Alexandre Boulle

Characterization and modelling of the ion-irradiation induced disorder in 6H-SiC and 3C-SiC single crystals

6H-SiC and 3C-SiC single crystals were simultaneously irradiated at room temperature with 100 keV Fe ions at fluences up to 4 × 1014 cm−2 (~0.7 dpa), i.e. up to amorphization. The disordering behaviour of both polytypes has been investigated by means of Rutherford backscattering spectrometry in the channelling mode and synchrotron x-ray diffraction. For the first time, it is experimentally demonstrated that the general damage build-up is similar in both polytypes. At low dose, irradiation induces the formation of small interstitial-type defects. With increasing dose, amorphous domains start to form at the expense of the defective crystalline regions. Full amorphization of the irradiated layer is achieved at the same dose (~0.45 dpa) for both polytypes. It is also shown that the interstitial-type defects formed during the first irradiation stage induce a tensile elastic strain (up to ~4.0%) with which is associated an elastic energy. It is conjectured that this stored energy destabilizes the current defective microstructure observed at low dose and stimulates the formation of the amorphous nanostructures at higher dose. Finally, the disorder accumulation has been successfully reproduced with two models (namely multi-step damage accumulation and direct-impact/defect-stimulated). Results obtained from this modelling are compared and discussed in the light of experimental data.

A high-resolution X-ray diffractometer for the study of imperfect materials

A high-resolution X-ray diffractometer devoted to the study of imperfect materials (mainly oxides and ceramics) is presented. It is based on a rotating anode generator, a four-bounce monochromator, a five-movement sample holder and a curved position-sensitive detector (PSD). This setup allows rapid acquisition of a reciprocal-space map (in less than 10 h) even for very poorly diffracting materials. The two-dimensional instrumental profile is calculated taking into account each optical element in the beam path. The one-dimensional instrumental profiles corresponding to widely used scans (ω scan, θ–2θ scan, rocking curve and powder scan) are also calculated. In the three former cases, the setup exhibits an excellent angular resolution (0.003°), whereas in the latter case the resolution is lowered by one order of magnitude at the benefit of a strong increase in the collected intensity. The possibilities of this diffractometer are illustrated with three examples: an epitaxic layer, a microstructured single crystal and a powder.

Optical properties of an epitaxial Na0.5Bi0.5TiO3 thin film grown by laser ablation: Experimental approach and density functional theory calculations

This study reports on the determination of the optical constants of a lead-free ferroelectric material, Na0.5Bi0.5TiO3. The optical transmission measurements were carried out in the 300–3000 nm wavelength range, on a (100)-oriented Na0.5Bi0.5TiO3 thin film, epitaxially grown by laser ablation on a (100)MgO single crystal substrate. Applying the “method of the envelopes,” developed by Manifacier et al. [J. Phys. E 9, 1002 (1976)] and by Swanepoel [J. Phys. E 16, 1214 (1983)], the analysis of the observed interference fringes allowed extracting some optical data for Na0.5Bi0.5TiO3, namely the linear refractive and extinction indices n and k, the absorption coefficient α, and as well the nature (direct or indirect transition) and value of the optical band gap. It was found that n∞=2.321 and the transmission data suggested a 3.30 eV indirect transition. Our experimental results are thus in opposition to the few data reported so far for Na0.5Bi0.5TiO3, where a direct transition was evoked. Therefore, we have c...

Effect of tensile and compressive strains on the transport properties of SmNiO3 layers epitaxially grown on (001) SrTiO3 and LaAlO3 substrates

This paper deals with the role of epitaxial strain on the structure and electronic transport properties of metastable SmNiO3 layers grown by metal-organic chemical vapor deposition onto SrTiO3 and LaAlO3 substrates. The characterization of these layers is carried out by high resolution x-ray diffraction and four-probe resistivity measurements. It is found that the SmNiO3 phase is stabilized by in-plane compressive strain whereas in-plane tensile strain induces the creation of oxygen vacancies that induces an annihilation of the metal-insulator transition and a huge increase of the resistivity.

Phenomenological analysis of heterogeneous strain fields in epitaxial thin films using x-ray scattering

A model that allows the quantitative analysis of heterogeneous strain fields in epitaxial thin films using x-ray diffraction (XRD) is presented. Particular emphasis is laid on the modelling of the two-component XRD profiles (i.e. profiles made of the superposition of a narrow coherent Bragg peak and a broad diffuse scattering profile) encountered in the XRD investigation of epitaxial thin films containing localized strain fields. The spatial properties of the strain field are included in a correlation function based on phenomenological parameters such as the defect correlation length ξ and the level of disorder σ∞. No assumption regarding the nature of the defect is hence required. The statistical properties of the strain field are described by means of Levy-stable distributions which allow us to account for profile shapes ranging between the Gaussian and profiles exhibiting pronounced power law-type tails, as well as for asymmetrical profiles. The effects of finite size of the domains (crystallites) over which diffraction is coherent are rigorously taken into account by calculating the auto-correlation function of the crystallite shape including the size distribution effects. The effects of each parameter are presented and discussed in detail and the applicability of the model is illustrated with two examples.

X-ray diffuse scattering from stacking faults in thick 3C-SiC single crystals

Stacking faults in thick (001)- and (111)-oriented 3C-SiC single crystals are studied by high resolution x-ray diffraction. The authors demonstrate that the analysis of the diffuse scattering intensity distribution can be used as a nondestructive means to accurately determine the densities of Shockley-type stacking faults. The diffuse scattering intensity is simulated with a scattering model based on a difference-equation description of faulting in fcc materials. It is shown that the (001) SiC crystals exhibit an anisotropic fault distribution, whereas the (111) SiC crystals exhibit an isotropic fault distribution, in excellent quantitative agreement with transmission electron microscopy observations.

Reciprocal-space mapping of epitaxic thin films with crystallite size and shape polydispersity

A development is presented that allows the simulation of reciprocal-space maps (RSMs) of epitaxic thin films exhibiting fluctuations in the size and shape of the crystalline domains over which diffraction is coherent (crystallites). Three different crystallite shapes are studied, namely parallelepipeds, trigonal prisms and hexagonal prisms. For each shape, two cases are considered. Firstly, the overall size is allowed to vary but with a fixed thickness/width ratio. Secondly, the thickness and width are allowed to vary independently. The calculations are performed assuming three different size probability density functions: the normal distribution, the lognormal distribution and a general histogram distribution. In all cases considered, the computation of the RSM only requires a two-dimensional Fourier integral and the integrand has a simple analytical expression, i.e. there is no significant increase in computing times by taking size and shape fluctuations into account. The approach presented is compatible with most lattice disorder models (dislocations, inclusions, mosaicity, ...) and allows a straightforward account of the instrumental resolution. The applicability of the model is illustrated with the case of an yttria-stabilized zirconia film grown on sapphire.

X-Ray diffraction line broadening by stacking faults in SrBi2Nb2O9/SrTiO3 epitaxial thin films

Abstract SrBi 2 Nb 2 O 9 thin films were deposited on (001) SrTiO 3 substrate by sol–gel spin coating. A previous study showed that the film crystallizes with the c -axis normal to the surface. Those epitaxial films are studied by means of X-ray diffraction (XRD) line profile analysis as a function of thermal annealing duration. The line profile analysis of the diffraction patterns collected in ω-2θ scan mode, gives detailed information on the coherently diffracting domain size and microstrains along a given direction. For low annealing duration the width of the (001) diffraction lines reaches values of approximately 1°. In accordance with a recent study, integral breadth and Fourier analysis suggest the presence of stacking faults separated by a mean distance of 5 nm. The profiles exhibit a marked Lorentzian character as expected from a faulted crystal. In addition to faulting, both finite grain size and microstrains contribute to the observed width. When heat treatment time is increased, the breadth and Lorentzian content of the (001) diffraction lines decrease attesting that the stacking fault density is lowered. For a 500-h treatment at 700°C the calculated domain size equals the films thickness. This indicates that stacking faults have almost disappeared: the SBN crystallites of the film have reached an equilibrium state.

Highly localized strain fields due to planar defects in epitaxial SrBi2Nb2O9 thin films

Thin films of (00l) oriented SrBi2Nb2O9 epitaxially grown on SrTiO3 by sol-gel spin coating have been studied by means of high-resolution x-ray diffraction reciprocal space mapping. It is shown that these materials contain highly localized heterogeneous strain fields due to imperfect stacking faults (i.e., faults that do not propagate throughout the crystallites building up the film). In the film plane, the strain fields are confined to 11 nm wide regions and characterized by a vertical displacement of 0.18c (where c is the cell parameter) showing that the stacking faults are mainly composed of one additional (or missing) perovskite layer. Prolonged thermal annealing at 700 °C strongly reduces the density of stacking faults and yields a more uniform strain distribution within the film volume without inducing significant grain growth.

A new method for the determination of strain profiles in epitaxic thin films using X-ray diffraction

A new and versatile method is proposed for the determination of strain profiles in epitaxic thin films. It is based on the simulation of the X-ray diffraction (XRD) profiles using cubic B-spline functions to model the vertical lattice displacement profile. The lattice displacement profile, and consequently the strain profile, directly results from a least-square fit of the model to the experimental XRD profiles. No a priori assumption is made regarding the shape of the strain profile. Moreover, as spline functions are used, the recovered lattice displacement profile is smooth and exhibits a minimum curvature, thus avoiding oscillating or saw-toothed unphysical solutions. The potential of this method is illustrated with (100) yttria-stabilized zirconia epitaxic thin films deposited onto (11\bar{2}0) sapphire substrates by sol–gel processing.