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Showing papers in "Applied Physics A in 2008"


Journal ArticleDOI
TL;DR: In this paper, the authors investigated the effect of water absorption on the long-term silver ion release in polyamide/silver nanocomposites, and found that the longterm ion release increases with a growing diffusion coefficient of water in the polymer.
Abstract: Spherical silver nanoparticles were grown in situ in different polyamides by a thermal reduction of silver acetate during melt processing of the polymers. Most of the particles have a diameter of about 20 nm. The absolute amount as well as the kinetics of the silver ion release from the various polyamide/silver nanocomposites differ strongly, although the filler content in all materials is the same (1.5 wt. %) and the morphologies of the silver particles are not very different. One result of the investigations was that the absolute amount of the long-term silver ion release increases exponentially with the maximum water absorption of the polymers used as matrix materials, because silver ions are formed from elemental silver particles in the presence of water, only. Moreover, it was also found that the long-term silver ion release increases with a growing diffusion coefficient of water in the polymer. The water absorption properties of the polymers govern the kinetics of the silver ion release, too: for strong hydrophilic polyamides like PA6 or PA6.6, which are plasticized by water, the silver ion release is a zero-order process. For nanocomposites with less hydrophilic polyamides like a cycloaliphatic polyamide or a P12 modified with polytetrahydrofurane (PA12-poly-THF), the silver ion release is governed by diffusion. As expected from the efficacy of the silver ion release, PA6, PA6.6, PA12 and PA12 modified with polytetrahydrofurane and a cycloaliphatic polyamide filled with 1.5 wt. % of silver nanoparticles are active against Escherichia coli. But, only nanocomposites with PA6, PA6.6 and P12-poly-THF as matrix materials are suitable as long-term biocidal materials.

169 citations


Journal ArticleDOI
TL;DR: In this article, the current status of self-organized pattern formation and surface smoothing by low-energy ion-beam erosion of Si and Ge is summarized, and the most important experimental parameters that control these processes are discussed.
Abstract: Low-energy ion-beam sputtering, i.e. the removal of atoms from a surface due to the impact of energetic ions or atoms, is an inherent part of numerous surface processing techniques. Besides the actual removal of material, this surface erosion process often results in a pronounced alteration of the surface topography. Under certain conditions, sputtering results in the formation of well-ordered patterns. This self-organized pattern formation is related to a surface instability between curvature-dependent sputtering that roughens the surface and smoothing by different surface relaxation mechanisms. If the evolution of surface topography is dominated by relaxation mechanisms, surface smoothing can occur. In this presentation the current status of self-organized pattern formation and surface smoothing by low-energy ion-beam erosion of Si and Ge is summarized. In detail it will be shown that a multitude of patterns as well as ultra-smooth surfaces can develop, particularly on Si surfaces. Additionally, the most important experimental parameters that control these processes are discussed. Finally, examples are given for the application of low-energy ion beams as a novel approach for passive optical device engineering for many advanced optical applications.

154 citations


Journal ArticleDOI
TL;DR: In this article, a regular array of sharp nano-textured conical microstructures are formed on the titanium metal surface by irradiation with ultrafast laser pulses of 130 fs duration, 800 nm wavelength in vacuum (∼ 1 mbar) or in 100 mbar He.
Abstract: We report for the first time that a regular array of sharp nano-textured conical microstructures are formed on the titanium metal surface by irradiation with ultrafast laser pulses of 130 fs duration, 800 nm wavelength in vacuum (∼1 mbar) or in 100 mbar He. The microstructures are up to 25 μm tall, and taper to about 500 nm diameters at the tip. Irradiation in the presence of SF6, air or HCl creates a textured surface but does not create sharp conical microstructures. The surfaces of these microstructures exhibit periodic nano-texture of feature size comparable to the wavelength of light consistent with ripple formation. Contrary to pillar formation by femtosecond laser irradiation of silicon where the initial ripples evolve into the pillars and the ripples disappear, the ripples on titanium pillars have a much smaller periodicity than the pillars and remain on the surface of the pillars. The textured surface is pitch black compared to its original silver-grayish color, i.e, it exhibits greatly reduced reflectivity throughout the measured visible spectrum.

153 citations


Journal ArticleDOI
TL;DR: In this article, the s-component of the incident field, not attenuated by the projection, determines length and orientation of the ordered ripples, resulting in curved structures bending from polarization-controlled to defect-controlled orientation.
Abstract: In self-organized nanostructure formation upon femtosecond laser ablation, the laser polarization is an important control parameter. Experiments on fluoride crystals, using circular and elliptical polarization, study this influence in more detail. For circular polarization, spherical nanoparticles of about 100 nm diameter are formed. With increasing ellipticity, longer and longer ordered chains and linear structures are generated, oriented perpendicular to the long axis of the polarization ellipse. A similar effect occurs when, for circular polarization, the angle of incidence is varied from normal to 45°: the s-component of the incident field, not attenuated by the projection, determines length and orientation of the ordered ripples. However, surface defects like scratches exert an even stronger influence on the ripples orientation than the polarization, resulting in curved structures bending from polarization-controlled to defect-controlled orientation. Since the structure formation takes place only long after the end of the laser pulse, a certain electrical field memorizer is required to account for this polarization dependence. A promising approach assumes directional atomic surface diffusion anisotropies, arising, e.g. from plasmon-coupled metal–colloid arrays.

138 citations


Journal ArticleDOI
TL;DR: In this article, a comprehensive investigation based on X-ray fluorescence, Fourier transform infrared and UV-visible absorption and emission spectroscopies was carried out on 13 organic pigments derived from eight different natural sources.
Abstract: Naturally occurring dyes have been used to produce painting pigments, called lakes, by precipitation or adsorption of an organic dyestuff onto an insoluble inorganic substrate. Most natural dyes link to metal cations, by means of coordination bonds. The stable complexes formed precipitate together with solid amorphous hydrous aluminum oxide in alkaline solutions, yielding a hybrid material called a lake. Conventional chromatographic methods for lake analysis require dye extraction from the substrate; as a consequence, they do not provide any information about the organo-metallic complexes. In this work a comprehensive investigation based on X-ray fluorescence, Fourier transform infrared and UV–visible absorption and emission spectroscopies was carried out on 13 organic pigments derived from eight different natural sources. Three different kinds of substrate containing aluminum hydroxide were distinguished dependent on different preparation procedures. Information concerning the recipe and the dye composition was obtained by UV–visible spectroscopies. Dyes from different sources (animal or vegetal) could be distinguished. This study shows that the combined use of different spectroscopic techniques provides complementary information to high-performance liquid chromatography and therefore can be proposed for a molecular non-invasive investigation of these materials on works of art.

128 citations


Journal ArticleDOI
TL;DR: In this paper, the authors reported the deposition of 3-aminopropyltrimethoxysilane (APTMS) multilayers on SiOx/Si(p++) substrates by a layer-by-layer self-assembly process.
Abstract: We report the deposition of 3-aminopropyltrimethoxysilane (APTMS) multilayers on SiOx/Si(p++) substrates by a layer-by-layer self-assembly process. The multilayers were grafted in a glove box having nitrogen ambient with both humidity and oxygen contents <1 ppm using APTMS solutions prepared in an anhydrous toluene. Deposition of the multilayers has been carried out as a function of solution concentration and grafting time. Characterization of the multilayers using static de-ionized water contact angle, ellipsometry, X-rayphotoelectron spectroscopy and atomic force microscope measurements revealed that self-assembling of the multilayers takes place in two distinct stages: (i) the first APTMS monolayer chemisorbs on a hydroxylated oxide surface by a silanization process and, (ii) the surface amino group of the first monolayer chemisorbs the hydrolyzed silane group of other APTMS molecules present in the solution, leading to the formation of a bilayer. The second stage is a self-replicating process that results in the layer-by-layer self-assembly of the multilayers with trapped NH3 + ions. The current–voltage characteristics of the multilayers exhibit a hysteresis effect along with a negative differential resistance, suggesting their potential application in the molecular memory devices. A possible mechanism for the observed hysteresis effect based on filling and de-filling of the NH3 + acting as traps is presented.

125 citations


Journal ArticleDOI
TL;DR: In this paper, a lead-free nano-silver paste was used to connect silicon diode chips to copper bases at 350°C in nitrogen ambient without external pressure, and the resulting diode packages had electrical and thermal properties about equal to those with lead-solder joints.
Abstract: We propose a lead-free silver paste as a replacement for a high-temperature lead-rich solder used for electronics. The pastes tested here contain a small amount of solvent, but primarily consist of silver powder and alkoxide-passivated silver nanoparticles that undergo nanosintering when heated. The pastes were used to connect silicon diode chips to copper bases at 350°C in nitrogen ambient without external pressure. The resulting diode packages had electrical and thermal properties about equal to those with lead-solder joints. The mechanical strengths also were comparable to the lead joint. These properties make this nanosilver paste the first viable lead-free alternative to a lead solder.

124 citations


Journal ArticleDOI
TL;DR: In this article, the fabrication of graphitic microstructures in the bulk of chemical vapor deposited (CVD) diamond using 120-fs laser pulses at 800-nm wavelength is studied with Raman spectroscopy.
Abstract: We report the fabrication of graphitic microstructures in the bulk of chemical vapor deposited (CVD) diamond using 120-fs laser pulses at 800-nm wavelength. The nature of the laser-modified region and generation of mechanical stresses in the surrounding diamond is studied with Raman spectroscopy. A spontaneous growth of the laser-modified region from the focal plane towards the laser has been visualized in the process of multipulse irradiation with different pulse energies. The formation of discrete or continuous graphitized structures is revealed depending on the varied local laser intensity. The physical processes governing the appearance of separate graphitic globules and continuous extension of the graphitized region are discussed. Controlling the laser irradiation conditions permits us to fabricate graphitic wires with typical length of 150 μm and diameter of 1.5 μm. The longer, 300-ps pulses, as applied to laser microstructuring of the CVD diamond bulk, are found to be inappropriate due to the stronger influence of structural defects on the damage threshold, the noticeable fluctuation of the structure diameter over the length and the pronounced cracking of the surrounding diamond.

121 citations


Journal ArticleDOI
TL;DR: In this paper, a femtosecond laser-assisted method was proposed for the preparation of metal nanoparticles in clean, biologically friendly aqueous environment (green synthesis) and thus completely solved the toxicity problem.
Abstract: Inorganic nanoparticles offer novel promising properties for biological sensing and imaging, as well as in therapeutics. However, these applications are often complicated by the possible toxicity of conventional nanomaterials, arising as a result of inadequate purification procedures of nanoparticles obtained via synthetic pathways using toxic or non-biocompatible substances. We review novel femtosecond laser-assisted methods, which enable the preparation of metal nanomaterials in clean, biologically friendly aqueous environment (“green” synthesis) and thus completely solve the toxicity problem. The proposed methods, including laser ablation and fragmentation, make possible the production of stable metal colloids of extremely small size (∼2 nm) with a low coefficient of variation (15–25%). Those nanoparticles exhibit unique surface chemistry and can be used for bio-imaging, cancer treatment and nanoparticle-enhanced Raman spectroscopy.

118 citations


Journal ArticleDOI
TL;DR: In this article, the authors derived thermodynamically the free energy functional of a ferroelectric under an applied field E that contains the depolarization field Ed. They found that it is crucial to recognize the relationship between the total polarization and the applied field due to the degradations of the field, and that this relationship effectively double-counts the field and thus causes serious overestimation of its effects.
Abstract: We derived thermodynamically from first principles the free energy functional of a ferroelectric under an applied field E that contains the depolarization field Ed. We found that it is crucial to recognize the relationship between the total polarization and the applied field due to the depolarization field when expressing the free energy functional in the Landau form. Ad hoc formulations of ferroelectric models that overlooked this relationship effectively double-count the depolarization field, and thus cause serious overestimation of its effects. Examples are given in which the Curie temperature and the critical thickness of ferroelectricity, etc., can be overestimated this way by orders of magnitude.

115 citations


Journal ArticleDOI
TL;DR: In this paper, the number of pulses to drill through the sheet as a function of pulse length and energy was obtained by recording the intensity on a photodiode placed under the sample while drilling the holes, which was successfully predicted using a Gaussian approximation and a material removal fluence threshold of 0.39 J/cm2 for a pulse length of 150 fs.
Abstract: Deep laser holes were drilled in copper sheets using various pulse lengths and environments. By recording the intensity on a photodiode placed under the sample while drilling the holes, we obtained the number of pulses to drill through the sheet as a function of pulse length and energy. The entrance diameter of the holes was successfully predicted using a Gaussian approximation and a material removal fluence threshold of 0.39 J/cm2 for a pulse length of 150 fs. From cross sections of the holes, the morphology of the inside walls was observed and shows an increase in the amount of molten material with pulse length. A transition pulse length is defined as the point at which the laser affected material goes from being mainly vaporized to mainly melted. This transition occurs near ∼10 ps, which corresponds approximately to the electron–phonon relaxation time for copper.

Journal ArticleDOI
TL;DR: In this article, the dynamics of the laser-induced forward transfer (LIFT) of an aqueous solution through time-resolved imaging was investigated at conditions under which droplets are deposited on a receptor substrate.
Abstract: The dynamics of the laser-induced forward transfer (LIFT) of an aqueous solution is investigated through time-resolved imaging. The experiment is carried out at conditions under which droplets are deposited on a receptor substrate. The obtained images reveal that after an initial balloon-like stage, a uniform jet with a very long length and high aspect ratio is formed, which advances at constant speed until it finally becomes unstable and breaks into several droplets. This dynamics demonstrates that the deposition process of well-defined droplets through LIFT results from the contact of the liquid jet with the receptor substrate, and not from a flying droplet.

Journal ArticleDOI
TL;DR: In this article, a numerical model for a loose packing process of spherical particles is presented, which starts with randomly choosing a sphere according to a pregenerated continuous particle-size distribution, and then dropping the sphere into a dimension-specified box, and obtaining its final position by using dropping and rolling rules which are derived from a similar physical process of spheres dropping in the gravitational field to minimize its gravity potential.
Abstract: A numerical model for a loose packing process of spherical particles is presented. The simulation model starts with randomly choosing a sphere according to a pregenerated continuous particle-size distribution, and then dropping the sphere into a dimension-specified box, and obtaining its final position by using dropping and rolling rules which are derived from a similar physical process of spheres dropping in the gravitational field to minimize its gravity potential. Effects of three different particle-size distributions on the packing structure were investigated. Analysis on the physical background of the powder-based manufacturing process is additionally applied to produce optimal packing parameters of bimodal and Gaussian distributions to improve the quality of the fabricated parts. The results showed that higher packing density can be obtained using bimodal size distribution with a particle-size ratio from 1.5 to 2.0 and the mixture composition around n2:n1=6:4. For particle size with a Gaussian distribution, the particle radii should be limited in a narrow range around 0.67 to 1.5.

Journal ArticleDOI
TL;DR: In this article, the transition region width of nanowire heterojunctions and pn-junctions grown using vapor-liquid-solid (VLS) processes is modeled and the achievable width or abruptness of the junctions is attributed to the residual I atom/molecule stored in the liquid droplet at the onset of introducing II to grow the junction, and the stored I atom or molecule consumption into the subsequently grown crystal layers.
Abstract: The transition region width of nanowire heterojunctions and pn-junctions grown using vapor–liquid–solid (VLS) processes has been modeled. With two constituents or dopants I and II, the achievable width or abruptness of the junctions is attributed to the residual I atom/molecule stored in the liquid droplet at the onset of introducing II to grow the junction, and the stored I atom/molecule consumption into the subsequently grown crystal layers. The model yields satisfactory quantitative fits to a set of available Si-Ge junction data. Moreover, the model provides a satisfactory explanation to the relative junction width or abruptness differences between elemental and compound semiconductor junction cases, as well as a guideline for achieving the most desirable pn-junction widths.

Journal ArticleDOI
TL;DR: In this paper, a simple method for preparing stable super-hydrophobic surfaces by irradiating silicon wafers with femtosecond (fs) laser pulses and subsequently coating them with chloroalkylsilane monolayers is presented.
Abstract: Control over the wettability of solids and manufacturing of functional surfaces with special hydrophobic and self-cleaning properties has aroused great interest because of its significance for a vast range of applications in daily life, industry and agriculture. We report here a simple method for preparing stable superhydrophobic surfaces by irradiating silicon (Si) wafers with femtosecond (fs) laser pulses and subsequently coating them with chloroalkylsilane monolayers. It is possible, by varying the laser pulse fluence on the surface, to achieve control of the wetting properties through a systematic and reproducible variation of roughness at micro- and nano-scale which mimics both the topology of the “model” superhydrophobic surface—the natural lotus leaf—, as well as its wetting response. Water droplets can move along these irradiated superhydrophobic surfaces, under the action of small gravitational forces, and experience subsequent immobilization, induced by surface tension gradients. These results demonstrate the potential of manipulating liquid motion through selective laser patterning.

Journal ArticleDOI
Guang-Hui Xu1, Qiang Zhang1, Weiping Zhou1, Jia-Qi Huang1, Fei Wei1 
TL;DR: In this paper, the authors used vacuum filtration to fabricate a CNT/PVA film by penetrating PVA into the CNT paper, which showed an increase by 12 and 7, respectively, although the material's electrical conductivity was lowered to 0.16×104 S/m.
Abstract: This study sought to produce carbon nanotube (CNT) pulp out of extremely long, vertically aligned CNT arrays as raw materials. After high-speed shearing and mixing nitric acid and sulfuric acid, which served as the treatment, the researchers produced the desired pulp, which was further transformed into CNT paper by a common filtration process. The paper’s tensile strength, Young’s modulus and electrical conductivity were 7.5 MPa, 785 MPa and 1.0×104 S/m, respectively, when the temperature of the acid treatment was at 110°C. Apart from this, the researchers also improved the mechanical property of CNT paper by polymers. The CNT paper was soaked in polyethylene oxide, polyvinyl pyrrolidone, and polyvinyl alcohol (PVA) solution, eventually making the CNT/PVA film show its mechanical properties, which increased, while its electrical conductivity decreased. To diffuse the polymer into the CNT paper thoroughly, the researchers used vacuum filtration to fabricate a CNT/PVA film by penetrating PVA into the CNT paper. After a ten-hour filtration, the tensile strength and Young’s modulus of CNT/PVA film were 96.1 MPa and 6.23 GPa, respectively, which show an increase by factors of 12 and 7, respectively, although the material’s electrical conductivity was lowered to 0.16×104 S/m.

Journal ArticleDOI
TL;DR: In this article, the physical mechanisms responsible for the formation of nanobump structures on a surface of a thin metal film irradiated by a tightly focused femtosecond laser pulse are investigated in a large-scale molecular dynamics simulation.
Abstract: The physical mechanisms responsible for the formation of nanobump structures on a surface of a thin metal film irradiated by a tightly focused femtosecond laser pulse are investigated in a large-scale molecular dynamics simulation. The simulation is performed with a combined atomistic-continuum model adapted for an adequate representation of laser-induced processes at the length-scale of the entire laser spot. The relaxation of the compressive stresses generated by the fast laser heating is identified as the main driving force responsible for the separation of the metal film from the substrate and formation of the nanobump. The kinetics of the transient melting and resolidification, occurring under conditions of the fast cooling due to the two-dimensional electron heat conduction, defines the shape of the nanobump. The predictions of the simulation are related to the surface structures observed in femtosecond laser nanostructuring.

Journal ArticleDOI
TL;DR: In this paper, the combination of a chemical liquid jet and a laser beam is used for the microstructuring of silicon with the focus on etching, selective doping of phosphorous, and combination of etching and doping.
Abstract: Laser Chemical Processing (LCP) is presented as a novel microstructuring method for multiple applications. Via the combination of a chemical liquid jet and a laser beam, thermochemical and photochemical reactions can be initiated. Due to the free choice of the chemistry for the carrier liquid and the laser source, efficient processes can be devised for a large variety of applications. We present some examples for the microstructuring of silicon with the focus on etching, selective doping of phosphorous and the combination of etching and doping.

Journal ArticleDOI
TL;DR: In this paper, the authors present a technique to implant ions through a small hole in the tip of an atomic force microscope. But this technique is not suitable for the handling of small structures using different projectiles at kinetic energies between 0.5 and 5.0 keV.
Abstract: Decreasing structure sizes in both conventional and quantum solid state devices require novel fabrication methods: we present a technology which allows to implant ions through a small hole in the tip of an atomic force microscope. This technique offers a maskless addressing of small structures using different projectiles at kinetic energies between 0.5 and 5.0 keV. Our method aims to implant single atomic ions, molecular ions or charged nanoparticles with nm resolution. We test the method by implanting N+ ions into diamond and generating nitrogen-vacancy color centers. The system is operated with a conventional ion gun. However, in future we will employ an ion trap as a deterministic source of cold single ions.

Journal ArticleDOI
TL;DR: In this paper, a femtosecond laser with pulse duration of 172 fs, central wavelength of 780 nm, and repetition rate of 1 kHz is used to fabricate voids.
Abstract: We propose an idea of fast cutting a display glass plate where the sample is pre-processed micromachining single shot rear-surface and internal void arrays aligned on working plane prior to glass cleaving. Single shot void morphology is investigated varying input pulse energy, focusing depth, and scanning speed. A femtosecond laser with pulse duration of 172 fs, central wavelength of 780 nm, and repetition rate of 1 kHz is used to fabricate voids.

Journal ArticleDOI
Abstract: A new equation for calculating the electrical conductivity of sintered powder compacts is proposed. In this equation, the effective resistivity of porous compacts is a function of the fully dense material conductivity, the porosity of the compact and the tap porosity of the starting powder. The new equation is applicable to powder sintered compacts from zero porosity to tap porosity. A connection between this equation and the percolation conduction theory is stated. The proposed equation has been experimentally validated with sintered compacts of six different metallic powders. Results confirm very good agreement with theoretical predictions.

Journal ArticleDOI
TL;DR: In this article, selective laser sintering and ablation of inkjet-printed metal nanoparticles enables low-temperature metal deposition as well as high-resolution patterning.
Abstract: Inkjet direct writing of functional materials provides a promising pathway towards realization of ultra-low-cost, large-area printed electronics, albeit at the expense of lowered resolution (∼20–50 μm). We demonstrate that selective laser sintering and ablation of inkjet-printed metal nanoparticles enables low-temperature metal deposition as well as high-resolution patterning. Combined with an air-stable carboxylate-functionalized polythiophene, all-inkjet-printed and laser-processed organic field effect transistors with micron to submicron critical feature resolution were fabricated in a fully maskless sequence, eliminating the need for any lithographic processes. All processing and characterization steps were carried out at plastic-compatible low temperatures and in air under ambient pressure.

Journal ArticleDOI
TL;DR: In this article, a comparison of growth morphology evolution for pulsed laser deposition and thermal deposition in the same dual-use chamber under identical thermal, background, and surface preparation conditions, and varying the kinetic energy by varying the laser fluence or using an inert background gas was made.
Abstract: This paper reviews our recent studies of the fundamentals of growth morphology evolution in Pulsed Laser Deposition in two prototypical growth modes: metal-on-insulator island growth and semiconductor homoepitaxy. By comparing morphology evolution for pulsed laser deposition and thermal deposition in the same dual-use chamber under identical thermal, background, and surface preparation conditions, and varying the kinetic energy by varying the laser fluence or using an inert background gas, we have isolated the effect of kinetic energy from that of flux pulsing in determining the differences between morphology evolution in these growth methods. In each growth mode analytical growth models and Kinetic Monte Carlo simulations for thermal deposition, modified to include kinetic energy effects, are successful at explaining much of what we observe experimentally.

Journal ArticleDOI
TL;DR: In this article, a systematic study on the transport properties by varying the lithium oxide content of the garnet-based solid electrolyte Li5+xBaLa2Ta2O2O11.
Abstract: We report systematic studies on the transport properties by varying the lithium oxide content of the garnet-based solid electrolyte Li5+xBaLa2Ta2O11.5+0.5x (x=0, 0.50, 0.75, 1.00, 1.25, 1.50, 1.75, 2.00) for understanding the ionic conductivity dependence on the crystal lattice parameter and carrier concentration. Powder X-ray diffraction data of Li5+xBaLa2Ta2O11.5+0.5x (x=0, 0.50, 0.75, 1.00, 1.25, 1.50, 1.75, 2.00) indicate the existence of the garnet-like structure for any of the compositions. The cubic lattice parameter was found to increase with increasing x and reaches a maximum at x=1.00, then decreases slightly with a further increase in x. Impedance measurements obtained at 50 °C indicate a maximum of the grain-boundary resistance (Rgb) contribution to the total resistance (Rb+Rgb) at x=0.0 and a considerable decrease with increase in lithium concentration. The total (bulk + grain-boundary) and bulk ionic conductivity increase with increasing lithium content and reach a maximum at x=1.00 and then decrease slightly with further increase in x. Among the investigated compounds, Li6BaLa2Ta2O12 exhibits the highest total (bulk + grain-boundary) and bulk ionic conductivity of 1.5×10-4 and 1.8×10-4 S/cm at 50 °C, respectively. The results obtained in the present investigation of the Li5+xBaLa2Ta2O11.5+0.5x (x=0–2) series clearly revealed that the lithium content plays a major role in decreasing the grain boundary resistance contribution to the total resistance and also in increasing the ionic conductivity of the garnet-like compound.

Journal ArticleDOI
TL;DR: In this article, two archaeological glass productions opacified with calcium and lead antimonates are studied in order to rediscover ancient opaque glass technologies: Roman mosaic tesserae and Nevers lampworking glass.
Abstract: The aim of the study is to understand how antimonate opacifying crystals were obtained throughout history. Two archaeological glass productions opacified with calcium and lead antimonates are studied in this paper, in order to rediscover ancient opaque glass technologies: Roman mosaic tesserae (1st cent. B.C.–4th cent. A.D.) and Nevers lampworking glass (18th cent. A.D.). The fine examination of crystalline phases and of the vitreous matrix is undertaken using various and complementary techniques. Results are compared with a modern reference production, for which the technological process is well known. We demonstrate that Ca-antimonate opacifiers in Roman mosaic tesserae, as well as in Nevers lampworking glass, were obtained by in situ crystallization. Nevertheless, Roman and Nevers glass would have undergone different firing processes. We propose that the addition of previously synthesized crystals or the use of “anime” could be the process used to obtain Pb-antimonate opacified glass, for both productions studied. We demonstrate that CaO, PbO and Sb2O3 concentrations in the bulk compositions and in the matrices, and their evolution with the crystallinity ratio, offer robust criteria for the distinction of the opacification process used. Also, the different crystalline structures help to provide information on the experimental conditions.

Journal ArticleDOI
TL;DR: In this paper, the authors used electron transmission microscopy techniques to locate the nanoparticles, which were then characterized using EDS and HRTEM, using the HAADF (Z contrast) technique.
Abstract: We biosynthesized iron oxide nanoparticles with four different pH in the solution to see its influence in the oxides obtained. This method allowed for generating aggregates of 1–10 nm, and under optimal conditions (pH=10) we could control the size in the range of 1–4 nm. With the purpose to analyze the biosynthesized iron oxide clusters we employed electron transmission microscopy techniques. Because the biosynthetic method with alfalfa has been used, the presence of the biomass, which is dense and within which are contained the nanoparticles, makes their observation difficult. Using the HAADF (Z contrast) technique it is possible to locate the nanoparticles, which are then characterized using EDS and HRTEM.

Journal ArticleDOI
TL;DR: In this paper, the relationship between the process parameters and the resulting film morphology, structure and properties for PLD performed with an alumina target in a background oxygen atmosphere is investigated, and three distinct growth regimes are found, leading to compact homogeneous films, columnar structures and open microstructures.
Abstract: Alumina is technologically exploited in several forms, ranging from compact hard films as protective coatings to open microstructures of high specific area as supports for catalysts. Currently, various production processes are used to deposit the different forms. PLD has the potential of obtaining not only the different forms, but also a continuous modulation of properties, by tuning of the process parameters. This work investigates the relationship between the process parameters and the resulting film morphology, structure and properties for PLD performed with an alumina target in a background oxygen atmosphere. Three distinct growth regimes are found, leading, respectively, to compact homogeneous films, columnar structures and open microstructures. These structures are quantitatively characterized, and the ranges of the process parameters corresponding to the three regimes are identified. An empirical scaling law is proposed, which can be exploited as a guide for the design of growth processes aimed at obtaining specific film properties.

Journal ArticleDOI
TL;DR: In this paper, the authors analyzed the feasibility of artificial neural networks (ANN) for the classification, in function of the provenance, of archaeological ceramics Terra Sigillata analyzed by means of laser-induced breakdown spectroscopy.
Abstract: The aim of this work is to analyze the feasibility of artificial neural networks (ANN) for the classification, in function of the provenance, of archaeological ceramics Terra Sigillata analyzed by means of laser-induced breakdown spectroscopy (LIBS). In order to automate and facilitate the task of comparison of LIBS spectra, two ANN algorithms are proposed: One is fed with the whole LIBS spectra and the other with the areas of the most intense peaks of the spectra. In both cases, an analysis of the network architecture as a function of the number of hidden neurons and number of epochs of training was carried out in order to optimize the performance of the network. Following both procedures, the correct classification (higher than the 95% of success) of Terra Sigillata pieces from their LIBS spectra can be achieved in a systematic and objective way.

Journal ArticleDOI
TL;DR: In this article, single shot structures at the surface of fused silica as a function of fluence and pulse shape were analyzed with the help of scanning electron microscopy, and different thresholds for surface material modification with respect to an asymmetric pulse and its time reversed counterpart were attributed to control of different ionization processes.
Abstract: Laser material processing of dielectrics with temporally asymmetric femtosecond laser pulses of identical fluence, spectrum, and statistical pulse duration is investigated experimentally. To that end single shot structures at the surface of fused silica as a function of fluence and pulse shape are analyzed with the help of scanning electron microscopy. Structures for the bandwidth limited pulses show the known expansion in structure size with increasing laser fluence approaching the diffraction limit, which is 1.4 μm for the 0.5NA microscope objective used. In contrast, structures from the asymmetric pulses are remarkably stable with respect to variations in laser fluence and stay below 300 nm despite doubling the fluence. Different thresholds for surface material modification with respect to an asymmetric pulse and its time reversed counterpart are attributed to control of different ionization processes.

Journal ArticleDOI
TL;DR: In this paper, single-pulse laser-Induced Breakdown Spectroscopy (LIBS) and Laser-Ablation Inductively Coupled Plasma Mass-Spectrometry (LA-ICP-MS) were applied for mapping the silver and copper distribution in Helianthus Annuus L.
Abstract: Single-pulse Laser-Induced Breakdown Spectroscopy (LIBS) and Laser-Ablation Inductively Coupled Plasma Mass-Spectrometry (LA-ICP-MS) were applied for mapping the silver and copper distribution in Helianthus Annuus L. samples treated with contaminant in controlled conditions. For Ag and Cu detection the 328.07 nm Ag(I) and 324.75 nm Cu(I) lines were used, respectively. The LIBS experimental conditions (mainly the laser energy and the observation window) were optimized in order to avoid self-absorption effect in the measured spectra. In the LA-ICP-MS analysis the Ag 107 and Cu 63 isotopes were detected. The capability of these two analytical techniques for high-resolution mapping of selected trace chemical elements was demonstrated.