became dominant. As a result, the Ta films deposited at the substrate bias voltage of − 50 V under Ar (9 Pa) + N₂ (3 Pa) atmosphere showed a dominant α-phase with good surface morphology, low resistivity, and superior thermal stability as a diffusion barrier.     

Transmission electron microscopy studies of nanostructured TiO2 films on various substrates

A chemical vapour deposition (CVD) synthetic route to the production of nanocrystalline titanium dioxide has been carefully investigated on various substrates. CVD was performed at a relatively low temperature of 320 °C on KCl crystal, Al foil, KBr pellet and freshly sliced MICA substrates. The influence of substrate material on film formation was studied in order to find a titanium dioxide film with good intercalation properties for an electrode in a dye-sensitized solar cell. Intercalation properties depend on average grain sizes and porosity in nanophased materials. These films were thoroughly characterized with respect to their surface morphology, crystal structure and the phase composition. Transmission electron microscopy (TEM) accompanied by selected area electron diffraction (SAED) was employed for structural characterization of TiO₂ films. The studies showed that films deposited on KCl crystal, KBr pellet and MICA are solely composed of an anatase phase whereas in the film deposited onto Al foil, the brookite phase of TiO₂ is also present. The structural parameters of anatase were determined using the Rietveld refinement of electron diffraction data. By comparison of anatase lattice parameters with their corresponding bulk values, the significant deviation in values of lattice parameters a and c in anatase phase was observed and attributed to the thin-film features. The average grain size and the grain size distribution obtained by TEM were compared for TiO₂ films deposited on different substrates.     

Deposition of superconducting niobium films for RF cavities by means of UHV cathodic Arc

The Ultra-High-Vacuum (UHV) arc technology was proposed as an alternative for depositing thin superconducting films of pure niobium on the internal surfaces of RF cavities for particle accelerators. The paper describes status of research on the deposition of such films for the RF accelerating cavities. UHV arc-based devices, equipped with planar- or cylindrical-cathodes, are described. The main results of experiments and some characteristics of the arc-deposited thin Nb-films, as well as results obtained recently with the formation of such films, are also presented. The critical temperature T_c of the deposited Nb-films appeared to be very close to that of pure bulk niobium (T_c=9.26 K) and the transition to the superconducting state was very narrow. The deposited Nb-films had higher residual resistivity ratio (RRR) values (up to 80) and larger grains sizes, as compared with those sputtered at the same temperature. The paper also presents recent results of the Cu-cavity coating by means of an UHV linear (cylindrical) arc, operated at IPJ in Poland.     

Intrinsic stress of magnetron-sputtered niobium films

The stresses in niobium films were studied and the following preliminary results were obtained. (1) Niobium films can be prepared in any stress state (tensile, stress free or compressive) by varying the argon sputtering pressure. (2) As the bias voltage increases, more argon is incorporated into the film; both T_c and R/R₀ decrease; and the stress becomes more compressive and seems to saturate at about 1.5 × 10¹⁰ dyn cm^?2 at higher bias voltages (at an argon sputtering pressure of 1.9 Pa). (3) The lattice parameters show a close relation to the film stresses. (4) Lowering the sputtering rate results in a higher argon content in the bias-sputtered films. (5) The as-deposited film surface is smoother when deposited at lower pressures; the film has a columnar structure and intercolumnar gaps at higher pressures. (6) The film prepared at a higher bias voltage has a smoother as-deposited surface and a much smaller column size.From this study of the behavior of the stresses in niobium films, it appears that the stress is determined mainly by the microstructure and the energetic particle bombardment. Energetic particle bombardment may promote compressive stress by the incorporation of argon, by the formation of a more dense microstructure and by a “shot-peening” action.     

Nanoscale characterization of anodic oxide films on Ti-6Al-4V alloy

The paper analyses, at nanoscale levels, the chemical composition and mechanical properties of the anodic oxide films formed on Ti-6Al-4V alloy by galvanostatic polarization at maximum final voltages of 12-100 V. For the investigations Auger Electron Spectroscopy, Photoelectron Spectroscopy and nanoindentation measurements have been used. The results have shown that anodizing the Ti-6Al-4V alloy produces an oxide film whose thickness depends on the final voltage. The chemical composition is not significantly dependent on the thickness, the film consists of TiO₂ and Al₂O₃. However, the best insulating properties of the films, determined from the growth parameter nm/V, are achieved with a final voltage between 30 and 65 V. Nanohardness and Young's modulus measurements have shown that the anodic films formed by different voltages exhibit similar mechanical properties which is consistent with the results of the surface analysis.     

Structures, varistor properties, and electrical stability of ZnO thin films

In this letter, we report the structures, varistor properties, and electrical stability of ZnO thin films deposited by the gas discharge activated reaction evaporation (GDARE) technique. The X-ray diffraction (XRD) and atomic force microscopy (AFM) measurements showed that the thin films thus prepared have polycrystalline structures with the preferred orientation along the (002) plane whose surface consists of ZnO aggregates with sizes of 50-200 nm. The ZnO thin films deposited by GDARE and annealed at 250 °C for 2 h have strong nonlinear varistor-type I-V characteristics. The nonlinear coefficient (α) of a single-layered ZnO thin film sample was 33 and that of a triple-layered sample obtained by the many-time deposition was 62. The varistor voltages (V_1mA) of the two samples are found rather close each other. Under a DC bias of 0.75 V_1mA and a temperature of 150 °C these thin films exhibit good electrical stability with a degradation rate coefficient K_T of 0.05 mA/h^1/2.     

Glancing angle deposited titania films for dye-sensitized solar cells

A series of sculptured porous nano-columnar titanium oxide films were prepared by glancing angle deposition (GLAD) method using an electron-beam evaporation system. The films were deposited on ITO glasses at various incident angles from 53° to 86°and used as photoanode in a dye-sensitized solar cell (DSSC). The as-deposited TiO₂ films are comprised of helical nano-columns and assembled in an orderly manner with gaps or pores in between. The porous nanostructured films provide a synergetic effect of high surface area, effective route for electron transfer, tight interfaces, and enhanced light trapping, which are all beneficial for higher cell efficiency. The DSSCs incorporated with the GLAD films of 4 μm thick exhibited a high fill factor (FF) up to 0.77. The TiO₂ film deposited at an incident angle of 73° provides the largest internal surface area and the largest amount of dye absorption and results in the highest light conversion efficiency of 2.78%.     

Characterization and properties of CrN films deposited by ion-source-enhanced middle frequency magnetron sputtering

CrN films with deposition rates of 130-180 nm/min were deposited on Si (111) and carbamide alloy substrates by an ion-source-enhanced middle frequency magnetron sputtering system. Increasing of ion source voltages promoted the growth of CrN films with preferred orientation of (200). The deposited CrN films are composed of nanocrystalline particles with sizes of ∼20 nm embedded in polycrystalline matrix. The hardness of the CrN films increases from 1300 Kg/mm² without ion source bombardment to 2400 Kg/mm² with ion source voltages of 1000 V. Origins for the increasing of hardness can be attributed to dislocation strengthening and densification effects.     

Influence of fabrication parameters on crystallization,microstructure, and surface composition of NbN thin films deposited by rf magnetron sputtering

In this work NbN thin films have been grown by magnetron rf sputtering of a δ-NbN (99.99%) target. In particular, the influence of certain fabrication parameters (substrate temperature, power supplied to the target or additional N₂ flux in the preparation chamber) on the crystallization, microstructure, and surface composition of the deposited films have been studied. The films have been characterized by X-ray diffraction (XRD) at grazing angle in the θ–2θ configuration, scanning electron microscopy (SEM), wavelength dispersive spectrometry (WDS), and X-ray photoelectron spectroscopy (XPS). XRD results show that films grown at a substrate temperature of 573 K and a power supply applied to the target of 300 W present the same crystalline structure of the target while films grown at these temperature and power supply conditions plus the additional presence of N₂ during fabrication, grow highly textured along the plane (200). SEM results indicate that the films present columnar growth and a high homogeneity. WDS analysis shows that films grown at 573 K and 300 W are stoichiometric. XPS shows a complex surface composition of the films most external 5 nm, indicating the presence of niobium nitride (NbN _x ), niobium oxy-nitride (NbN _x O _y ), and niobium oxide (Nb₂O₅).     

The structural and electrical properties of Zn-Sn-O buffer layers and their effect on CdTe solar cell performance

Thin films of zinc-tin-oxide (ZTO) have been deposited on SnO₂:F coated glass substrates by co-sputtering of SnO₂ and ZnO. The deposition conditions for ZTO were controlled in order to vary film stoichiometry. The electro-optical and structural properties of ZTO have been studied as a function of their stoichiometric ratio and post-deposition annealing conditions. The same films were subsequently utilized as part of a bi-layer transparent front contact for the fabrication of CdTe solar cells: glass/SnO₂:F/ZTO. The performance of these devices suggested that the ZTO deposition and cell processing conditions can be optimized for enhanced device performance in particular for devices with thin CdS. Specifically, high blue spectral response (> 70% at 450 nm), accompanied by high open-circuit voltages (830 mV), and fill factors (70⁺%) have been demonstrated. Best solar cell performance was obtained for multi-phase ZTO films deposited at substrate temperatures of 400°C and a Zn/Sn ratio of 2.0, and which contained the binary phase of ZnO₂.     

Nanocrystalline SnO2 and Au:SnO2 thin films prepared by direct current magnetron reactive sputtering

Nanocrystalline pure and gold doped SnO₂(Au:SnO₂) films were prepared on unheated glass substrates by dc magnetron reactive sputtering and, subsequently, the as deposited films were annealed in air. The films structure, surface morphology, photoluminescence, electrical and optical properties were investigated. After annealing the as deposited SnO₂ films, crystallinity increased and the surface roughness decreased. The intensity of PL peaks increases sharply with the annealing temperature. The optical transmittance of the films was around 89% after annealing the as deposited SnO₂ films at 450 °C. The as deposited Au:SnO₂ films show better crystallinity than the as deposited SnO₂ films, the average grain size was around 4.4 nm. The emission peaks of Au:SnO₂ films are slightly blue shifted as compare to undoped SnO₂ films. The Au:SnO₂ films show the lowest electrical resistivity of 0.001 Ωcm with optical transmittance of 76%, after annealing at 450 °C.     

Electrical properties of r.f. magnetron sputtered BaxSr1−xTiO3 films on multi-layered bottom electrodes for high-density memory application

Ba_xSr_1–xTiO₃ (BST) thin films have been deposited by r.f. magnetron sputtering on silicon and platinum-coated silicon substrates with different buffer and barrier layers. Electrical properties of BST films have been evaluated using both metal–insulator–semiconductor (MIS) and metal–insulator–metal (MIM) structures. MIS capacitor C–V and G–V characteristics have been utilized to determine the fixed charge density, interface trap density and the trap distribution in the silicon bandgap. BST films deposited on Si/SiO₂/SiN/Pt and Si/SiO₂/Ti/TiN/Pt multilayer bottom electrodes have been used for the fabrication of MIM capacitors. The role of bottom electrode, processing temperature and Ba to Sr ratio on the electrical properties of Ba_xSr_1–xTiO₃ films have been investigated. Current–voltage behavior has indicated an ohmic nature at lower voltages and Poole–Frenkel conduction at higher voltages. Deposited films have shown an excellent time-dependent dielectric breakdown under constant-current stressing.     

The effect of composition on surface morphology, formation mechanism and pinhole generation of cosputtered ytterbium silicide

The surface morphology including pinhole and silicide formation mechanism of codeposited ytterbium silicide films are investigated with various compositions of Yb and Si. Film properties depend on the growth mode of the deposited films. At Si compositions more than half of the stable phase of ytterbium silicide, films have a rough surface with islands of ytterbium silicide formed by the Stranski-Krastanov and Volmer-Weber growth mode. At Si composition below half of the stoichiometic value, films grow in a layer by layer, Frank-van der Merwe mode, with a smooth surface. The transition of the formation mode is due to a trade-off in the dominance of the reaction between the internal atoms in the deposited films or between the deposited films and the substrates. A Si composition of 0.59 provides the smoothest surface with roughness of 1.13 nm in root mean square value and no observed pinholes. Ytterbium silicide films are deposited with a 5% composition tolerance by cosputtering and forming at 450 °C in a conventional furnace.     

Pb(Zr0.52Ti0.48)O3/TiNi multilayered heterostructures on Si substrates for smart systems

Ferroelectric/shape memory alloy thin film multilayered heterostructures possess both sensing and actuating functions and are considered to be smart. In this article, Pb(Zr_0.52Ti_0.48)O₃ (PZT) ferroelectric thin films and Ti-riched TiNi shape memory alloy thin films have been deposited on Si and SiO₂/Si substrates in the 400-600 °C temperature range by pulsed laser deposition technique. Deposition processing, microstructure and surface morphology of these films are described. The TiNi films deposited at 500 °C had an austenitic B2 structure with preferred (110) orientation. The surfaces of the films were very smooth with the root-mean-square roughness on a unit cell level. The structure of the TiNi films had a significant influence on that of the subsequently deposited PZT films. The single B2 austenite phase of the TiNi favored the growth of perovskite PZT films. The PZT/TiNi heterostructures with the PZT and TiNi films respectively deposited at 600 and 500 °C exhibited a polarization-electric field hysteresis behavior with a leakage current of about 2 × 10^− 6 A/cm².     

Structural and optical properties of nanocrystalline WO<Subscript>3</Subscript> thin films

The nanocrystalline WO₃ thin films were deposited by r.f. magnetron sputtering on quartz and p- type Si (100) substrates at a constant power of 25 W and at three different sputtering pressures (0.05, 0.01 and 0.5 mbar) and post annealed at different temperatures. The deposited films were characterized by XRD, UV–VIS spectrophotometry, ellipsometry and atomic force microscopy (AFM). The structural studies from XRD spectra reveals that the films deposited at 0.05 mbar and post annealed at 573 and 673 K have the predominant orthorhombic phase, whereas at 0.1 mbar and 573, 673 K triclinic phase is predominant. When sputtering pressure is at 0.5 mbar the predominant phase is monoclinic when annealed at 473 K and triclinic at 673 K. The optical energy gap is influenced significantly by sputtering pressure and post annealing temperatures. The optical energy gap of the films deposited at higher sputtering pressures and post annealed at lower temperatures is high due to smaller crystallite sizes. The thickness of all deposited films at different conditions is around 200 nm.     

Electrical behaviour,characteristics and properties of anodic aluminium oxide films coloured by nickel electrodeposition

Porous anodic films on 1050 aluminium substrate were coloured by AC electrodeposition of nickel. Several experiments were performed at different deposition voltages and nickel concentrations in the electrolyte in order to correlate the applied electrical power to the electrical behaviour, as well as the characteristics and properties of the coatings. The content of nickel inside the coatings reached 1.67 g/m², depending on the experimental conditions. According to the applied AC voltage in comparison with the threshold voltage U _t, the coating either acted only as a capacitor when U < U _t and, when U > U _t, the behaviour during the anodic and cathodic parts of the power sine wave was different. In particular, due to the semi-conducting characteristics of the barrier layer, additional oxidation of the aluminium substrate occurred during the anodic part of the electrical signal, whilst metal deposition (and solvent reduction) occurred during the cathodic part; these mechanisms correspond to the blocked and pass directions of the barrier layer/electrolyte junction, respectively.     

Thermal degradation of anodic niobia on niobium and oxygen-containing niobium

Thermal treatment of anodized niobium and oxygen-containing niobium has been carried out to elucidate the thermal degradation mechanism of niobium capacitors and to clarify the influence of oxygen dissolved in niobium on thermal degradation. The capacitance and leakage current of the anodized specimens increase with thermal treatment above 423 K in air, although the oxygen content in the substrate has no significant effect up to 523 K. At increased temperatures, the changes in capacitance and leakage current are suppressed with increasing oxygen content. The anodic film formed on the Nb-50 at.% O substrate thickens significantly during thermal treatment at 623 K in air, while only a slight reduction of the thickness is evident for those on the niobium and Nb-20 at.% O substrates. In contrast, vacuum thermal treatment at 623 K causes thinning of the anodic film on niobium, with evidently no change in the film thickness on the Nb-50 at.% O substrate. These are interpreted in terms of oxygen diffusion from the anodic film to the substrate as well as thermal oxide growth.