Growth and characterization of non-polar ZnO thin films by pulsed laser deposition

Non-polar ZnO thin films were fabricated on r-plane sapphire substrates by pulsed laser deposition at various temperatures from 100 to 500 °C. The effects of the substrate temperature on structural, morphological and optical properties of the films were investigated. Based on the X-ray diffraction analysis, the ZnO thin films grown at 300, 400 and 500 °C exhibited the non-polar (a-plane) orientation and those deposited below 300 °C exhibited polar (c-plane) orientation. In the optical properties of non-polar ZnO films, there were two photoluminescence peaks detected. The peaks (near-band edge emission, blue emission) are due to electron transitions from band-to-band and shallow donor level to valence band, respectively.     

Synthesis of nanostructured SiC using the pulsed laser deposition technique

We report the new results on the direct synthesis of nanostructured silicon carbide (SiC) materials using the pulsed laser deposition technique. Scanning electron microscopy images revealed that SiC nanoholes, nanosprouts, nanowires, and nanoneedles were obtained. The crystallographic structure, chemical composition, and bond structure of the nanoscale SiC materials were investigated using X-ray diffraction, energy dispersive X-ray spectroscopy, X-ray photoelectron spectroscopy, and Raman scattering spectroscopy. The transverse optical mode and longitudinal optical mode in Raman spectra were found to become sharper as the substrate temperature was increased, while the material structure evolved from amorphous to crystalline.     

Structural investigations of InZnO films grown by pulsed laser deposition technique

Thin films of indium zinc oxide were grown from targets with In atomic concentration [In/(In + Zn)] of 2.8%, 4.3%, and 16.8%, respectively, by pulsed laser deposition technique (KrF laser, 10 Hz, 4 J/cm² fluence) on Si(001) and glass substrates that were heated at 500 °C. X-ray diffraction investigations showed that targets that had an atomic In concentration of 2.8% exhibited only the wurtzite-type ZnO lattice, while the targets that contained In concentrations of 4.3% and 16.8% consisted of a mixture of the wurtzite-type ZnO and the homologous compound Zn₇In₂O₁₀. All deposited films exhibited only the wurtzite-type ZnO lattice, being c-axis textured. The increase of the In concentration resulted in films less textured that also exhibited increased lattice parameters a and c. X-ray photoelectron spectroscopy investigations showed slight changes of the In 3d and Zn 2p binding energies for increased In content, consistent with an In doped ZnO lattice.     

Effect of cadmium oxide incorporation on the microstructural and optical properties of pulsed laser deposited nanostructured zinc oxide thin films

CdO doped (doping concentration 0, 1, 3 and 16 wt%) ZnO nanostructured thin films are grown on quartz substrate by pulsed laser deposition and the films are annealed at temperature 500 °C. The structural, morphological and optical properties of the annealed films are systematically studied using grazing incidence X-ray diffraction (GIXRD), energy dispersive X-ray analysis (EDX), scanning electron microscopy (SEM), atomic force microscopy (AFM), Micro-Raman spectra, UV–vis spectroscopy, photoluminescence spectra and open aperture z-scan. 1 wt% CdO doped ZnO films are annealed at different temperatures viz., 300, 400, 500, 600, 700 and 800 °C and the structural and optical properties of these films are also investigated. The XRD patterns suggest a hexagonal wurtzite structure for the films. The crystallite size, lattice constants, stress and lattice strain in the films are calculated. The presence of high-frequency E₂ mode and the longitudinal optical A₁ (LO) modes in the Raman spectra confirms the hexagonal wurtzite structure for the films. The presence of CdO in the doped films is confirmed from the EDX spectrum. SEM and AFM micrographs show that the films are uniform and the crystallites are in the nano-dimension. AFM picture suggests a porous network structure for 3% CdO doped film. The porosity and refractive indices of the films are calculated from the transmittance and reflectance spectra. Optical band gap energy is found to decrease in the CdO doped films as the CdO doping concentration increases. The PL spectra show emissions corresponding to the near band edge (NBE) ultra violet emission and deep level emission in the visible region. The 16CdZnO film shows an intense deep green PL emission. Non-linear optical measurements using the z-scan technique indicate that the saturable absorption (SA) behavior exhibited by undoped ZnO under green light excitation (532 nm) can be changed to reverse saturable absorption (RSA) with CdO doping. From numerical simulations the saturation intensity (I_s) and the effective two-photon absorption coefficient (β) are calculated for the undoped and CdO doped ZnO films.     

Growth and characterization of nitrogen-doped TiO2 thin films prepared by reactive pulsed laser deposition

Nitrogen-doped titanium dioxide (TiO₂) thin films were grown on (001) SiO₂ substrates by reactive pulsed laser deposition. A KrF* excimer laser source (λ = 248 nm, τ_FWHM ≅ 10 ns, ν = 10 Hz) was used for the irradiations of pressed powder targets composed by both anatase and rutile phase TiO₂. The experiments were performed in a controlled reactive atmosphere consisting of oxygen or mixtures of oxygen and nitrogen gases. The obtained thin film crystal structure was investigated by X-ray diffraction, while their chemical composition as well as chemical bonding states between the elements were studied by X-ray photoelectron spectroscopy. An interrelation was found between nitrogen concentration, crystalline structure, bonding states between the elements, and the formation of titanium oxinitride compounds. Moreover, as a result of the nitrogen incorporation in the films a continuous red-shift of the optical absorption edge accompanied by absorption in the visible spectral range between 400 and 500 nm wavelength was observed.     

Preparation,characterization, and photoluminescence study of PVA/ZnO nanocomposite films

ZnO nanoparticles with average diameter of 25 nm were synthesized by a modified sol–gel method and used in the preparation of (in wt.%) (100 − x) poly(vinyl alcohol) (PVA)/x ZnO nanocomposite films, with x = 0, 1, 2, 3, 4, and 5. The PVA/ZnO films were exposed to UV radiation for 96 h and their thermal, morphological, and spectroscopic properties were investigated. In inert atmosphere, the nanocomposite films showed lower thermal stability than the pure PVA film, and the calorimetric data suggest an interaction between PVA and ZnO in the nanocomposite films. Some crystalline phases could be seen in the films with ZnO, and a direct dependence on the ZnO concentration was also observed. The original structure of ZnO nanoparticles remained unaltered in the PVA matrix and they were uniformly distributed on the film surface. The roughness of the PVA film was not modified by the addition of ZnO; however, it increased after 96 h of UV irradiation, more significantly in the nanocomposite films. The films showed an absorption band centered at 370 nm and a broad emission band in the UV–vis region when excited at 325 nm.     

Growth of polycrystalline InP thin films by the pulsed laser deposition technique

The growth of polycrystalline InP films on glass substrates by the pulsed laser deposition technique is reported. Optimal growth conditions as high vacuum and relatively low substrate temperature were necessary to obtain stoichiometric InP layers. Structural and morphological characterizations of the samples are shown. X-ray diffraction shows that the stoichiometric InP films were face-centered cubic with preferred orientation of the crystallites over the (111) plane and mean grain size of about 60 nm. We also discuss the consequences of adverse growth conditions as bad vacuum and high substrate temperature on the film stoichiometry.     

Synthesis and characterization of cross-linked silicone thin films by pulsed laser ablation deposition (PLAD)

Stable, uniform and cross-linked silicone films have been synthesized by pulsed laser ablation deposition (PLAD) for the first time. A KrF excimer (248 nm) laser was used in the synthesis. The effect of incident energy density on the deposited film chemistry was examined in depth. The surface analysis showed that at low energy densities (100–150 mJ/cm²), smooth, hydrophobic films similar in structure to the starting cross-linked silicone elastomer were obtained. Beyond 200 mJ/cm², hydrophilic films with oxygen contents much higher than the starting polymer were obtained. These films also exhibited a more particulate texture suggesting ablation of particles and/or polymeric clusters from the silicone target. The results demonstrate that the PLAD process may prove valuable for the preparation of cross-linked silicone thin films with tailored properties. Received: 27 June 2001 / Accepted: 17 July 2001     

ITO thin films deposited by advanced pulsed laser deposition

Indium tin oxide thin films were deposited by computer assisted advanced PLD method in order to obtain transparent, conductive and homogeneous films on a large area. The films were deposited on glass substrates. We studied the influence of the temperature (room temperature (RT)-180 °C), pressure (1-6 × 10^− 2 Torr), laser fluence (1-4 J/cm²) and wavelength (266-355 nm) on the film properties. The deposition rate, roughness, film structure, optical transmission, electrical conductivity measurements were done. We deposited uniform ITO thin films (thickness 100-600 nm, roughness 5-10 nm) between RT and 180 °C on a large area (5 × 5 cm²). The films have electrical resistivity of 8 × 10^− 4 Ω cm at RT, 5 × 10^− 4 Ω cm at 180 °C and an optical transmission in the visible range, around 89%.     

Surface morphology of AlN films synthesized by pulsed laser deposition

Surface morphology of AlN films, synthesized on Si substrates by pulsed laser deposition, has been examined by recording atomic-force-microscopy (AFM) images. The influence of N₂ ambient pressure, ranging from 5 × 10⁻⁴ Pa to 10 Pa, is reflected well in the alteration of the surface roughness and size of crystallites of the AlN films. A tendency of a decrease in the surface roughness with increasing N₂ pressure was observed, which also correlates with the polycrystalline structure of the films. Deposition in vacuum resulted in the highest surface roughness due to the large size of crystallites emerging from the surface, while increasing the nitrogen pressure yielded smaller crystallites and a smoother film surface. The presented results could be useful for applications of pulsed laser deposited AlN in different optical and acoustic devices, where the crystalline quality of the AlN films and the surface is very important.     

Preparation of mixed (Cd,Bi)S composite thin films via surfactant facilitated electrodeposition process and their photoelectrochemical characterization

In the present investigation we explored possibilities of preparing mixed CdS–Bi₂S₃ composite thin films of nanodimensions using a single step surfactant facilitated electrochemical process from aqueous solutions containing different colloidal concentrations of CdS and Bi₂S₃ particles. As deposited composite thin films has been characterized on the basis of SEM, AFM and XRD studies for determination of their surface morphology, surface roughness and grain size. Photoelectrochemical characterization of these composite materials has been carried out on the basis of photopotential, current–voltage (I–V) characteristics under dark and illumination conditions and photoaction spectral studies. Attempt has also been made to estimate the resistance of these composite materials towards their electrochemical corrosion. As prepared mixed (Cd,Bi)S composite semiconductor film exhibits substantial improvement in their photoelectrochemical properties.     

Characterization on pulsed laser deposited nanocrystalline ZnO thin films

Nanocrystalline zinc oxide thin films were deposited on glass and silicon substrates by using pulsed laser deposition at different laser energy densities (1.5, 2, and 3 J/cm²). The film thickness, surface roughness, composition, optical and structural properties of the deposited films were studied using an α-step surface profilometer, atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), optical transmittance, and X-ray diffraction (XRD), respectively. The film thickness was calculated as 244 nm. AFM analysis shows that the root-mean-square roughness increases with increasing laser energy density. XPS analysis shows that the interaction of zinc with oxygen atoms is greatly increased at high laser energy density. In the optical transmittance spectra, a shift of the absorption edge towards higher wavelength region confirms that the optical band gap increases with an increase in laser energy density. The particle size of the deposited films was measured by XRD, it is found to be in the range from 7.87 to 11.81 nm. It reveals that the particle size increases with an increase in laser energy density.     

Corrosion resistant behaviour of DLC films

Diamond like carbon (DLC) films are deposited on AISI 304 SS using Plasma Enhanced Chemical Vapour Deposition (PECVD) method and their corrosion behaviour is studied. Corrosion resistance of DLC-coated AISI 304 SS has been found to increase in presence of corrosive solution (3.5% NaCl) as DLC functions physical barrier and restrain it from anodizing. DLC film is deposited using acetylene. Corrosion behaviour of the coated samples is tested by potentio-dynamic method. Surface morphology of the samples before and after corrosion tests is observed using high-resolution optical microscope as well as AFM.     

Nanoindentation and nanoscratch measurements on silicone thin films synthesized by pulsed laser ablation deposition (PLAD)

Nanoindentation and nanoscratch studies were conducted on silicone thin films synthesized by pulsed laser ablation deposition (PLAD). The nanoindentation studies showed that the modulus of the silicone films varied as a function of the energy density of deposition. The modulus values measured for PLAD silicone films were in the range of 1–6 GPa compared to 5–10 MPa reported for a typical silicone elastomer. Nanoscratch measurements also showed that PLAD silicone films exhibited much greater scratch resistance compared to silicone elastomer. These studies demonstrated that, even for low energy density depositions, the PLAD process can produced films which were are stronger and more abrasion resistant than conventional cross-linked silicone elastomers. Received: 27 June 2001 / Accepted: 27 June 2001     

Fabrication, structural and electrical characterization of lanthanum tungstate films by pulsed laser deposition

Films of lanthanum tungstate, 3 μm in thickness, were fabricated by means of pulsed laser deposition on a Pd foil. The films were characterized by X-ray diffraction, scanning electron microscopy, X-ray photoelectron spectroscopy and their electrical conductivity was measured at temperatures between 400 and 800 °C in different gas atmospheres. The films' structure and electrical characteristics are close to what is reported in the literature for corresponding polycrystalline material. The films exhibit fairly high proton conductivity at elevated temperatures, which make them interesting for components in hydrogen-related technologies. Changes in microstructure and the crystallographic orientation observed at higher temperatures were accompanied by changes in the conductivity characteristics.     

Nanoporous films obtained by sacrificial layer pulsed laser deposition

Integration of solid state gas sensors and solid oxide fuel cells into third generation microelectronic products requires the development of unique fabrication methods. Highly porous electrodes, critical to the performance of many gas dependent devices, typically require harsh production methods and high sintering temperatures that are incompatible with a variety of platforms including those based on silicon or glass. In this study, an alternative procedure for overcoming these problems has been developed. It is based on the synthesis of nano-porous films at reduced fabrication temperatures by means of the Sacrificial Layer Pulsed Laser Deposition (SL-PLD). SL-PLD utilizes simultaneous oxide and carbon deposition to deposit thin dense films. These amorphous films are then transformed into nano-porous perovskite films by thermal annealing in ambient air at 600 ºC. In this paper, an alternative process for the development of nano-porous thin films at reduced fabrication temperatures is presented. It takes advantage of the low temperatures needed for both carbon burn-off and the structural transformation of many perovskite oxides. This alternative method for thin film fabrication opens the possibility for low temperature fabrication of porous ceramic materials.     

Growth and characterization of Bi2Se3 thin films by pulsed laser deposition using alloy target

Bi₂Se₃ thin films were deposited on the (100) oriented Si substrates by pulsed laser deposition technique at different substrate temperatures (room temperature −400 °C). The effects of the substrate temperature on the structural and electrical properties of the Bi₂Se₃ films were studied. The film prepared at room temperature showed a very poor polycrystalline structure with the mainly orthorhombic phase. The crystallinity of the films was improved by heating the substrate during the deposition and the crystal phase of the film changed to the rhombohedral phase as the substrate temperature was higher than 200 °C. The stoichiometry of the films and the chemical state of Bi and Se elements in the films were studied by fitting the Se 3d and the Bi 4d5/2 peaks of the X-ray photoelectron spectra. The hexagonal structure was seen clearly for the film prepared at the substrate temperature of 400 °C. The surface roughness of the film increased as the substrate temperature was increased. The electrical resistivity of the film decreased from 1 × 10⁻³ to 3 × 10⁻⁴ Ω cm as the substrate temperature was increased from room temperature to 400 °C.     

Amorphous Terfenol-D films using nanosecond pulsed laser deposition

Thin films of Terfenol-D were produced by nanosecond pulsed laser deposition (PLD) at two fluences. Electron dispersive spectroscopy conducted using scanning electron and transmission electron microscopes showed that the film compositions were similar to that of the PLD target. Contrary to previous assertions that suggested that nanosecond PLD results in crystalline films, X-ray diffraction and transmission electron microscopy analysis showed that the films produced at both fluences were amorphous. Splatters present on the film had similar compositions to the overall film and were also amorphous. Magnetic measurements showed that the films had high saturation magnetization and magnetostriction, similar to high quality films produced using other physical vapor deposition methods.     

Ellipsometric study of nanostructured carbon films deposited by pulsed laser deposition

When depositing carbon films by plasma processes the resulting structure and bonding nature strongly depends on the plasma energy and background gas pressure. To produce different energy plasma, glassy carbon targets were ablated by laser pulses of different excimer lasers: KrF (248 nm) and ArF (193 nm). To modify plume characteristics argon atmosphere was applied. The laser plume was directed onto Si substrates, where the films were grown. To evaluate ellipsometric measurements first a combination of the Tauc-Lorentz oscillator and the Sellmeier formula (TL/S) was applied. Effective Medium Approximation models were also used to investigate film properties. Applying argon pressures above 10 Pa the deposits became nanostructured as indicated by high resolution scanning electron microscopy. Above ~ 100 and ~ 20 Pa films could not be deposited by KrF and ArF laser, respectively. Our ellipsometric investigations showed, that with increasing pressure the maximal refractive index of both series decreased, while the optical band gap starts with a decrease, but shows a non monotonous course. Correlation between the size of the nanostructures, bonding structure, which was followed by Raman spectroscopy and optical properties were also investigated.     

Growth of diborides thin films on different substrates by pulsed laser ablation

The growth of scandium, titanium and zirconium diborides thin films by pulsed laser ablation technique on different substrates has been studied. In situ reflection high energy electron diffraction and ex situ X-ray diffraction analyses indicate that the films are strongly c-axis oriented on all the substrates and also epitaxial, apart from Si(111), where the in plane orientation is poor. Atomic force microscopy imaging reveals a flat surface in all the epitaxial samples, with roughness lower than 1 nm. The results on silicon carbide and sapphire are very promising for using these materials as buffer layers in magnesium diboride thin films growth, especially to improve epitaxy and to prevent oxygen diffusion from the substrate, and also to study the influence of lattice strain on MgB₂ critical temperature.