Detection limits of high temperature superconducting materials on various substrates by energy dispersive X-ray fluorescence and proton induced X-ray emission methods

Application of energy dispersive X-ray fluorescence (EDXRF) and proton induced X-ray emission (PIXE) methods has been demonstrated for determining the elemental composition of thin film superconducting materials. The results of analysis carried out by EDXRF method have been compared with those obtained by PIXE method. Thin films of YBa₂Cu₃O₇ superconducting material were deposited on various substrates such as thin mylar sheet and thick substrates of SrTiO₃, MgO and Al₂O₃. In thin backing the minimum detection limits obtained for Cu, Y, Ba by the PIXE method are 20 ng, 70 ng and 800 ng respectively and the corresponding values by the EDXRF method are 3000 ng, 600 ng and 1000 ng. Detection limits for samples on thick backings deteriorated to a large extent by both methods.     

XPS studies of short pulse laser interaction with copper

The effect of laser ablation on copper foil irradiated by a short 30 ns laser pulse was investigated by X-ray photoelectron spectroscopy. The laser fluence was varied from 8 to 16.5 J/cm² and the velocity of the laser beam from 10 to 100 mm/s. This range of laser fluence is characterized by a different intensity of laser ablation. The experiments were done in two kinds of ambient atmosphere: air and argon jet gas.The chemical state and composition of the irradiated copper surface were determined using the modified Auger parameter (α′) and O/Cu intensity ratio. The ablation atmosphere was found to influence the size and chemical state of the copper particles deposited from the vapor plume. During irradiation in air atmosphere the copper nanoparticles react with oxygen and water vapor from the air and are deposited in the form of a CuO and Cu(OH)₂ thin film. In argon atmosphere the processed copper surface is oxidized after exposure to air.     

Gold nano-wires and nano-layers at laser-induced nano-ripples on PET

Gold nano-layers were deposited onto laser irradiated polyethyleneterephthalate (PET) surfaces. For irradiation, we used the linearly polarized light of a pulsed 248 nm KrF and 157 nm F₂ laser, respectively. In a certain range of irradiation parameters, the irradiation resulted in the formation of coherent ripples patterns with a lateral periodicity in the order of the wavelength of the laser light and with a corrugation height of several 10 nm. The deposited layers were then prepared by sputtering. The layers were analyzed by atomic force microscopy (AFM), focused ion beam (FIB) cuts, scanning electron microscopy (SEM), and angular resolved X-ray induced photoelectron spectroscopy (ARXPS). Gold sputtering on KrF laser irradiated PET led to the formation of separated “nano-wires” at the ridges of the nano-patterns and not to a continuous metal layer, as we obtained in case of gold sputtering onto F₂ irradiated PET. The results of the XPS analysis indicated, that the KrF irradiation caused degradation on the ridge of the ripples, whereas no noticeable degradation occurred for F₂ laser treatment. We attribute the different growth mechanisms of the deposited gold layers mainly to the difference in surface chemical composition of laser irradiated PET with the two different lasers employed.     

准分子激光扫描消融淀积大尺寸超导薄膜

利用我们设计的一套光学变换传输系统实现了激光束在超导靶上一定范围内扫描消融来淀积高T_c超导薄膜。实验表明用这种激光扫描消融方法可使大尺寸超导薄膜的厚度均匀性得到较大的改善。我们采用激光扫描半径为9mm在12mm×33mm的Y-ZrO₂基片上淀积出零电阻温度T_c≥90K,临界电流密度J_c(零磁场,77K)≥1×10⁶A/cm²,薄膜c轴择优取向,厚度均匀性较好的YBa _关键词：     

The influence of substrate material and annealing procedure on the properties of superconducting thin films

Thin layers YBa₂Cu₃O_7–x. are deposited by a laser ablation technique using a pulsed excimer laser operating at 308 nm. The influence of the substrate material and the annealing procedure on the superconducting behaviour of the 123 film and the reactions between the film and the substrate are studied by resistance, X-ray patterns and TEM measurements. The best results are obtained for deposition on (100) SrTiO₃ substrates. The resistance of the 1 m thick film shows a metallic behaviour, an onset in superconductivity at a temperature of 90 K, and has zero resistance at 86 K. The 123 material has a preferential oriented c-axis perpendicular to the surface plane.     

Thin films prepared from tungstate glass matrix

Vitreous samples containing high concentrations of WO₃ (above 40% M) have been used as a target to prepare thin films. Such films were deposited using the electron beam evaporation method onto soda-lime glass substrates. These films were characterized by X-ray diffraction (XRD), perfilometry, X-ray energy dispersion spectroscopy (EDS), M-Lines and UV-vis absorption spectroscopy. In this work, experimental parameters were established to obtain stable thin films showing a chemical composition close to the glass precursor composition and with a high concentration of WO₃. These amorphous thin films of about 4 μm in thickness exhibit a deep blue coloration but they can be bleached by thermal treatment near the glass transition temperature. Such bleached films show several guided modes in the visible region and have a high refractive index. Controlled crystallization was realized and thus it was possible to obtain WO₃ microcrystals in the amorphous phase.     

The characteristics of Au:VO2 nanocomposite thin film for photo-electricity applications

Au nanoparticles have been fabricated on normal glass substrates using nanosphere lithography (NSL) method. Vanadium dioxide has been deposited on Au/glass by reactive radio frequency (rf) magnetron sputtering. The structure and composition were determined by X-ray diffraction and X-ray photoelectron spectroscope. Electrical and optical properties of bare VO₂ and Au:VO₂ nanocomposite thin films were measured. Typical hysteresis behavior and sharp phase transition were observed. Nanopartical Au could effectively reduce the transition temperature to 40 °C. The transmittance spectrum for both Au:VO₂ nanocomposite thin film shows high transmittance under transition temperature and low transmittance above transition temperature. The characteristics present the Au:VO₂ nanocomposite thin film can be used for applications, such as “smart window” or “laser protector”.     

Growth and characterization of infinite-layer films deposited by pulsed-laser deposition

Summary The increasing interest for infinite-layer materials is due essentially to the possibility of studying the simplest high-T _c superconductors parent structure. The usual method to produce this material is high-pressure synthesis. In this paper we report on this new material deposited by pulsed laser deposition and on the possibility to create infinite-layer superconducting films. Paper presented at the ?VII Congresso SATT?, Torino, 4–7 October 1994.     

Structural characterization and magnetoresistance of manganates thin films and Fe-doped manganates thin films

Perovskites thin films with the composition La_0.6Ca_0.4MnO₃ doped with 20% Fe, were prepared by pulsed reactive crossed beam laser ablation, where a synchronized reaction gas pulse interacts with the ablation plume. The films were grown on various substrates and the highest colossal magnetoresistance ratio (CMR) was detected by Hall measurements for films grown on LaAlO₃ (1 0 0), which was selected as substrate for further investigations.Several growth parameters, such as substrate temperature and target to substrate distance were varied to analyze their influence on the film properties.The structure of the deposited thin films was characterized by X-ray diffraction and atomic force microscope, while Rutherford backscattering (RBS) was used to determine the film stoichiometry. The electrical properties were determined by Hall effect measurements in a magnetic field of 0.51 T.These measurements reveal that the amplitude of the CMR ratio depends strongly on the substrate and that the oxygen content influences the temperature where the transition from semiconductor to metal is observed.     

Influences of CO2 laser annealing on mechanical and laser-induced damage properties of ZrO2 thin films

Zirconium dioxide (ZrO₂) thin films were deposited on BK7 glass substrates by the electron beam evaporation method. A continuous wave CO₂ laser was used to anneal the ZrO₂ thin films to investigate whether beneficial changes could be produced. After annealing at different laser scanning speeds by CO₂ laser, weak absorption of the coatings was measured by the surface thermal lensing (STL) technique, and then laser-induced damage threshold (LIDT) was also determined. It was found that the weak absorption decreased first, while the laser scanning speed is below some value, then increased. The LIDT of the ZrO₂ coatings decreased greatly when the laser scanning speeds were below some value. A Nomarski microscope was employed to map the damage morphology, and it was found that the damage behavior was defect-initiated both for annealed and as-deposited samples. The influences of post-deposition CO₂ laser annealing on the structural and mechanical properties of the films have also been investigated by X-ray diffraction and ZYGO interferometer. It was found that the microstructure of the ZrO₂ films did not change. The residual stress in ZrO₂ films showed a tendency from tensile to compressive after CO₂ laser annealing, and the variation quantity of the residual stress increased with decreasing laser scanning speed. The residual stress may be mitigated to some extent at proper treatment parameters.     

Development of laser deposited multilayer zone plate structures for soft X-ray radiation

As a novel approach, the combination of pulsed laser deposition and focused ion beam was applied to fabricate different types of multilayer zone plate structures for soft X-ray applications. For this purpose, high quality non-periodic ZrO₂/Ti multilayers were deposited by pulsed laser deposition on planar Si substrates and on rotating steel wires with layer thicknesses according to the Fresnel zone plate law. Linear focusing optics were fabricated by cutting slices out of the multilayers by focused ion beam and placing them directly over pinholes within Si₃N₄ substrates. Additionally, it was shown that laser deposition of depth-graded multilayers on a wire is also a promising way for building up multilayer zone plates with point focus. First experiments using a table-top X-ray source based on a laser-induced plasma show that the determined focal length and spatial resolution of the fabricated multilayer Laue lens corresponds to the designed optic.     

Structural,optical and electrical properties of post annealed Mg doped ZnO films for optoelectronics applications

Mg _x Zn_1-x O films with 0.15 mole composition of Magnesium were successfully deposited by the spin coating sol–gel method. Zinc acetate dihydrate and Magnesium acetate were used as starting precursors to prepare the solution in ethanol solvent. The MgZnO films were deposited on microscopic glass substrates and post annealed at three different temperatures. X-ray Diffractometer (XRD), Scanning Electron Microscopy (SEM) and UV–VIS Spectrophotometer were used to characterize the deposited films for studying structural and optical properties. Energy dispersive analysis by X-ray (EDAX) was used to determine incorporation of Mg content in ZnO films. XRD spectrum reveals that, the deposited Mg doped ZnO films were polycrystalline in nature. The intensity of c-axis in the XRD spectrum goes on decreasing as Mg composition slightly increasing corresponding to increase in annealing temperature. EDAX spectra clearly showed the incorporation of Mg into the ZnO films. Semiconductor characterization system was used for the I–V characterization of MgZnO films. I–V characteristics show decrease in current as increase in the biased voltage. Optical band gap of MgZnO films was found to be increased from 3.2 to 3.38 eV as estimated from the absorption coefficients.     

AlN thin films prepared by ArF plasma assisted PLD. Role of process conditions on electronic and chemical–morphological properties

Aluminium nitride thin films were deposited on n-Si <100> substrates by RF plasma activated reactive pulsed laser deposition (PLD). An ArF excimer pulsed laser, 10 Hz and 2.5 J/cm² energy fluence, has been used to ablate a pure Al target in a reactive atmosphere of N₂ plasma (generated by a RF source), at varying processing parameters (substrate temperature, time, and N₂ plasma configuration). We studied the dependence and correlation of structural and electronic properties with the experimental conditions. The chemical composition of deposited material has been determined by both Raman and X-ray photoelectron spectroscopy (XPS). Electrical resistivity has been evaluated by the sheet resistance method. Both spectroscopic characterizations (Raman and XPS) show a strong dependence in the formation of AlN on the deposition temperature. At low temperatures, there is little formation of nitride, with a prevalence of aluminium oxide, while at higher temperatures the N uptake increases, with AlN formation. Raman analysis also highlights the formation of nano-structures, for temperatures ≥400^°C. These material characteristics have a fundamental influence on the electronic properties. Indeed, electrical resistivity properties have been found to be strongly dependent on the film structure, nitrogen incorporation, and presence of mixed oxide compounds, closely related to deposition temperature.     

X-ray photoelectron study of annealed Co thin film on Si surface

The X-ray photoelectron spectroscopy (XPS) study on as deposited as well as 500 °C annealed Co (400 Å)/Si thin film synthesized by electron beam evaporation technique under UHV conditions is reported here. The XPS measurements carried out on as deposited sample rule out the possibility of any phase formation at room temperature. Whereas in 500 °C annealed sample the Co-2p_3/2 peak is observed at ∼778.6 eV binding energy position, where the peak expected due to CoSi₂ resides. The Auger parameters were also calculated at each step of experiment because Auger parameter is always very sensitive to changes in the chemical state of the material. The recorded spectrum on annealed sample shows Auger parameter value of ∼1551.4 eV, which is different from that observed in the as deposited sample (∼1552.1 eV). The obtained results are analyzed and interpreted in terms of CoSi₂ phase formation at the interface with annealing.     

Vacancies ordered in screw form (VOSF) and layered indium selenide thin film deposition by laser back ablation

Indium selenide thin films are important due to their applications in non-volatile memory and solar cells. In this work, we present an initial study of a new application of deposition-site selective laser back ablation (LBA) for making thin films of In₂Se₃. Invacuo annealing and subsequent characterization of the films by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS) indicate that control of substrate temperature during deposition and post-deposition annealing temperature is critical in determining the phase and composition of the films. The initial laser fluence and target film thickness determine the amount of material deposited onto the substrate.     

Pulsed laser deposition of silicon substituted hydroxyapatite coatings from synthetical and biological sources

Silicon substituted hydroxyapatite (Si-HA) is a new material with an enhanced bioactibity and it can be produced by chemical synthesis. Nevertheless, the coating of metallic substrates with a bioactive material is a common method nowadays to improve its integration with the receptor bone.Si-HA films were deposited by pulsed laser deposition (PLD), using targets composed of mixtures of HA with different Si containing sources such as SiO₂ and diatomaceous earth. The Si-HA films were characterized in terms of structure and chemical composition by spectroscopic techniques (FTIR, XPS), and several ion beam techniques (RBS, PIXE). The analysis revealed that the Si is successfully incorporated into the HA structure, as well as traces of other elements such as Na, Fe or K.     

Improvement of corrosion resistance of carbon steel using chemical vapor deposition from Cr(CO)6 with an ArF excimer laser

Corrosion resistance of carbon steel coated with thin film deposited from Cr(CO)₆ using an ArF excimer laser (193 nm) has been evaluated by an electrochemical method as a function of laser beam intensity. The carbon steel coated with the film formed at higher beam intensity shows higher corrosion resistance. Microstructure, composition, and thickness of the films have also been investigated. SEM micrographs show that the films consist of small grains which decrease in size with increasing beam intensity. Auger electron spectroscopy (AES) combined with Ar⁺ beam sputtering reveals that the films deposited at higher beam intensity give higher chromium content, and that the thickness at a fixed total irradiation energy increases up to the intensity of 10 MW cm^–2, falling above this intensity. In addition, the change of film thickness by addition of buffer gases (Ar, CO, and H₂O) has been investigated. The thickness is 10 times smaller under the addition of H₂O, and twice smaller under the addition of Ar or CO than without the addition of gases. A deposition mechanism based on photolysis of Cr(CO)₆ in the gas phase is proposed related to the experimental data after the discussion of several possible mechanisms.     

Experimental study of conditions for the 3D laser cladding of nickel aluminide

The layerwise laser cladding of powdered alloy based on intermetallic gamma Ni₃Al phase is studied. The effect deposition parameters have on the geometry of the deposited beads is shown. Microstructures are investigated and the cracking susceptibility of the deposited material is analyzed. The effective deposition parameters are determined within a range of specific laser energy inputs of (2–8) × 10⁶ J kg^?1 at beam scanning rates of (1.67–10) × 10^?3 m/s and a powder feed of 6.3 × 10^?5 kg/s^?1.     

Pulsed laser deposition of c * axis oriented pentacene films

Pulsed laser desorption and film deposition behaviors have been investigated on pentacene as an organic molecule primarily due to its applications in electronics. The laser desorption time-of-flight (LDTOF) mass spectrum exhibited a single parent peak when a pressed pentacene pellet was ablated by an N₂ laser beam of its fluence lower than 100 mJ/cm², indicating that pentacene could be evaporated without an appreciable photodecomposition by the pulsed laser beam. Nd:YAG pulsed laser deposition of pentacene films was performed using such optimization parameters as laser fluences and wavelength (second, third and forth harmonic generations (SHG, THG, FHG)). The analyses with AFM, XRD and UV-Vis spectroscopy revealed the fabrication of c^* axis oriented pentacene films on quartz, silicon, and CaF₂ substrates by the SHG. The SHG films have a surface morphology superior to those of films deposited by THG and FHG. PACS 81.15.Fg; 81.05.Lg; 82.80.Rt     

Submicron focusing of XUV radiation from a laser plasma source using a multilayer Laue lens

The focusing properties of a one-dimensional multilayer Laue lens (MLL) were investigated using monochromatic soft X-ray radiation from a table-top, laser-produced plasma source. The MLL was fabricated by a focused ion beam (FIB) structuring of pulsed laser deposited ZrO₂/Ti multilayers. This novel method offers the potential to overcome limitations encountered in electron lithographic processes. Utilizing this multilayer Laue lens, a line focus of XUV radiation from a laser-induced plasma in a nitrogen gas puff target could be generated. The evaluated focal length is close to the designed value of 220 μm for the measurement wavelength of 2.88 nm. Divergence angle and beam waist diameter are measured by a moving knife edge and a far-field experiment, determining all relevant second-order moments based beam parameters. The waist diameter has been found to be approximately 370 nm (FWHM).