Local structure studies using the pair distribution function

The pair distribution analysis method is a fast spreading structural analysis method allowing to go beyond classical crystallographic analysis by providing quantitative information about local as well as meso-structure. It based on powder diffraction data fourier transformed to direct space. We will present here the main characteristics of the method, and its domain of application

Jahn-Teller, polarity and insulator-to-metal transition in BiMnO3 at high pressure

The interaction of coexisting structural instabilities in multiferroic materials gives rise to intriguing coupling phenomena and extraordinarily rich phase diagrams, both in bulk materials and strained thin films. Here we investigate the multiferroic BiMnO3 with its peculiar 6s2 electrons and four interacting mechanisms: electric polarity, octahedra tilts, magnetism, and cooperative Jahn-Teller distortion. We have probed structural transitions under high pressure by synchrotron x-ray diffraction and Raman spectroscopy up to 60 GPa. We show that BiMnO3 displays under pressure a rich sequence of five phases with a great variety of structures and properties, including a metallic phase above 53 GPa and, between 37 and 53 GPa, a strongly elongated monoclinic phase that allows ferroelectricity, which contradicts the traditional expectation that ferroelectricity vanishes under pressure. Between 7 and 37 GPa, the Pnma structure remains remarkably stable but shows a reduction of the Jahn-Teller distortion in a way that differs from the behavior observed in the archetypal orthorhombic Jahn-Teller distorted perovskite LaMnO3.Comment: 5 pages, 3 figures + supplemental material included (3 pages, 1 figure, 3 tables

Magnetic phase diagram of the S=1/2 triangular layered compound NaNiO2: a single crystal study

Using magnetic torque measurement on a NaNiO2 single crystal, we have established the magnetic phase diagram of this triangular compound. It presents 5 different phases depending on the temperature (4 K - 300 K) and magnetic field (0 - 22 T) revealing several spin reorientations coupled to different magnetic anisotropies

Spin liquid correlations in Nd-langasite anisotropic Kagom\'e antiferromagnet

Dynamical magnetic correlations in the geometrically frustrated Nd$\_3$Ga$\_5$SiO$\_{14}$ compound were probed by inelastic neutron scattering on a single crystal. A scattering signal with a ring shape distribution in reciprocal space and unprecedented dispersive features was discovered. Comparison with calculated static magnetic scattering from models of correlated spins suggests that the observed phase is a spin liquid inherent to an antiferromagnetic kagom\'e-like lattice of anisotropic Nd moments.Comment: 4 page

Advanced survival models for risk-factor analysis in scrapie

Because of the confounding effects of long incubation duration and flock management, accurate epidemiological studies of scrapie outbreaks are difficult to carry out. In this study, 641 Manech red-faced sheep from six scrapie-affected field flocks in Pyrénées Atlantiques, France, were monitored for clinical scrapie over a 6–9 year period. Over this period, 170 scrapie clinical cases were recorded and half of the culled animals were submitted for post-mortem transmissible spongiform encephalopathy diagnosis to assess their infectious status. Collected data were analysed using a ‘mixture cure model’ approach, which allowed for the discriminating effect of PrP genotype and flock origin on incidence and incubation period. Simulations were performed to evaluate the applicability of such a statistical model to the collected data. As expected, ARR heterozygote sheep were less at risk of becoming infected than ARQ/ARQ individuals and had a greater age at clinical onset. Conversely, when compared with ARQ/ARQ, the VRQ haplotype was associated with an increased infection risk, but not a shorter incubation period. Considering the flock effect, we observed that a high incidence rate was not associated with shorter incubation periods and that the incubation period could be significantly different in flocks harbouring similar infection risks. These results strongly support the conclusion that other parameters, such as the nature of the agent or flock management, could interfere with epidemiological dynamics of the infection in scrapie-affected flocks

Parity Broken Chiral Spin Dynamics in Ba3_3NbFe3_3Si2_2O14_{14}

The spin wave excitations emerging from the chiral helically modulated 120$^{\circ}$ magnetic order in a langasite Ba$_3$NbFe$_3$Si$_2$O$_{14}$ enantiopure crystal were investigated by unpolarized and polarized inelastic neutron scattering. A dynamical fingerprint of the chiral ground state is obtained, singularized by (i) spectral weight asymmetries answerable to the structural chirality and (ii) a full chirality of the spin correlations observed over the whole energy spectrum. The intrinsic chiral nature of the spin waves elementary excitations is shown in absence of macroscopic time reversal symmetry breaking

High pressure and high temperature in situ X-ray diffraction studies in the Paris-Edinburgh cell using a laboratory X-ray source

International audienceWe have developed a new laboratory experimental set-up to study in situ the pressure-temperature phase diagram of a given pure element or compound, its associated phase transitions, or the chemical reactions involved at high pressure and high temperature (HP-HT) between different solids and liquids. This new tool allows laboratory studies before conducting further detailed experiments using more brilliant synchrotron X-ray sources or before kinetic studies. This device uses the diffraction of X-rays produced by a quasi-monochromatic micro-beam source operating at the silver radiation (λ(Ag)Kα1,2 ≈ 0.56Å). The experimental set-up is based on a VX Paris-Edinburgh cell equipped with tungsten carbide or sintered diamond anvils and uses standard B-epoxy 5 or 7mm gaskets. The diffracted signal coming from the compressed (and heated) sample is collected on an image plate. The pressure and temperature calibrations were performed by diffraction, using conventional calibrants (BN, NaCl and MgO) for determination of the pressure, and by crossing isochores of BN, NaCl, Cu or Au for the determination of the temperature. The first examples of studies performed with this new laboratory set-up are presented in the article: determination of the melting point of germanium and magnesium under HP-HT, synthesis of MgB2 or C-diamond and partial study of the P, T phase diagram of MgH2

Lu5Ir4Si10 whiskers : morphologies, structure cristalline, mosaïcité, supraconductivité et onde de densité de charge

National audienceParmi la famille très riche de composés intermétalliques R5Ir4Si10 (R=terre-rare), la phase Lu5Ir4Si10 est supraconductrice en dessous de 4K et présente une transition liée à une onde de densité de charge à 80K [1]. Des cristaux en forme d'aiguilles ou whiskers ont été obtenus. Les conditions de synthèses sont présentées ainsi qu'une observation détaillée de leur taille et morphologie, obtenue au microscope électronique à balayage [2]. Des analyses par diffraction de rayons X ont confirmé que ces aiguilles cristallisaient sous la même structure quadratique P4/mbm que les cristaux massifs. Les paramètres de mailles a = 12.484(1) Å et c = 4.190(2) Å sont comparables à ceux de la littérature [3]. A l'aide d'un diffractomètre 4-cercles, nous avons trouvé que les aiguilles poussent selon l'axe c et que les faces latérales sont orientées selon la direction [110]. La mosaïcité de ces cristaux a été mesurée à l'ESRF, ligne ID27. Elle est inférieure à 0.15° le long de l'axe c. Enfin, des mesures de résistivité électriques sont détaillées. Elles confirment l'excellente qualité de ces cristaux

Fe-MOF Materials as Precursors for the Catalytic Dehydrogenation of Isobutane.

We investigate the use of a series of iron-based metal-organic frameworks as precursors for the manufacturing of isobutane dehydrogenation catalysts. Both the as-prepared and spent catalysts were characterized by PXRD, XPS, PDF, ICP-OES, and CHNS+O to determine the physicochemical properties of the materials and the active phases responsible for the catalytic activity. In contrast to the previous literature, our results indicate that (i) the formation of metallic Fe under reaction conditions results in secondary cracking and coke formation; (ii) the formation of iron carbide only contributes to coke formation; and (iii) the stabilization of the Fe2+ species is paramount to achieve stable and selective catalysts. In this sense, promotion with potassium and incorporation of titanium improve the catalytic performance. While potassium is well known to improve the selectivity in iron-catalyzed dehydrogenation reactions, the unprecedented effect of titanium in the stabilization of a nanometric titanomaghemite phase, even under reductive reaction conditions, results in a moderately active and highly selective catalyst for several hours on stream with a remarkable resistance to coke formation

A highly conductive nanostructured PEDOT polymer confined into the mesoporous MIL-100(Fe)

[EN] Despite the higher efficiency, larger color range and faster stimulus response of polymeric electrochromic materials, their poor cyclability strongly hampers their application in optoelectronics. As an original strategy to stabilize and further nanostructure these polymers, herein an efficient encapsulation and in situ polymerization inside highly porous metal-organic frameworks (MOFs) is reported. In particular, the successful accommodation of poly(3,4-ethylendioxythiophene) (PEDOT) and its partially oxidized polarons inside the mesopores of the nontoxic iron trimesate MIL-100(Fe) is convincingly proved by a large panel of experimental techniques. Remarkably, the polymer-MOF interaction occurring for entrapped PEDOT within the pores (deeply assessed by experimental and simulation methods) might be responsible for the enhanced electrical conductivity of the resulting PEDOT@MIL-100(Fe) composite when compared to the insulating MIL-100(Fe) and the conductive free PEDOT. Furthermore, it was possible to observe the electrochromic properties of the PEDOT@MIL-100(Fe) composite, achieving an improved stability and good cyclability as a consequence of the effective protection by the MOF matrix.This work was supported by a 2017 Leonardo Grant for Researchers and Cultural Creators, BBVA Foundation (IN[17]_CBB_QUI_0197). The work was also partially supported by IMDEA Energy and Raphuel project (ENE2016-79608-C2-1-R, MINECOAEI/FEDER, UE). PH acknowledges the Spanish Ramon y Cajal Programme (grant agreement no. 2014-16823). S. N. thanks the Spanish Ministerio de Educacion, Cultura y Deporte for Jose Castillejo mobility programme (CAS14/00067) and financial support by Fundacion Ramon Areces (XVIII Concurso Nacional para la Adjudicacion de Ayudas a la Investigacion en Ciencias de la Vida y de la Materia, 2016). 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