P.-O. Renault

Measuring thin film and multilayer elastic constants by coupling in situ tensile testing with x-ray diffraction

A direct determination of the Young’s modulus and the Poisson’s ratio in a 140 nm polycrystalline tungsten thin film deposited by ion-beam sputtering on a polyimide substrate has been performed by coupling x-ray diffraction measurements with in situ tensile testing. The method described in this article to extract the Young’s modulus of thin films from the evolution of the sin2 ψ curves as a function of applied load only requires to know the substrate Young’s modulus. The determination of the thin film Poisson’s ratio can be realized without knowing any of the substrate elastic constants. In the case of the tungsten thin film, the obtained Young’s modulus was close to the bulk material one whereas the Poisson’s ratio was significantly larger than the bulk one.

Size effect on intragranular elastic constants in thin tungsten films

The size effect on the elastic constants of nanocrystalline tungsten has been investigated in the case of W/Cu multilayers with two modulation wavelengths (3.1 and 24.0 nm). Tungsten Young’s modulus and Poisson’s ratio have been measured thanks to a technique coupling x-ray diffraction with in situ tensile testing. It is demonstrated that the in-grain thin film elastic constants are highly microstructure—sensitive: in the “3.1 nm” multilayer, tungsten Poisson’s ratio is larger than the bulk one while it is smaller in the “24.0 nm” multilayer; a softening of tungsten Young’s modulus is evidenced in the case of the specimen with the smallest period.

Plasticity of multiscale nanofilamentary Cu/Nb composite wires during in situ neutron diffraction: Codeformation and size effect

In situ neutron diffraction was performed on Cu∕Nb nanocomposite wires composed of a multiscale Cu matrix embedding Nb nanofilaments with a diameter of 267nm and spacing of 45nm. The evolution of elastic strains and peak profiles versus applied stress evidenced the codeformation behavior with different elastic-plastic regimes: the Cu matrix exhibit size effect in the finest channels while the Nb nanowhiskers remain elastic up to the macroscopic failure, with a strong load transfer from the Cu matrix onto the Nb filaments. The measured yield stress in the finest Cu channels is in agreement with calculations based on a single dislocation regime.

Poisson’s ratio measurement in tungsten thin films combining an x-ray diffractometer with in situ tensile tester

A direct determination of the Poisson’s ratio in 150 nm polycrystalline tungsten thin films deposited by ion-beam sputtering on Duralumin substrates has been performed by combining x-ray diffraction measurements with in situ traction on the sample. X-ray diffraction experiments using the sin2 ψ method have been done at LURE, the French synchrotron facility (Orsay, France) on a four-circle diffractometer. The method described in this letter allows us to extract in a simple way and with a good precision the Poisson’s ratio of thin films on substrates from the evolution of the sin2 ψ curves as a function of applied strains. In the case of tungsten thin film, the value obtained is close to the bulk material one.

Pvd grown (Ti, Si, Al)N nanocomposite coatings and (Ti, Al)N/(Ti, Si)N multilayers: structural and mechanical properties

Abstract In the last few years a considerable effort has been undertaken in order to optimise the production techniques of thin films and improve their quality. In this work, nanocomposite films resulting from Si additions to a (Ti,Al)N matrix have been prepared by RF and/or DC magnetron sputtering, with deposition rates varying from 0.21 μm/h to 4.6 μm/h. Rutherford Backscattering (RBS) and Electron Microprobe Analysis (EMPA) were used in order to access the chemical composition as well as the density of the films. For samples prepared with low deposition rates (deposited by a combination of RF and DC reactive magnetron sputtering) both symmetric and asymmetric XRD scans showed the development of crystalline phases whose structure is very similar to that of bulk TiN. The peak positions revealed changes of the lattice parameter from 0.420 to 0.428 nm with an increase of Si content dependent on the deposition rate. The lowest lattice parameter corresponds to a Ti–Si–Al–N phase where some of the Si and Al atoms are occupying Ti positions in the f.c.c. TiN lattice, while the highest lattice parameter corresponds to a system where at least a partial Si segregation can be enough to nucleate and develop the Si 3 N 4 phase that forms a layer on the growth surface, covering the (Ti,Al)N nanocrystallites and limiting their growth. As for the (Ti,Al,Si)N crystalline texture evolution, a (111) preferential growth for (Ti,Al)N and for low Si content was observed, while at intermediate Si content the texture changed to (200). With the increase of the Si content there is a corresponding decrease in the size of the diffracting grains. For samples prepared with high deposition rates (DC sputtered samples) High-Resolution Transmission Electron Microscopy (HRTEM) micrographs revealed a columnar growth associated with the f.c.c.-type structure of both phases. Small crystallites with sizes between ±7 and ±10 nm were observed. The use of (Ti,Al) and (Ti,Si) targets, relatively high deposition rates and an alternate deposition resulted in a multilayer of (Ti,Si)N/(Ti,Al)N. This system was produced with modulation periods between 5 and 10 nm, as shown by HR-TEM results, when the samples were grown with a deposition rate between 2 and 4.6 μm/h, respectively. Their average ultramicrohardness can be as high as 50 GPa. The residual stress values for the multilayer system are significantly lower than that of (Ti,Si,Al)N nanocomposite coatings.

Oxidation of phosphated iron powders

The present work deals with the influence of phosphating treatment on the oxidation resistance of iron powders. Iron powders with particles diameter size of approximately 100 μm, have been immersed in phosphoric acid (0.102 mol l−1) in an acetone solution. After half an hour, a phosphate layer of less than 0.1 μm is formed at the metal surface. XRD spectrum is characteristic of an amorphous or nanocrystalline coating. The oxidation is performed by in situ thermogravimetric experiments in artificial air (20% O2–80% N2). For oxidation times of 24 or 48 h, between 350 and 700°C the kinetics are recorded for both untreated and phosphated powders. At all temperatures, the phosphate acts as a protective barrier layer. Between 350 and 450°C the coated powders present two parabolic stages in their oxidation kinetics and progressively with increasing temperature, the first stage disappears. On the other hand, uncoated iron powders show only one parabolic stage when oxidised. The oxidation constants kp were plotted for each stage of the curves vs. 1/T. From each Arrhenius plot an activation energy is deduced. For the phosphated powders, an activation energy of less than 0.6 eV is found in the first stage while for the second stage the deduced value of approximately 1.8 eV is the same that for the uncoated iron. That second parabolic stage for the coated powders can be compared with the oxidation of cast iron while in the first stage another mechanism may be involved. XRD studies of the oxidised powders at 350°C for 48 h show that Fe3O4 and Fe2O3 are formed both on uncoated iron and on the coated powder. For phosphated powders, the amount of oxide is less important. As a result the phosphate layer acts as a diffusion barrier that slows down the oxidation of iron.

Measurement of the elastic constants of textured anisotropic thin films from x-ray diffraction data

The elastic constants (compliances sij) of a textured anisotropic thin film deposited on a substrate have been determined. Using x-ray diffraction to measure the intragranular strain and a tensile machine to deform in situ the samples, an analytical method is described and has been developed for fiber textured thin films. The determination of thin film compliances only requires the knowledge of the substrate elastic constants. In the case of a 260-nm-thin gold film, the compliances were found to be slightly different from the corresponding bulk material ones.

In situ diffraction strain analysis of elastically deformed polycrystalline thin films, and micromechanical interpretation

In situ tensile tests have been carried out under synchrotron radiation on supported gold (Au) thin films exhibiting a pronounced crystallographic texture. The 2θ shift of X-ray diffraction lines has been recorded for different specimen orientations and several loading levels in the elastic domain. The data obtained demonstrate the large strain heterogeneities generated within the specimen because of the intergranular interactions associated with the large elastic anisotropy of Au grains. To interpret these results, the use of a multi-scale micromechanical approach is unavoidable. The theoretical background of such methods is described, and the points where exact results can be obtained and where approximations have to be introduced are highlighted. It is shown that the Vook–Witt model, for which a general formulation is provided, is the exact solution for polycrystals exhibiting a laminate microstructure, which is a significant departure from the standard thin-film microstructures. Among several standard models used in the field, the self-consistent model is the only one that reproduces the experimental data correctly. This is achieved by accounting for the actual crystallographic texture of the specimen, and assuming pancake-shaped two-point statistics for the morphological texture. A discussion of the limitations of this approach, originally developed for bulk materials, is given for the specific case of thin films.

Development of a synchrotron biaxial tensile device for in situ characterization of thin films mechanical response

We have developed on the DIFFABS-SOLEIL beamline a biaxial tensile machine working in the synchrotron environment for in situ diffraction characterization of thin polycrystalline films mechanical response. The machine has been designed to test compliant substrates coated by the studied films under controlled, applied strain field. Technological challenges comprise the sample design including fixation of the substrate ends, the related generation of a uniform strain field in the studied (central) volume, and the operations from the beamline pilot. Preliminary tests on 150 nm thick W films deposited onto polyimide cruciform substrates are presented. The obtained results for applied strains using x-ray diffraction and digital image correlation methods clearly show the full potentialities of this new setup.

Damage mode tensile testing of thin gold films on polyimide substrates by X-ray diffraction and atomic force microscopy

Abstract In situ tensile testing has been performed on thin gold film, 320 nm thick, deposited on polyimide substrates. During the tensile testing, strain/stress measurements have been carried out by X-ray diffraction using the d-sin 2 ψ method. The X-ray stress analysis suggests crack formation in the films for stresses greater than 670 MPa. The surface of the deformed specimen observed by atomic force microscopy (AFM) exhibits both cracks and two types of straight-sided buckling patterns lying perpendicular to the tensile axis. These buckling patterns can have a symmetrical or asymmetrical shape. The evolution of these two kinds of buckling structures under tensile stress has been observed in situ by AFM and compared to X-ray stress data. The results indicate that symmetrical straight-sided buckling patterns are induced by the compressive stress during unloading, whereas the asymmetrical result from the delamination of the film during the tensile deformation.