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High-Pressure X-ray Diffraction and Raman Spectroscopy of Ice VIII
In situ high-pressure/low-temperature synchrotron x-ray diffraction and optical Raman spectroscopy were used to examine the structural properties, equation of state, and vibrational dynamics of ice VIII. The x-ray measurements show that the pressure-volume relations remain smooth up to 23 GPa at 80 K. Although there is no evidence for structural changes to at least 14 GPa, the unit-cell axial ratio c/a undergoes changes at 10-14 GPa. Raman measurements carried out at 80 K show that the nu(Tz)A(1g)+nu Tx,yEg lattice modes for the Raman spectra of ice VIII in the lower-frequency regions (50-800 cm(-1)) disappear at around 10 GPa, and then a new peak of similar to 150 cm(-1) appears at 14 GPa. The combined data provide evidence for a transition beginning near 10 GPa. The results are consistent with recent synchrotron far-IR measurements and theoretical calculations. The decompressed phase recovered at ambient pressure transforms to low-density amorphous ice when heated to similar to 125 K.Engineering and Applied Science
Studies of multiferroic palladium perovskites
Work at St. Andrews supported by EPSRC grant EP/P024637/1; at Queens University Belfast by EPSRC Grant No. EP/J017191/1 and EP/N018389/1, at Univ. Puerto Rico by DoD AFOSR Grant FA9550-16-1-0295 and at West Virginia University by DOE (DE-SC0016176).We have studied the atomic force microscopy (AFM), X-ray Bragg reflections, X-ray absorption spectra (XAS) of the Pd L-edge, Scanning electron microscopey (SEM) and Raman spectra, and direct magnetoelectric tensor of Pd-substituted lead titanate and lead zirconate-titanate. A primary aim is to determine the percentage of Pd+4 and Pd+2 substitutional at the Ti-sites (we find that it is almost fully substitutional). The atomic force microscopy data uniquely reveal a surprise: both threefold vertical (polarized out-of-plane) and fourfold in-plane domain vertices. This is discussed in terms of the general rules for Voronoi patterns (Dirichlet tessellations) in two and three dimensions. At high pressures Raman soft modes are observed, as in pure lead titanate, and X-ray diffraction (XRD) indicates a nearly second-order displacive phase transition. However, two or three transitions are involved: First, there are anomalies in c/a ratio and Raman spectra at low pressures (P = 1 − 2 GPa); and second, the c/a ratio reaches unity at ca. P = 10 GPa, where a monoclinic (Mc) but metrically cubic transition occurs from the ambient tetragonal P4 mm structure in pure PbTiO3; whereas the Raman lines (forbidden in the cubic phase) remain until ca. 17 GPa, where a monoclinic-cubic transition is known in lead titanate.Publisher PDFPeer reviewe
Mechanisms of Pressure-Induced Phase Transitions by Real-Time Laue Diffraction
Synchrotron X-ray radiation Laue diffraction is a widely used diagnostic technique for characterizing the microstructure of materials. An exciting feature of this technique is that comparable numbers of reflections can be measured several orders of magnitude faster than using monochromatic methods. This makes polychromatic beam diffraction a powerful tool for time-resolved microstructural studies, critical for understanding pressure-induced phase transition mechanisms, by in situ and in operando measurements. The current status of this technique, including experimental routines and data analysis, is presented along with some case studies. The new experimental setup at the High-Pressure Collaborative Access Team (HPCAT) facility at the Advanced Photon Source, specifically dedicated for in situ and in operando microstructural studies by Laue diffraction under high pressure, is presented
Observation of a New Polyhalide Phase in Ag-Cl<sub>2</sub> System at High Pressure
In this short contribution, we examine Raman spectroscopic data from high-pressure and high-temperature experiments with an Ag-Cl2 system, and find that they are in good agreement with previously observed and calculated spectra of polychloride species. Our results imply the formation of a hitherto unknown AgClx compound, which warrants further study