New Raman measurements for HO ice VII in the range of 300 cm to 4000 cm at pressures up to 120 GPa.

Raman spectroscopic measurements for HO ice VII have been conducted to 120 GPa at 300 K in the spectroscopic range of 300-4000 cm. Both moissanite and diamond anvils were used for the experiments. This overcomes the problems of overlapping spectra between the diamond anvil and sample, which had prevented the observation of the stretching modes at pressures higher than ∼23 GPa in all previous measurements.

Pressure Processing of Nanocube Assemblies Toward Harvesting of a Metastable PbS Phase.

This materials-by-design approach combines nanocrystal assembly with pressure processing to drive the attachment and coalescence of PbS nanocubes along directed crystallographic dimensions to form a large 3D porous architecture. This quenchable and strained mesostructure holds the storage of large internal stress, which stabilizes the high-pressure PbS phase in atmospheric conditions. Nanocube fusion enhances the structural stability; the large surface area maintains the size-dependent properties.

Decoding the superlattice and interface structure of truncate PbS nanocrystal-assembled supercrystal and associated interaction forces.

Large scale three-dimensional supercrystals were grown by controlling evaporation of truncate PbS nanocrystal (NC) dispersed hexane suspensions. Electron microscopy analysis confirmed the nature of single supercrystal with a face-centered cubic (fcc) lattice. Synchrotron small/wide angle scattering (SAXS/WAXS) images from three typical crystallographic projections allowed ultimate reconstruction of shape orientations of NCs at different crystallographic sites.

Correlating superlattice polymorphs to internanoparticle distance, packing density, and surface lattice in assemblies of PbS nanoparticles.

Assemblies of 3.5 nm PbS nanoparticles (NPs) nucleate in three dominant superlattice polymorphs: amorphous, body-centered-cubic (bcc) and face-centered-cubic (fcc) phase. This superlattice relationship can be controlled by the inter-NP distance without changing the NP size.

Deviatoric stress driven formation of large single-crystal PbS nanosheet from nanoparticles and in situ monitoring of oriented attachment.

Two-dimensional single-crystal PbS nanosheets were synthesized by deviatoric stress-driven orientation and attachment of nanoparticles (NPs). In situ small- and wide-angle synchrotron X-ray scattering measurements on the same spot of the sample under pressure coupled with transmission electron microscopy enable reconstruction of the nucleation route showing how enhanced deviatoric stress causes ordering NPs into single-crystal nanosheets with a lamellar mesostructure. At the same time that deviatoric stress drives SC(110) orientation in a face-centered-cubic supercrystal (SC), rocksalt (RS) NPs rotate and align their RS(200) and RS(220) planes within the SC(110) plane.

Integrating in situ high pressure small and wide angle synchrotron x-ray scattering for exploiting new physics of nanoparticle supercrystals.

Combined small and wide angle synchrotron x-ray scattering (SAXS and WAXS) techniques have been developed for in situ high pressure samples, enabling exploration of the atomic structure and nanoscale superstructure phase relations. These studies can then be used to find connections between nanoparticle surfaces and internal atomic arrangements. We developed a four-axis control system for the detector, which we then employed for the study of two supercrystals assembled from 5 nm Fe(3)O(4) and 10 nm Au nanoparticles.

Containment of fluid samples in the hydrothermal diamond-anvil cell without the use of metal gaskets: performance and advantages for in situ analysis.

Metal gaskets (Re, Ir, Inconel, or stainless steel) normally used to contain fluid samples in the hydrothermal diamond-anvil cell (HDAC) are sometimes undesirable due to possible contamination and to gasket deformation at high pressures and temperatures resulting in nonisochoric behavior. Furthermore, in x-ray spectroscopic experiments, metal gaskets may attenuate the incident x-ray beam and emitted fluorescence x-rays, and the interaction of scattered radiation with the gasket may produce fluorescence that interferes with the x-ray spectrum of the sample. New arrangements and procedures were tested for the operation of the HDAC without using the metal gaskets.

Synchrotron x-ray spectroscopy of EuHNO3 aqueous solutions at high temperatures and pressures and Nb-bearing silicate melt phases coexisting with hydrothermal fluids using a modified hydrothermal diamond anvil cell and rail assembly.

A modified hydrothermal diamond anvil cell (HDAC) rail assembly has been constructed for making synchrotron x-ray absorption spectroscopy, x-ray fluorescence, and x-ray mapping measurements on fluids or solid phases in contact with hydrothermal fluids up to approximately 900 degrees C and 700 MPa. The diamond anvils of the HDAC are modified by laser milling grooves or holes, for the reduction of attenuation of incident and fluorescent x rays and sample cavities. The modified HDAC rail assembly has flexibility in design for measurement of light elements at low concentrations or heavy elements at trace levels in the sample and the capability to probe minute individual phases of a multiphase fluid-based system using focused x-ray microbeam.

Optical study of H2O ice to 120 GPa: dielectric function, molecular polarizability, and equation of state.

The refractive index of H2O ice has been measured to 120 GPa at room temperature using reflectivity methods. The refractive index increases significantly with pressure on initial compression and exhibits small changes with pressure at previously identified phase transitions. Pressure dependencies of the molecular polarizability show changing slopes in different pressure regions.