Phase transformations during the reaction heat treatment of Powder-In-Tube Nb3_{3}Sn superconductors

The phase transformations prior to the superconducting A15 phase nucleation can influence the critical properties of fully reacted Nb$_{3}$Sn superconductors. We describe for the first time the phase transformations occurring during the heat treatment of state-of-the-art Nb$_{3}$Sn Powder-in-Tube strands, based on in-situ synchrotron diffraction measurements. All pure Sn present in the non-heat treated PIT strand is transformed into Cu6Sn5 by solid state diffusion. Subsequently NbSn2 and Cu6Sn5 are partly transformed into a Sn-rich ternary Cu-Nb-Sn phase. When Sn starts to diffuse into the Nb tubes at about 520°C all Sn-containing phases are transformed into NbSn2 and subsequently into Nb6Sn5

On the formation of voids in internal tin Nb3_{3}Sn superconductors

In this article we describe three void growth mechanisms in Nb$_{3}$Sn strands of the internal tin design on the basis of combined synchrotron micro-tomography and x-ray diffraction measurements during in-situ heating cycles. Initially void growth is driven by a reduction of void surface area by void agglomeration. The main void volume increase is caused by density changes during the formation of Cu3Sn in the strand. Subsequent transformation of Cu-Sn intermetallics into the lower density a-bronze reduces the void volume again. Long lasting temperature ramps and isothermal holding steps can neither reduce the void volume nor improve the chemical strand homogeneity prior to the superconducting A15 phase nucleation and growth

Evidence for length-dependent wire expansion, filament dedensification and consequent degradation of critical current density in Ag-alloy sheathed Bi-2212 wires

It is well known that longer Bi-2212 conductors have significantly lower critical current density (Jc) than shorter ones, and recently it has become clear that a major cause of this reduction is internal gas pressure generated during heat treatment, which expands the wire diameter and dedensifies the Bi-2212 filaments. Here we report on the length-dependent expansion of 5 to 240 cm lengths of state-of-the-art, commercial Ag alloy-sheathed Bi-2212 wire after full and some partial heat treatments. Detailed image analysis along the wire length shows that the wire diameter increases with distance from the ends, longer samples often showing evident damage and leaks provoked by the internal gas pressure. Comparison of heat treatments carried out just below the melting point and with the usual melt process makes it clear that melting is crucial to developing high internal pressure. The decay of Jc away from the ends is directly correlated to the local wire diameter increase, which decreases the local Bi-2212 filament mass density and lowers Jc, often by well over 50%. It is clear that control of the internal gas pressure is crucial to attaining the full Jc of these very promising round wires and that the very variable properties of Bi-2212 wires are due to the fact that this internal gas pressure has so far not been well controlled

Investigating lithium-ion battery materials during overcharge-induced thermal runaway: an operando and multi-scale X-ray CT study

Catastrophic failure of lithium-ion batteries occurs across multiple length scales and over very short time periods. A combination of high-speed operando tomography, thermal imaging and electrochemical measurements is used to probe the degradation mechanisms leading up to overcharge-induced thermal runaway of a LiCoO2 pouch cell, through its interrelated dynamic structural, thermal and electrical responses. Failure mechanisms across multiple length scales are explored using a post-mortem multi-scale tomography approach, revealing significant morphological and phase changes in the LiCoO2 electrode microstructure and location dependent degradation. This combined operando and multi-scale X-ray computed tomography (CT) technique is demonstrated as a comprehensive approach to understanding battery degradation and failure

Removing multiple outliers and single-crystal artefacts from X-ray diffraction computed tomography data

This paper reports a simple but effective filtering approach to deal with single-crystal artefacts in X-ray diffraction computed tomography (XRD-CT). In XRD-CT, large crystallites can produce spots on top of the powder diffraction rings, which, after azimuthal integration and tomographic reconstruction, lead to line/streak artefacts in the tomograms. In the simple approach presented here, the polar transform is taken of collected two-dimensional diffraction patterns followed by directional median/mean filtering prior to integration. Reconstruction of one-dimensional diffraction projection data sets treated in such a way leads to a very significant improvement in reconstructed image quality for systems that exhibit powder spottiness arising from large crystallites. This approach is not computationally heavy which is an important consideration with big data sets such as is the case with XRD-CT. The method should have application to two-dimensional X-ray diffraction data in general where such spottiness arises

Interlaced X-ray diffraction computed tomography

An X-ray diffraction computed tomography data-collection strategy that allows, post experiment, a choice between temporal and spatial resolution is reported. This strategy enables time-resolved studies on comparatively short timescales, or alternatively allows for improved spatial resolution if the system under study, or components within it, appear to be unchanging. The application of the method for studying an Mn–Na–W/SiO2 fixed-bed reactor in situ is demonstrated. Additionally, the opportunities to improve the data-collection strategy further, enabling post-collection tuning between statistical, temporal and spatial resolutions, are discussed. In principle, the interlaced scanning approach can also be applied to other pencil-beam tomographic techniques, like X-ray fluorescence computed tomography, X-ray absorption fine structure computed tomography, pair distribution function computed tomography and tomographic scanning transmission X-ray microscopy

X-ray physico-chemical imaging during activation of cobalt-based Fischer-Tropsch synthesis catalysts

The imaging of catalysts and other functional materials under reaction conditions has advanced significantly in recent years. The combination of the computed tomography (CT) approach with methods such as X-ray diffraction (XRD), X-ray fluorescence (XRF) and X-ray absorption near-edge spectroscopy (XANES) now enables local chemical and physical state information to be extracted from within the interiors of intact materials which are, by accident or design, inhomogeneous. In this work, we follow the phase evolution during the initial reduction step(s) to form Co metal, for Co-containing particles employed as Fischer–Tropsch synthesis (FTS) catalysts; firstly, working at small length scales (approx. micrometre spatial resolution), a combination of sample size and density allows for transmission of comparatively low energy signals enabling the recording of ‘multimodal’ tomography, i.e. simultaneous XRF–CT, XANES–CT and XRD–CT. Subsequently, we show high-energy XRD–CT can be employed to reveal extent of reduction and uniformity of crystallite size on millimetre-sized TiO2 trilobes. In both studies, the CoO phase is seen to persist or else evolve under particular operating conditions and we speculate as to why this is observed

MOSFET dosimetry for microbeam radiation therapy at the European Synchrotron Radiation Facility

Preclinical experiments are carried out with ~20–30 μm wide, ~10 mm high parallel microbeams of hard, broad-‘‘white’’-spectrum x rays (~50–600 keV) to investigate microbeam radiation therapy (MRT) of brain tumors in infants for whom other kinds of radiotherapy are inadequate and/or unsafe. Novel physical microdosimetry (implemented with MOSFET chips in the ‘‘edge-on’’ mode) and Monte Carlo computer-simulated dosimetry are described here for selected points in the peak and valley regions of a microbeam-irradiated tissue-equivalent phantom. Such microbeam irradiation causes minimal damage to normal tissues, possible because of rapid repair of their microscopic lesions. Radiation damage from an array of parallel microbeams tends to correlate with the range of peak-valley dose ratios (PVDR). This paper summarizes comparisons of our dosimetric MOSFET measurements with Monte Carlo calculations. Peak doses at depths \u3c22 mm are 18% less than Monte Carlo values, whereas those depths \u3e22 mm and valley doses at all depths investigated (2 mm–62 mm) are within 2–13% of the Monte Carlo values. These results lend credence to the use of MOSFET detector systems in edge-on mode for microplanar irradiation dosimetry

Genetic and biochemical analyses of chromosome and plasmid gene homologues encoding ICL and ArCP domains in Vibrioanguillarum strain 775

Anguibactin, the siderophore produced by Vibrio anguillarum 775 is synthesized from 2,3-dihydroxybenzoic acid (DHBA), cysteine and hydroxyhistamine via a nonribosomal peptide synthetase (NRPS) mechanism. Most of the genes encoding anguibactin biosynthetic proteins are harbored by the pJM1 plasmid. In this work we report the identification of a homologue of the plasmid-encoded angB on the chromosome of strain 775. The product of both genes harbor an isochorismate lyase (ICL) domain that converts isochorismic acid to 2,3-dihydro-2,3-dihydroxybenzoic acid, one of the steps of DHBA synthesis. We show in this work that both ICL domains are functional in the production of DHBA in V. anguillarum as well as in E. coli. Substitution by alanine of the aspartic acid residue in the active site of both ICL domains completely abolishes their isochorismate lyase activity in vivo. The two proteins also carry an aryl carrier protein (ArCP) domain. In contrast with the ICL domains only the plasmid encoded ArCP can participate in anguibactin production as determined by complementation analyses and site-directed mutagenesis in the active site of the plasmid encoded protein, S248A. The site-directed mutants, D37A in the ICL domain and S248A in the ArCP domain of the plasmid encoded AngB were also tested in vitro and clearly show the importance of each residue for the domain function and that each domain operates independently.

Phase Transformations during the Reaction Heat Treatment

The evolution of Nb containing phases during the diffusion heat treatment of three different high critical current Nb$_{3}$Sn strand types is compared, based on synchrotron X-ray diffraction results that have been obtained at the ID15 beam line of the European Synchrotron Radiation Facility (ESRF). In all strands studied, Nb$_{3}$Sn formation is preceded by the formation of a Cu-Nb-Sn ternary phase, NbSn2 and Nb6Sn5. As compared to the PIT and Tube Type strand, the amount of these phases formed in the RRP strand is relatively small. In the RRP strand subelements with a fine filament structure Nb$_{3}$Sn grows more quickly, thereby preventing to a large extent the formation of the other higher tin phases