Orientation study of iron phthalocyanine (FePc) thin films deposited on silicon substrate investigated by atomic force microscopy and micro-Raman spectroscopy

In this article, we present temperature and orientation study of iron phthalocyanine (FePc) thin films with different thickness deposited on silicon substrate. The organic thin films were obtained by the quasi-molecular beam evaporation. The micro-Raman scattering spectra of FePc thin layers were investigated in the spectral range 550–1,800 cm⁻¹ using 488-nm excitation wavelength. The Raman scattering and atomic force microscopy studies were performed at room temperature before and after annealing process. Annealing process of thin layers was carried out at 453 K for 6 h. From polarized Raman spectra using surface Raman mapping procedure the information on distribution of polymorphic phases of FePc layers has been carried out. Moreover, the obtained results showed the influence of the annealing process on the ordering of the molecular structure of thin films deposited on silicon substrate. For the very thin layers we did not observe the change of the polymorphic phase but only reordering of the thin layers and change of molecular structure to intermediate phase. Using atomic force microscopy method, we observed arrangement of the thin layers structure connected with the change of roughness of the thin layers after annealing process. The obtained results indicate that the structure of thin layer deposited on silicon substrate is strongly affected by the annealing process.     

Effect of inserting a buffer layer on the characteristics of transparent conducting impurity-doped ZnO thin films prepared by dc magnetron sputtering

In transparent conducting impurity-doped ZnO thin films prepared on glass substrates by a dc magnetron sputtering (dc-MS) deposition, the obtainable lowest resistivity and the spatial resistivity distribution on the substrate surface were improved by a newly developed MS deposition method. The decrease of obtainable lowest resistivity as well as the improvement of spatial resistivity distribution on the substrate surface in Al- or Ga-doped ZnO (AZO or GZO) thin films were successfully achieved by inserting a very thin buffer layer, prepared using the same MS apparatus with the same target, between the thin film and the glass substrate. The deposition of the buffer layer required a more strongly oxidized target surface than possible to attain during a conventional dc-MS deposition. The optimal thickness of the buffer layer was found to be about 10 nm for both GZO and AZO thin films. The resistivity decrease is mainly attributed to an increase of Hall mobility rather than carrier concentration, resulting from an improvement of crystallinity coming from insertion of the buffer layer. Resistivities of 3 × 10^− 4 and 4 × 10^− 4Ω cm were obtained in 100 nm-thick-GZO and AZO thin films, respectively, incorporating a 10 nm-thick-buffer layer prepared at a substrate temperature around 200 °C.     

Growth of highly c-axis oriented aluminum nitride thin films on β-tantalum bottom electrodes

We have investigated the influence of tantalum (Ta) bottom electrodes on the crystallinity and crystal orientation of aluminum nitride (AlN) thin films. AlN thin films and Ta electrodes were prepared by using rf magnetron sputtering method. The crystal structure of the Ta electrodes was tetragonal (β-Ta, a metastable phase) at room temperature. The crystallinity and orientation of the AlN thin films and Ta electrodes strongly depended on sputtering conditions. Especially, the crystallinity and crystal orientation of the Ta electrodes were influenced by their film thickness and the substrate temperature. When the thickness of the Ta bottom electrodes was 200 nm and the substrate temperature was 100 °C, the AlN thin films indicated high c-axis orientation (the full width at half maximum of rocking curve of 3.9°). The crystal orientation of the AlN film was comparable to that of AlN thin films deposited on face centered cubic (fcc) lattice structure metal, such as Au, Pt and Al, bottom electrodes.     

Fabrication of <Emphasis Type="Italic">p</Emphasis>-type doped ZnO thin films using pulsed laser deposition

Two new methods were investigated for the fabrication of p-type doped ZnO thin films in a conventional pulsed laser deposition apparatus, but using only pure materials as targets. One of these is a sequential method and consists in firing alternatively the laser on a pure ZnO target and either a monocrystalline InP target (for phosphorus doping) or a Bi₂O₃ ceramic target (for bismuth doping). The other method consists in taking advantage of the lithium diffusion into a ZnO thin film while being deposited on a c-LiNbO₃ substrate at high temperature. Some structural and electronic properties of the ZnO material obtained using these methods were measured using secondary ion mass spectrometry, X-ray diffraction, laser photoluminescence and Hall apparatus respectively and compared with those obtained for pure n-type thin films. The main results of this study are as follows. The sequential deposition method was successful in incorporating InP in ZnO films but led to inhomogeneous In and P spatial distributions, while segregation of Bi₂O₃ within the ZnO was evidenced by both the X-ray diffraction and photoluminescence results. Electrical measurements have revealed n-type conductivity for the ZnO/InP and the ZnO/c-LiNbO₃ thin films and a peculiar behaviour for the ZnO/Bi₂O₃ samples which could point out to successful p-type doping for films containing smaller amounts of Bi₂O₃.     

Effects of High Magnetic Field on the Structure and Magnetic Properties of Molecular Beam Vapor Deposited Fe₆₀Ni₄₀ Thin Films

The Fe₆₀Ni₄₀ (in atomic %) polycrystalline thin films with 90 nm thickness were prepared on 200 °C quartz substrate by using molecular beam vapor deposition method. The influence of 0 T and 6 T magnetic fields on the structural evolution and magnetic properties of thin films was studied by using EDXS, XRD, AFM and VSM. In this study, only α phase was formed in both thin films. It was found that the application of a 6 T magnetic field obviously decreases the RMS of surface roughness and the grain size. For the magnetic properties of the thin films, the 6 T magnetic field increases the saturation magnetism Ms in-plane and the squareness (Mr/Ms) of the hysteresis loop and decreases the coercive force Hc. This indicates the soft magnetic properties of the thin films have been notably enhanced in-plane by a high magnetic field. The relationship between the structural evolution and magnetic properties was discussed in details.     

Thermal Diffusivity Measurement for Titanium Thin Films on Copper Substrate by Laser Produced Plasmas

The transport properties of condensed phase materials are, in principle, dependent on the local structure and composition of the specimen. This is particularly evident near the free surface of a solid alloy specimen where the morphology, composition, and thermal diffusivity exhibit significant depth dependence, as demonstrated in an earlier study of the depth-resolved thermal diffusivity of a galvanized steel specimen. A new non-contact method was used, based on time-resolved, spectroscopic measurement of the total mass removed from the specimen surface representatively in elemental composition by a high-power laser pulse. A new study of a titanium thin film of varying thickness deposited on a copper substrate is presented. The titanium thin film is first fabricated in a vacuum and then immediately analyzed for composition and thermophysical properties in situ, both by the method of representative laser-produced plasmas (LPP). Successive ablation layers of the thin film, as exposed by LPP ablation, have revealed the dependence of the thermophysical properties on film thickness as well as on depth. The existence of a characteristic length over which the substrate influences the dynamics of thermal transport in the titanium thin film has also been observed.     

A combinatorial characterization scheme for high-throughput investigations of hydrogen storage materials

Abstract

In order to increase measurement throughput, a characterization scheme has been developed that accurately measures the hydrogen storage properties of materials in quantities ranging from 10 ng to 1 g. Initial identification of promising materials is realized by rapidly screening thin-film composition spread and thickness wedge samples using normalized IR emissivity imaging. The hydrogen storage properties of promising samples are confirmed through measurements on single-composition films with high-sensitivity (resolution <0.3 μg) Sievert’s-type apparatus. For selected samples, larger quantities of up to ～100 mg may be prepared and their (de)hydrogenation and micro-structural properties probed via parallel in situ Raman spectroscopy. Final confirmation of the hydrogen storage properties is obtained on ～1 g powder samples using a combined Raman spectroscopy/Sievert’s apparatus.     

Densification of amorphous sol-gel TiO2 films: An X-ray reflectometry study

Sol-gel TiO₂ thin films were dip coated on soda lime glass substrate using tetraisopropoxide as titania precursor. Four withdrawal speeds were tested and the resulting dried thin films have been annealed at 400 °C, 450 °C and 500 °C for 1 h. Glancing Incidence X-ray Diffraction has revealed the amorphous nature of the thin films whatever is the annealing temperature. In order to study the thin films densification, X-ray Reflectometry curves have been fitted by a three layers Parrat model and by the Distorded Wave Born Approximation (DWBA) box model which provides more details on the Electron Density Profile. The presence of high density layers localized at the film surface and at the substrate-film interface has been evidenced for the annealed films. The DWBA fitting method allows us to point out a density gradient, probably arising from the initial packing density and to the constraint due to the substrate, along the film thickness.     

Determination of interface properties between micron-thick metal film and ceramic substrate using peel test

Peel test measurements have been performed to estimate both the interface toughness and the separation strength between copper thin film and Al₂O₃ substrate with film thicknesses ranging between 1 and 15 μm. An inverse analysis based on the artificial neural network method is adopted to determine the interface parameters. The interface parameters are characterized by the cohesive zone (CZ) model. The results of finite element simulations based on the strain gradient plasticity theory are used to train the artificial neural network. Using both the trained neural network and the experimental measurements for one test result, both the interface toughness and the separation strength are determined. Finally, the finite element predictions adopting the determined interface parameters are performed for the other film thickness cases, and are in agreement with the experimental results.     

Aqueous lateral epitaxy overgrowth of ZnO on (0001) GaN at 90 °C: Part I. Increasing the critical thickness

Thick, epitaxial ZnO thin films have been grown on (0001) GaN buffered Al₂O₃ substrates using an aqueous solution at 90 °C. Films with improved structural, optical and electrical characteristics, were grown using a lateral epitaxial overgrowth (LEO) method. Different photoresist masks were used to enable LEO. The masks included linear windows and two different hexagonal arrays of circular windows. Films that exceeded a critical thickness mechanically failed through buckling, consistent with the large compressive stresses expected due to the mismatch of the ZnO lattice with the underlying GaN substrate. It was shown that improved mechanical stability could be achieved using the LEO method. Without LEO, a film thickness no greater than 4 µm could be grown without buckling. The critical thickness could be increased to 10 µm using linear windows, whereas a critical thickness of 50 μm was achieved with one array of circular windows, and 80 µm for a second array. The two different arrays of circular windows differed relative to their orientation on the substrate. It was also shown that the critical thickness increased with increasing distance between the growth windows. Optical transmission, micro-photoluminescence and Hall Effect measurements showed that the LEO method also results in improved optoelectronic properties.     

Effect of spatial relationship between arc plasma and substrate on the properties of transparent conducting Ga-doped ZnO thin films prepared by vacuum arc plasma evaporation

The effect of the spatial relationship between the arc plasma flow and the substrate surface on the resulting film thickness and electrical properties is investigated in transparent conducting Ga-doped ZnO (GZO) thin films deposited by a vacuum arc plasma evaporation (VAPE) method. It was found that the resulting electrical properties of GZO thin films produced by a VAPE deposition on a fixed substrate were considerably dependent on both the film thickness and the location on the substrate surface, extending from the area nearest the arc plasma source to that at the opposite end of the substrate in a direction parallel to the arc plasma flow; with GZO thin films deposited with various thicknesses in the range from 20 to 200 nm, the films exhibited a thickness dependence of resistivity that was considerably affected by the location on the substrate surface. The variation of resistivity relative to the location on the substrate surface was related to that of carrier concentration, which is mainly attributed to the distribution of the amount of oxygen reaching the substrate surface. In GZO thin films deposited with a thickness of 30-40 nm at a substrate temperature of 250 °C, a resistivity as low as 4 × 10^− 4 Ω cm was obtained in the area of the substrate nearest the arc plasma source.     

Heat treatment effects on the formation of lanthanum-modified lead zirconate titanate thin films

The microstructural and compositional properties of lanthanum-modified lead zirconate titanate (PLZT) thin films deposited on platinum coated Si substrates by RF magnetron sputtering have been studied. The heat treatment processes of substrate heating during deposition and post deposition furnace and rapid thermal annealing were compared as processes for obtaining the desired pervoskite phase. PLZT thin films deposited with in-situ substrate heating showed little evidence of micro-cracking. The XRD data obtained showed the formation of pervoskite phase at 550 °C and indicated the suppression of the pyrochlore phase for increasing temperatures. The RBS analysis revealed a film thickness of 140 nm and composition of (Pb_0.91La_0.09)(Zr_0.6Ti_0.4)O₃. Deposition performed with in-situ substrate heating at 650 °C resulted in highly (110) pervoskite orientated thin films with an average grain size around 160 to 200 nm and an RMS roughness of 3 nm.     

Berührungslose Prüfung von Kunststoffen mittels photothermischer Wärmewellenanalyse

Remote Testing of Polymers with Photothermal Analysis of Thermal Waves After an introduction to thermal waves a comparison is made of photoacoustic detection methods (gas cell, piezoceramic) and photothermal detection arrangements (front surface and rear surface methods). Previously only photoacoustic methods have been applied to polymer related problems, while the advantages of photothermal measurements – remote and nondestructive evaluation – have been demonstrated on metals. The experimental part of this paper presents first steps to apply photothermal analysis of thermal waves to some problems of polymers: thickness measurement of thin layers; on-surface and subsurface defects; delamination of bonding and coating curing reactions; glass fibre content; orientation of fibres and molecules; aging processes. The present results indicate that the method can be used for nondestructive remote quality assurance of thin layers and foils. Further development is required to apply the method to nondestructive testing of thick walled components.     

Effect of Sputtering Parameters on Superconducting Properties of GdBaCuO Epitaxial Thin Film Deposited by ICP Method

Thin films of GdBaCuO (GBCO) have been deposited in situ onto LaAlO₃ single crystal substrates by inverted cylindrical sputtering pattern (ICP). The superconductive properties of the thin films' dependence on the substrate temperature and sputtering pressure have been systematically investigated. By optimization of the deposition parameter, high-quality c-axis epitaxial GBCO thin films of T _c0>92 K were reproducibly grown. The T _c of the best sample is as high as 93.2 K. Upon changing the target composition to GdBa₂Cu₄O _y (Gd₁₂₄), it was observed that the samples always show some a-axis oriented films, implying that excess copper would favor a-axis growth in thin films. The superconductivity of the thin films under higher substrate temperature (T _s>800°C) was clearly improved by the procedure of special post-oxygenization at 400°C with an ozone atmosphere. This is very useful for preparing large-area thin films of GBCO.     

Studies on the thermoelectric effect in semiconducting ZnTe thin films

The thermoelectric power of Zinc Telluride (ZnTe) thin films, prepared onto glass substrate by e-beam evaporation technique in vacuum at ∼8 × 10⁻⁴ Pa, has been measured from room temperature up to 413 K with reference to pure copper. The deposition rate of the ZnTe thin films was maintained at about 2.05 nm s⁻¹. The thickness and temperature dependence of its related parameters have been studied. The Fermi-levels were determined using a non-degenerate semiconducting model. The carrier scattering index, activation energy and temperature of coefficient of activation energy have all been obtained at different ranges of thickness and temperature. All the samples were optically transparent and amorphous in structure.     

Electrocaloric effect of PMN-PT thin films near morphotropic phase boundary

The electrocaloric effect is calculated for PMN-PT relaxor ferroelectric thin film near morphotropic phase boundary composition. Thin film of thickness, ∼240 nm, has been deposited using pulsed laser deposition technique on a highly (111) oriented platinized silicon substrate at 700°C and at 100 mtorr oxygen partial pressure. Prior to the deposition of PMN-PT, a template layer of LSCO of thickness, ∼60 nm, is deposited on the platinized silicon substrate to hinder the pyrochlore phase formation. The temperature dependent P-E loops were measured at 200 Hz triangular wave operating at the virtual ground mode. Maximum reversible adiabatic temperature change, ΔT = 31 K, was calculated at 140°C for an external applied voltage of 18 V.     

Photoacoustic analysis and imaging techniques: Sound of light

An unusual form of imaging and analysis applications combines optics and acoustics to probe the features and behaviors of materials. The name of photoacoustic like all other techniques of spectroscopy reveals underlying its theoretical basis. Even if the prefix “photo” makes sense for a spectroscopy, acoustic may be initially amazing. Photoacoustic technique is extension of the photothermal effect, which is based on light beam hitting the sample and altering its thermal status. More precisely, photoacoustic effect is a transformation between light, heat, and sound caused by light absorption. After the successful formulation of general theoretical model, photoacoustic technique, which initially was only used for the analysis of gas samples, has been efficiently extended to analysis of condensed matters. Variety of samples, nondestructive analysis and imaging, depth profiling, high specificity and sensitivity, analysis of opaque samples are the most important advantages of photoacoustic technique. As of today, many researchers have performed in vitro and in vivo analysis and imaging application using photoacoustic technique; moreover, increasing number of companies are manufacturing biomedical imaging devices based on this effect. If the obstacles to experimental restrictions are removed, we will begin to hear the sound of light as more powerfully in many applications, particularly physics, materials science, and medicine.     

Experimental investigations of three-dimensional effects near a crack tip using computer vision

An experimental study of the near tip deformation fields for a Single Edge-Cracked specimen (SEC) has been completed. The surface deformation fields for a thin SEC plexiglas specimen have been obtained in the region 0.15 <- r/t <- 0.60, where r is radial distance from the crack tip and t is the specimen thickness, by using a novel computer vision method. The results of the study indicate that the value of the J-Integral obtained from the measured surface deformation, and under the assumption of plane stress linearly elastic behavior, is essentially path independent over a region that is considered to be within the crack tip three-dimensional zone by researchers who have performed tests on other materials.However, the near-tip, in-plane displacement field does show a deviation from the traditional linear elastic crack tip singularity over the same region, suggesting the need for further studies to address this inconsistency.     

Structural and electrical properties of RuO2 thin films prepared by rf-magnetron sputtering and annealing at different temperatures

Conductive ruthenium oxide (RuO₂) thin films have been deposited at different substrate temperatures on various substrates by radio-frequency (rf) magnetron sputtering and were later annealed at different temperatures. The thickness of the films ranges from 50 to 700 nm. Films deposited at higher temperatures show larger grain size (about 140 nm) with (200) preferred orientation. Films deposited at lower substrate temperature have smaller grains (about 55 nm) with (110) preferred orientation. The electrical resistivity decreases slightly with increasing film thickness but is more influenced by the deposition and annealing temperature. Maximum resistivity is 861 μΩ cm, observed for films deposited at room temperature on glass substrates. Minimum resistivity is 40 μΩ cm observed for a thin film (50 nm) deposited at 540°C on a quartz substrate. Micro-Raman investigations indicate that strain-free well-crystallized thin films are deposited on oxidized Si substrates.     

Preparation and characterization of radio-frequency-sputtered Ba2Si2TiO8 thin films

Radio-frequency-sputtered barium titanium silicate (BST, Ba₂Si₂TiO₈) thin films were grown on crystalline Si (100) substrates and were characterized using wavelength-dispersive spectrometry (WDS), X-ray diffraction (XRD), optical microscopy (OM) and scanning electron microscopy (SEM), and diagonal techniques for dielectric properties. The chemical compositions of the films increasingly deviated from stoichiometry with film thickness. At the initial stage of deposition the grain configuration is dependent on the Si substrate texture. XRD analysis indicates that the BST films deposited at an optimum substrate temperature of 845 °C were strongly c-axis oriented, and that the film orientation is manipulated by substrate temperature and supersaturation. The corresponding film-growth rate in the direction normal to the film surface at 845 °C was 1.95 nm min^–1 at the initial stage, and decreased with sputtering time. The as-deposited films have a room-temperature bulk resistivity of 1.8 ×10⁷ m in the direction of thickness and an isotropic surface resistivity of 1.5×10³ m. The high-frequency relative dielectric constant, 0.05 at frequencies higher than 9 MHz, is lower than that of many typical piezoelectric materials. The high-frequency impedance character is typical of piezoelectric materials, giving a minimum impedance frequency of 9.0 MHz and a serial resonant frequency at about 9.5 MHz.