There is considerable controversy about swift heavy ion (SHI) irradiation induced displacive phase transitions in thermally insulating oxides. We present here unambiguous evidence for tetragonal to monoclinic and rhombohedral to monoclinic phase transitions in BaTiO3 under swift heavy ion irradiation (120MeV 108Ag+9 ions) using in-situ x-ray powder diffraction (XRPD) studies. The anomalous splitting/broadening of 111/222pc, 200pc and 220pc pseudocubic peaks for fluences greater than 3*1012 ions/cm2 reveal structural changes before amorphization at higher fluences. Lebail analysis of XRPD profiles confirm that the monoclinic phase is of MA type in the Cm space group. Shear stress for the structural phase transition is estimated to be ~ 430MPa, which we believe is generated as a result of stopping of the SHI.
The high energy density of electronic excitations due to the impact of swift heavy ions can induce structural modifications in materials. We present a X-ray diffractometer called ALIX, which has been set up at the low-energy IRRSUD beamline of the GANIL facility, to allow the study of structural modification kinetics as a function of the ion fluence. The X-ray setup has been modified and optimized to enable irradiation by swift heavy ions simultaneously to X-ray pattern recording. We present the capability of ALIX to perform simultaneous irradiation - diffraction by using energy discrimination between X-rays from diffraction and from ion-target interaction. To illustrate its potential, results of sequential or simultaneous irradiation - diffraction are presented in this article to show radiation effects on the structural properties of ceramics. Phase transition kinetics have been studied during xenon ion irradiation of polycrystalline MgO and SrTiO3. We have observed that MgO oxide is radiation-resistant to high electronic excitations, contrary to the high sensitivity of SrTiO3, which exhibits transition from the crystalline to the amorphous state during irradiation. By interpreting the amorphization kinetics of SrTiO3, defect overlapping models are discussed as well as latent track characteristics. Together with a transmission electron microscopy study, we conclude that a single impact model describes the phase transition mechanism.
Through powder x-ray diffraction we have investigated the structural behavior of SmVO3, in which orbital and magnetic degrees of freedom are believed to be closely coupled to the crystal lattice. We have found, contrary to previous reports, that SmVO3 exists in a single, monoclinic, phase below 200 K. The associated crystallographic distortion is then stabilized through the magnetostriction that occurs below 134 K. The crystal structure has been refined using synchrotron x-ray powder diffraction data measured throughout the structural phase diagram, showing a substantial Jahn-Teller distortion of the VO6 octahedra in the monoclinic phase, compatible with the expected G-type orbital order. Changes in the vanadium ion crystal field due to the structural and magnetic transitions have then been probed by resonant x-ray diffraction.
Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain, however these protocols need to be evaluated for their effectiveness. Here we use non-destructive Bragg coherent X-ray diffraction imaging to study the in situ annealing of FIB-milled gold microcrystals. We simultaneously measure two non-collinear reflections for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared to thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, we analyse each reflection by considering facet area evolution, cross-correlation maps of displacement field and binarised morphology, and average strain plots. The crystals strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ~280{deg}C and the self-diffusion of gold above ~280{deg}C. The majority of FIB-induced strains are removed by 380-410degree C, depending on which reflection is being considered. Our observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.
In this paper we show how single layer graphene can be utilized to study swift heavy ion (SHI) modifications on various substrates. The samples were prepared by mechanical exfoliation of bulk graphite onto SrTiO$_3$, NaCl and Si(111), respectively. SHI irradiations were performed under glancing angles of incidence and the samples were analysed by means of atomic force microscopy in ambient conditions. We show that graphene can be used to check whether the irradiation was successful or not, to determine the nominal ion fluence and to locally mark SHI impacts. In case of samples prepared in situ, graphene is shown to be able to catch material which would otherwise escape from the surface.
Certain alumino-silicates display exotic properties enabled by their framework structure made of corner-sharing tetrahedral rigid units. Using textit{in situ} diamond-anvil cell x-ray diffraction (XRD), we study the pressure-induced transformation of $beta$ eucryptite, a prototypical alumino-silicate. $beta$ eucryptite undergoes a phase transformation at moderate pressures, but the atomic structure of the new phase has not yet been reported. Based on density functional theory stability studies and Rietveld analysis of XRD patterns, we find that the pressure-stabilized phase belongs to the Pna2$_1$ space group. Furthermore, we discover two other possible pressure-stabilized polymorphs, P1c1 and Pca2$_1$.