Pulsed Laser Deposition allows to obtain W and W-Ta alloy coatings with different nanostructures, monitored by X-ray diffraction. The correlation between such structures and the elastic properties is investigated for amorphous-like, ultra-nano-and nano-crystalline coatings obtained by tuning the gas pressure during deposition, annealing temperature and Ta concentration. The full elastic characterization is achieved by surface Brillouin spectroscopy, interpreted by isotropic and anisotropic film models. Amorphous like coatings are obtained with He pressures of tens of Pa. In comparison with bulk W, they have lower stiffness, by about 60%, closely correlated to the mass density (lower by about 40%). In the nanocrystalline regime the stiffness is more correlated to the average grain size, approaching the bulk values for increasing crystallite size. Vacuum annealing of amorphous like coatings leads to the nucleation of ultra-nano crystalline seeds, embedded in an amorphous matrix with intermediate values for mass density and stiffness. Here, the stiffness results from an interplay between the crystal size and the density. Alloying with Ta leads to properties which are consistent with the lever rule in the nanocrystalline regime, and deviate from it when the higher Ta concentration, interfering with crystal growth, induces an ultra-nano crystalline structure.
Micron-thick boron films have been deposited by Pulsed Laser Deposition in vacuum on several substrates at room temperature. The use of high energy pulses (>700 mJ) results in the deposition of smooth coatings with low oxygen uptake even at base pressures of 10 -4 -10 -3 Pa. A detailed structural analysis, by X-Ray Diffraction and Raman, allowed to assess the amorphous nature of the deposited films as well as to determine the base pressure that prevents boron oxide formation. In addition the crystallization dynamics has been characterized showing that film crystallinity already improves at relatively low temperatures (800 °C). Elastic properties of the boron films have been determined by Brillouin spectroscopy. Finally, micro-hardness tests have been used to explore cohesion and hardness of B films deposited on aluminum, silicon and alumina. The reported deposition strategy allows the growth of reliable boron coatings paving the way for their use in many technology fields.
Metallic amorphous tungsten-oxygen and amorphous tungsten-oxide films, deposited by Pulsed Laser Deposition, are characterized. The correlation is investigated between morphology, composition, and structure, measured by various techniques, and the mechanical properties, characterized by Brillouin Spectroscopy and the substrate curvature method. The stiffness of the films is correlated to the oxygen content and the mass density. The elastic moduli decrease as the mass density decreases and the oxygen-tungsten ratio increases. A plateau region is observed around the transition between the metal-like (conductive and opaque) films and the oxide ones (non conductive and transparent). The compressive residual stresses, moderate stiffness and high local ductility of compact amorphous tungsten-oxide films are interesting for applications involving thermal or mechanical loads. The coefficient of thermal expansion is quite high (8.9 · 10 −6 K −1 ), being strictly correlated to the amorphous structure and stoichiometry of the films. Upon thermal treatments the coatings show a quite low relaxation temperature of 450 K. Starting from 670 K, they crystallize into the γ monoclinic phase of WO 3 , the stiffness increasing by about 70%. The measured thermomechanical properties provide a guidance for the design of devices which include a tungsten based layer, in order to assure their mechanical integrity. mitigating or favoring crack formation. Similarly, in high temperature applications, a significant mismatch between the coefficients of thermal expansion of the coating and of the substrate can induce high interface stresses, with possible coating delamination and device failure. More specifically, in an electrochromic system the W oxide film is part of a complex multilayer system: it is deposited on a transparent conductor, like ITO, and faces the electrolyte, solid or liquid, containing the ions responsible of the electrochromic effect, and can be subject to various and very different stress states [15]. Moreover, in some applications (e.g. solar-cells, thermophotovoltaic) tungsten oxide coatings operate at temperatures above room temperature [16]; this could induce phase transition or recrystallization, with a consequent variation of the as-deposited properties. Although the thermomechanical properties of tungsten based coatings can be crucial for the design of devices which exploit them, relatively fewer studies have investigated the relationship between their nanostructure, composition and mechanical properties [17,18,19]. The goal of this work is to achieve a more comprehensive understanding of the effects of structure, morphology and chemical composition on the thermomechanical properties of different systems of amorphous W-O and WO x coatings, providing useful results for the design of devices. We investigate amorphous films characterized by different oxygen/tungsten ratios and morphologies. To produce them we selected the Pulsed Laser Deposition (PLD) technique, which allows a significant versatility in tailoring the str...
In this work, we exploit nanosecond laser irradiation as a compact solution for investigating the thermomechanical behavior of tungsten materials under extreme thermal loads at the laboratory scale. Heat flux factor thresholds for various thermal effects, such as melting, cracking and recrystallization, are determined under both single and multishot experiments. The use of nanosecond lasers for mimicking thermal effects induced on W by fusionrelevant thermal loads is thus validated by direct comparison of the thresholds obtained in this work and the ones reported in the literature for electron beams and millisecond laser irradiation. Numerical simulations of temperature and thermal stress performed on a 2D thermomechanical code are used to predict the heat flux factor thresholds of the different thermal effects. We also investigate the thermal effect thresholds of various nanostructured W coatings. These coatings are produced by pulsed laser deposition, mimicking W coatings in tokamaks and W redeposited layers. All the coatings show lower damage thresholds with respect to bulk W. In general, thresholds decrease as the porosity degree of the materials increases. We thus propose a model to predict these thresholds for coatings with various morphologies, simply based on their porosity degree, which can be directly estimated by measuring the variation of the coating mass density with respect to that of the bulk.
The in plane coefficient of thermal expansion (CTE) and the residual stress of nanostructured W based coatings are extensively investigated. The CTE and the residual stresses are derived by means of an optimized ad-hoc developed experimental setup based on the detection of the substrate curvature by a laser system. The nanostructured coatings are deposited by Pulsed Laser Deposition. Thanks to its versatility, nanocrystalline W metallic coatings, ultra-nano-crystalline pure W and W-Tantalum coatings and amorphous-like W coatings are obtained. The correlation between the nanostructure, the residual stress and the CTE of the coatings are thus elucidated. We find that all the samples show a compressive state of stress that decreases as the structure goes from columnar nanocrystalline to amorphous-like. The CTE of all the coatings is higher than the one of the corresponding bulk W form. In particular, as the grain size shrinks, the CTE increases from 5
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