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Scientific tasks aimed at decoding and characterizing complex systems and processes at high pressures set new challenges for modern X-ray diffraction instrumentation in terms of X-ray flux, focal spot size and sample positioning. Presented here are new developments at the Extreme Conditions beamline (P02.2, PETRA III, DESY, Germany) that enable considerable improvements in data collection at very high pressures and small scattering volumes. In particular, the focusing of the X-ray beam to the sub-micrometer level is described, and control of the aberrations of the focusing compound refractive lenses is made possible with the implementation of a correcting phase plate. This device provides a significant enhancement of the signal-to-noise ratio by conditioning the beam shape profile at the focal spot. A new sample alignment system with a small sphere of confusion enables single-crystal data collection from grains of micrometer to sub-micrometer dimensions subjected to pressures as high as 200 GPa. The combination of the technical development of the optical path and the sample alignment system contributes to research and gives benefits on various levels, including rapid and accurate diffraction mapping of samples with sub-micrometer resolution at multimegabar pressures., Funding Agencies: Federal Ministry of Education and Research, Germany (BMBF) [05K19WC1]; Deutsche Forschungsgemeinschaft (DFG) [DU 954-11/1, DU 393-9/2, DU 393-13/1]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linköping University (Faculty Grant SFO-Mat-LiU) [2009 00971]; Alexander von Humboldt Foundation

Scientific tasks aimed at decoding and characterizing complex systems and processes at high pressures set new challenges for modern X-ray diffraction instrumentation in terms of X-ray flux, focal spot size and sample positioning. Presented here are new developments at the Extreme Conditions beamline (P02.2, PETRA III, DESY, Germany) that enable considerable improvements in data collection at very high pressures and small scattering volumes. In particular, the focusing of the X-ray beam to the sub-micrometer level is described, and control of the aberrations of the focusing compound refractive lenses is made possible with the implementation of a correcting phase plate. This device provides a significant enhancement of the signal-to-noise ratio by conditioning the beam shape profile at the focal spot. A new sample alignment system with a small sphere of confusion enables single-crystal data collection from grains of micrometer to sub-micrometer dimensions subjected to pressures as high as 200 GPa. The combination of the technical development of the optical path and the sample alignment system contributes to research and gives benefits on various levels, including rapid and accurate diffraction mapping of samples with sub-micrometer resolution at multimegabar pressures., Funding Agencies: Federal Ministry of Education and Research, Germany (BMBF) [05K19WC1]; Deutsche Forschungsgemeinschaft (DFG) [DU 954-11/1, DU 393-9/2, DU 393-13/1]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linköping University (Faculty Grant SFO-Mat-LiU) [2009 00971]; Alexander von Humboldt Foundation

Scientific tasks aimed at decoding and characterizing complex systems and processes at high pressures set new challenges for modern X-ray diffraction instrumentation in terms of X-ray flux, focal spot size and sample positioning. Presented here are new developments at the Extreme Conditions beamline (P02.2, PETRA III, DESY, Germany) that enable considerable improvements in data collection at very high pressures and small scattering volumes. In particular, the focusing of the X-ray beam to the sub-micrometer level is described, and control of the aberrations of the focusing compound refractive lenses is made possible with the implementation of a correcting phase plate. This device provides a significant enhancement of the signal-to-noise ratio by conditioning the beam shape profile at the focal spot. A new sample alignment system with a small sphere of confusion enables single-crystal data collection from grains of micrometer to sub-micrometer dimensions subjected to pressures as high as 200 GPa. The combination of the technical development of the optical path and the sample alignment system contributes to research and gives benefits on various levels, including rapid and accurate diffraction mapping of samples with sub-micrometer resolution at multimegabar pressures., Funding Agencies: Federal Ministry of Education and Research, Germany (BMBF) [05K19WC1]; Deutsche Forschungsgemeinschaft (DFG) [DU 954-11/1, DU 393-9/2, DU 393-13/1]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linköping University (Faculty Grant SFO-Mat-LiU) [2009 00971]; Alexander von Humboldt Foundation

Scientific tasks aimed at decoding and characterizing complex systems and processes at high pressures set new challenges for modern X-ray diffraction instrumentation in terms of X-ray flux, focal spot size and sample positioning. Presented here are new developments at the Extreme Conditions beamline (P02.2, PETRA III, DESY, Germany) that enable considerable improvements in data collection at very high pressures and small scattering volumes. In particular, the focusing of the X-ray beam to the sub-micrometer level is described, and control of the aberrations of the focusing compound refractive lenses is made possible with the implementation of a correcting phase plate. This device provides a significant enhancement of the signal-to-noise ratio by conditioning the beam shape profile at the focal spot. A new sample alignment system with a small sphere of confusion enables single-crystal data collection from grains of micrometer to sub-micrometer dimensions subjected to pressures as high as 200 GPa. The combination of the technical development of the optical path and the sample alignment system contributes to research and gives benefits on various levels, including rapid and accurate diffraction mapping of samples with sub-micrometer resolution at multimegabar pressures., Funding Agencies: Federal Ministry of Education and Research, Germany (BMBF) [05K19WC1]; Deutsche Forschungsgemeinschaft (DFG) [DU 954-11/1, DU 393-9/2, DU 393-13/1]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linköping University (Faculty Grant SFO-Mat-LiU) [2009 00971]; Alexander von Humboldt Foundation

Scientific tasks aimed at decoding and characterizing complex systems and processes at high pressures set new challenges for modern X-ray diffraction instrumentation in terms of X-ray flux, focal spot size and sample positioning. Presented here are new developments at the Extreme Conditions beamline (P02.2, PETRA III, DESY, Germany) that enable considerable improvements in data collection at very high pressures and small scattering volumes. In particular, the focusing of the X-ray beam to the sub-micrometer level is described, and control of the aberrations of the focusing compound refractive lenses is made possible with the implementation of a correcting phase plate. This device provides a significant enhancement of the signal-to-noise ratio by conditioning the beam shape profile at the focal spot. A new sample alignment system with a small sphere of confusion enables single-crystal data collection from grains of micrometer to sub-micrometer dimensions subjected to pressures as high as 200 GPa. The combination of the technical development of the optical path and the sample alignment system contributes to research and gives benefits on various levels, including rapid and accurate diffraction mapping of samples with sub-micrometer resolution at multimegabar pressures., Funding Agencies: Federal Ministry of Education and Research, Germany (BMBF) [05K19WC1]; Deutsche Forschungsgemeinschaft (DFG) [DU 954-11/1, DU 393-9/2, DU 393-13/1]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linköping University (Faculty Grant SFO-Mat-LiU) [2009 00971]; Alexander von Humboldt Foundation

Here, we present a method to study the equation of state of opaque amorphous and crystalline materials in diamond anvil cells. The approach is based on measurements of sample dimensions using high-resolution optical microscopy. Data on the volumetric strain as a function of pressure allow deriving the isothermal equation of state of the studied material. The analysis of optical images is fully automatized and allows measuring the sample dimensions with the precision of about 60 nm. The methodology was validated by studying isothermal compression of omega-Ti up to 30 GPa in a Ne pressure transmitting medium. Within the accuracy of the measurements, the bulk modulus of omega-Ti determined using optical microscopy was similar to that obtained from x-ray diffraction. For glassy carbon compressed to similar to 30 GPa, the previously unknown bulk modulus was found to be equal to K-0 = 28 (2) GPa [K = 5.5(5)]. Published under an exclusive license by AIP Publishing., Funding Agencies|Federal Ministry of Education and Research, Germany (BMBF)Federal Ministry of Education & Research (BMBF) [05K19WC1]; Deutsche Forschungsgemeinschaft (DFG)German Research Foundation (DFG) [DU 954-11/1, DU 393-9/2, DU 393-13/1]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linkoping University [2009 00971]

The diamond anvil cell (DAC) technique is a powerful method for the synthesis and studying of novel materials at extreme conditions. In this work we report on high-pressure high-temperature (HPHT) synthesis of palladium carbides (PdCx) and palladium hydride (PdH) in a laser heated diamond anvil cell. Formation of PdCx with a face-centered cubic (fcc) structure resulted from a chemical reaction of Pd with carbon from the diamond anvils at a pressure of about 50 GPa and temperature of 2500-3000 K. The samples were analyzed in situ using synchrotron X-ray diffraction. The compressional behavior of PdC0.19(3) and PdC0.17(3), was studied on decompression. The fit of the pressure-volume data using the 3rd order Birch-Murnaghan equation of state gave the following parameters: V-0 = 65.1 (1) angstrom 3, K-0 = 241 (9) GPa and K-0 = 2.1 (3) for PdC0.19(3), and V-0 = 64.51 (5) angstrom(3), K-0 = 189 (8) GPa and K-0 = 4.5 (4) for PdC0.17(3). The palladium hydride PdH was synthesized at P = 39 (2) GPa and T = 1500 (200) K through a direct reaction of Pd with paraffin oil. (C) 2020 Elsevier B.V. All rights reserved., Funding Agencies|Federal Ministry of Education and Research, Germany (BMBF)Federal Ministry of Education & Research (BMBF) [05K19WC1]; Deutsche Forschungsgemeinschaft (DFG)German Research Foundation (DFG) [DU 954-11/1, DU 393-9/2, DU 393-13/1]; Swedish Government Strategic Research Area in Materials Science on Functional Materials at Linkoping University (Faculty Grant SFO-Mat-LiU) [2009 00971]