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Register a new userA 31T split-pair pulsed magnet for single crystal x-ray diffraction at low temperature
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We have developed a pulsed magnet system with panoramic access for synchrotron x-ray diffraction in magnetic fields up to 31T and at low temperature down to 1.5 K. The apparatus consists of a split-pair magnet, a liquid nitrogen bath to cool the pulsed coil, and a helium cryostat allowing sample temperatures from 1.5 up to 250 K. Using a 1.15MJ mobile generator, magnetic field pulses of 60 ms length were generated in the magnet, with a rise time of 16.5 ms and a repetition rate of 2 pulses/hour at 31 T. The setup was validated for single crystal diffraction on the ESRF beamline ID06.
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We report the design and construction of a novel soft x-ray diffractometer installed at Diamond Light Source. The beamline endstation RASOR is constructed for general users and designed primarily for the study of single crystal diffraction and thin film reflectivity. The instrument is comprised of a limited three circle ({theta}, 2{theta}, {chi}) diffractometer with an additional removable rotation ({phi}) stage. It is equipped with a liquid helium cryostat, and post-scatter polarization analysis. Motorised motions are provided for the precise positioning of the sample onto the diffractometer centre of rotation, and for positioning the centre of rotation onto the x-ray beam. The functions of the instrument have been tested at Diamond Light Source, and initial test measurements are provided, demonstrating the potential of the instrument.
We present a pulsed-magnet system that enables x-ray single-crystal diffraction in addition to powder and spectroscopic studies with the magnetic field applied on or close to the scattering plane. The apparatus consists of a single large-bore solenoid, cooled by liquid nitrogen. A second independent closed-cycle cryostat is used for cooling samples near liquid helium temperatures. Pulsed magnetic fields close to $sim 30$ T with a zero-to-peak-field rise time of $sim$2.9 ms are generated by discharging a 40 kJ capacitor bank into the magnet coil. The unique characteristic of this instrument is the preservation of maximum scattering angle ($sim 23.6^circ$) on the entrance and exit sides of the magnet bore by virtue of a novel double-funnel insert. This instrument will facilitate x-ray diffraction and spectroscopic studies that are impractical, if not impossible, to perform using split-pair and narrow-opening solenoid magnets, and offers a practical solution for preserving optical access in future higher-field pulsed magnets.
The highly transient nature of shock loading and pronounced microstructure effects on dynamic materials response call for {it in situ}, temporally and spatially resolved, x-ray-based diagnostics. Third-generation synchrotron x-ray sources are advantageous for x-ray phase contrast imaging (PCI) and diffraction under dynamic loading, due to their high photon energy, high photon fluxes, high coherency, and high pulse repetition rates. The feasibility of bulk-scale gas gun shock experiments with dynamic x-ray PCI and diffraction measurements was investigated at the beamline 32ID-B of the Advanced Photon Source. The x-ray beam characteristics, experimental setup, x-ray diagnostics, and static and dynamic test results are described. We demonstrate ultrafast, multiframe, single-pulse PCI measurements with unprecedented temporal ($<$100 ps) and spatial ($sim$2 $mu$m) resolutions for bulk-scale shock experiments, as well as single-pulse dynamic Laue diffraction. The results not only substantiate the potential of synchrotron-based experiments for addressing a variety of shock physics problems, but also allow us to identify the technical challenges related to image detection, x-ray source, and dynamic loading.
The diffraction technique is widely used in the determination of crystal structures and is one of the bases for the modern science and technology. All related structure determination methods are based on the assumption that perfect single crystal X-ray diffraction (SXRD) can determine a structure uniquely. But as the structure factor phases are lost in SXRD and even more information is lost in powder X-ray diffraction (PXRD), this assumption is still questionable. In this work, we found that structures with certain characteristic can have its sister structure with exactly the same PXRD or even SXRD pattern. A computer program is developed to search the ICSD database, and about 1000 structures were identified to have this characteristic. The original structure and its sister structures can have different space groups, topologies, crystal systems etc. and some may even have multiple sisters. Our studies indicate that special caution is needed since a structure with reasonable atomic positions and perfect match of experimental diffraction intensities could still be wrong.
The crystal structure of the new superconductor UTe2 has been investigated for the first time at low temperature (LT) of 2.7 K, just closely above the superconducting transition temperature of about 1.7 K by single crystal neutron diffraction, in order to prove, whether the orthorhombic structure of type Immm (Nr. 71 Int. Tabl.) reported for room temperature (RT) persists down to the superconducting phase and can be considered as a parent symmetry for the development of spin triplet superconductivity. Our results show that the RT structure reported previously obtained by single crystal X-Ray diffraction indeed describes also the LT neutron diffraction data with high precision. No structural change from RT down to 2.7 K is observed. Detailed structural parameters for UTe2 at LT are reported.
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