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At least 343 records · Page 19

Probing the lattice structure of dynamically compressed and released single crystal iron through the alpha to epsilon phase transition

In this work, experiments using broadband Laue x-ray diffraction (XRD) were used to examine the lattice structure of dynamically compressed [100]-oriented single crystal iron samples at the Dynamic Compression Sector at the Advanced Photon Source. These experiments used 1 μm thick iron single crystal samples sandwiched between a polyimide ablator and a polycarbonate window. A 100 J, 10 ns duration laser pulse incident on the polyimide ablator was used to shock compress the iron samples to initial stresses greater than 25 GPa, exceeding the ~13 GPa alpha (body-centered-cubic or bcc structure) to epsilon (hexagonal-close-packed or hcp structure) phase transition stress. XRD measurements were performed at various times relative to the shock wave entering the iron sample: early times, <~150 ps while the initial shock waves propagated through the iron; intermediate times, after the iron equilibrated with the ablator and window reaching a plateau stress state (12 or 17 GPa) lasting several nanoseconds; and late times, during uniaxial strain release. The early time measurements show that in <~150 ps, the high-pressure hcp phase is relaxed with a c/a ratio of 1.61, contrary to previous laser shock experiments where a c/a ratio of 1.7 was inferred. In the plateau stress state and partially released states, XRD measurements showed that the hcp structure retained a c/a ratio of 1.61 with no observable changes in the microstructure. Upon stress release at ~1 GPa/ns release rate, the reverse phase transition (hcp to bcc) to the original single crystal orientation (implying a transformation memory effect) was observed to reach completion somewhere between 13 and 11 GPa, indicating little stress hysteresis under rapid uniaxial strain release. A similar memory effect for the reverse hcp to bcc transformation has been previously observed under hydrostatic compression. However, the bcc/hcp orientation relationships differ somewhat between dynamic and static compression experiments, implying that the transformation pathway under uniaxial dynamic strain differs from the Burgers mechanism.

36 MATERIALS SCIENCE↗

Telecommunication-wavelength two-dimensional photonic crystal cavities in a thin single-crystal diamond membrane

We demonstrate two-dimensional photonic crystal cavities operating at telecommunication wavelengths in a single-crystal diamond membrane. We use a high-optical-quality and thin (~300 nm) diamond membrane, supported by a polycrystalline diamond frame, to realize fully suspended two-dimensional photonic crystal cavities with a high theoretical quality factor of ~8 × 10 6 and a relatively small mode volume of ~2(λ/n) 3 . The cavities are fabricated in the membrane using electron-beam lithography and vertical dry etching. We observe cavity resonances over a wide wavelength range spanning the telecommunication O- and S-bands (1360–1470 nm) with Q factors of up to ~1800. Our method paves the way for on-chip diamond nanophotonic applications in the telecommunication-wavelength range.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Crystal response measurement of the x-ray transmission crystals used by the Imaging Spectroscopy Snout at the National Ignition Facility

The Imaging Spectroscopy Snout (ISS) used at the National Ignition Facility is able to simultaneously collect neutron pinhole images, 1D spatially resolved x-ray spectra, and time resolved x-ray pinhole images. To measure the x-ray spectra, the ISS can be equipped with up to four different transmission crystals, each offering different energy ranges from ∼7.5 to ∼12 keV and different resolutions. Characterizing and calibrating such instruments is of paramount importance in order to extract meaningful results from experiments. More specifically, we characterized different ISS transmission-type alpha-Quartz crystals by measuring their responses as a function of photon energy, from which we inferred the angle-integrated reflectivity for each crystal’s working reflections. These measurements were made at the Lawrence Livermore National Laboratory calibration station dedicated to the characterization of x-ray spectrometers. The sources used covered a wide x-ray range—from a few to 30 keV; the source diameter was ∼0.6 mm. The experimental results are discussed alongside theoretical calculations using the pyTTE model.

Dozieres, M. (ORCID:0000000286401459)↗

Laser radiation frequency doubling in a single-crystal fibre based on a stoichiometric LiNbO{sub 3} crystal

We demonstrate the employment of single-crystal optical fibres based on lithium niobate for doubling the laser radiation frequency. The measured characteristics of the fibre confirm its high quality and spatial homogeneity. Parameters of the frequency doublers for neodymium laser radiation (λ = 1 mm) based on fibre and bulk single crystals are compared. Single crystals are grown by the method of laser-heated pedestal growing with heating by radiation of a CO{sub 2} laser (LHPG-method). (nonlinear optical phenomena)

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Coupling between phonon and crystal-field excitations in multiferroic PrFe 3 ( BO 3 ) 4

Far-infrared reflection and ellipsometry measurements on multiferroic PrFe 3 ( BO 3 ) 4 and SmFe 3 ( BO 3 ) 4 single crystals were used to investigate the interaction between lattice phonons and electronic excitations associated with 4 f crystal-field transitions. A temperature-dependent interference between two types of excitations was observed in PrFe 3 ( BO 3 ) 4 in which the frequency of 4 f crystal-field electronic excitation of Pr 3 + falls into the TO-LO frequency interval of the optical phonon mode near 50 cm - 1 (1.5 THz). Experimental data were explained on the basis of a theoretical model of coupled electron-phonon modes. The fitting procedure revealed the value 14.8 cm - 1 for the electron-phonon coupling constant. This rather large value points to an essential role played by the electron-phonon interaction in the physics of multiferroics.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Twinning and Dislocation Evolution during Shock Compression and Release of Single Crystals: Real-Time X-Ray Diffraction

Determining the temporal evolution of twinning and/or dislocation slip, in real time (nanoseconds), in single crystals subjected to plane shock wave loading is a long-standing scientific need. Non-cubic crystals pose special challenges because they have many competing slip and twinning systems. Here, we report on time-resolved, in situ, synchrotron Laue x-ray diffraction measurements during shock compression and release of magnesium single crystals that are subjected to compression along the c-axis. Significant twinning was observed directly during stress release following shock compression; during compression, only dislocation slip was observed. Our measurements unambiguously distinguish between twinning and dislocation slip on nanosecond timescales in a shocked hexagonal-close-packed metal.

36 MATERIALS SCIENCE↗

Irradiation-driven amorphous-to-glassy transition in quartz: The crucial role of the medium-range order in crystallization

Noncrystalline solids can be classified into glassy and amorphous, wherein glasses and amorphous solids relax toward the supercooled liquid and crystalline states upon heating, respectively. However, the structural origin of such distinction remains unknown. Here in this study, based on molecular-dynamics simulations of irradiation-induced disordering of α-quartz, we demonstrate the existence of an amorphous-to-glassy transition. We show that the transition to the glassy state originates from the appearance of structural defects within the medium-range order of the atomic network. Such defects arise from the percolation of short-range defects and kinetically prevent crystallization. Overall, this suggests that the propensity of a disordered system for crystallization is controlled by the similarity between its medium-range order and that of the isochemical crystal.

36 MATERIALS SCIENCE↗

Crystal structure of a 2:1 piroxicam–gentisic acid co-crystal featuring neutral and zwitterionic piroxicam molecules

A new 2:1 co-crystal of piroxicam and gentisic acid [systematic name: 4-hydroxy-1,1-dioxo- N -(pyridin-2-yl)-2 H -1λ 6 ,2-benzothiazine-3-carboxamide–2-(4-oxido-1,1-dioxo-2 H -1λ 6 ,2-benzothiazine-3-amido)pyridin-1-ium–2,5-dihydroxybenzoic acid, 2C 15 H 13 N 3 O 4 S·C 7 H 6 O 4 ] has been synthesized using a microfluidic platform and initially identified using Raman spectroscopy. In the co-crystal, one piroxicam molecule is in its neutral form and an intramolecular O—H...O hydrogen bond is observed. The other piroxicam molecule is zwitterionic (proton transfer from the OH group to the pyridine N atom) and two intramolecular N—H...O hydrogen bonds occur. The gentisic acid molecule shows whole-molecule disorder over two sets of sites in a 0.809(2):0.191(2) ratio. In the crystal, extensive hydrogen bonding between the components forms layers propagating in the ab plane.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Role of the PbTiO 3 Seed Layer on the Crystallization Behavior of PZT Thin Films

The role of a highly crystalline and oriented lead titanate ( PTO ) seed layer on the subsequent phase and texture evolution of lead zirconate titanate ( PZT ) thin films is investigated in situ using X‐ray diffraction ( XRD ) during crystallization. Crystalline PTO seed layers were first prepared via a 2‐methoxyethanol route. Amorphous PZT with a Zr/Ti ratio of 52/48 was then deposited on the seed layer using the same synthesis route and subsequently crystallized in situ during XRD . During heating, a tetragonal‐to‐cubic transformation of the seed layer occurs prior to the formation of perovskite PZT . Subsequent nucleation of the crystalline PZT occurs in the cubic phase. Simultaneous to nucleation of PZT , development of a dominant 100 texture component was observed in the PZT phase of the thin films. The results indicate that 100 textured PTO nucleates 100 texture of PZT thin films during crystallization.

Mhin, Sungwook↗

Phase transition and energy storage behavior of antiferroelectric PLZT thin films epitaxially deposited on SRO buffered STO single crystal substrates [Phase transition and energy storage behavior of antiferroelectric PLZT thin films epitaxially deposited on SRO buffered STO single crystal substrates]

Thin films of 300-nm-thick (Pb 0.98 , La 0.02 )(Zr 0.95 , Ti 0.05 )O 3 (PLZT) were epitaxially deposited on (100), (110), and (111) SrTiO3 single crystal substrates by pulsed laser deposition. X-ray diffraction line and reciprocal space mapping (RSM) scans were used to determine the crystal structure. Tetragonal ((001) PLZT) and monoclinic MA ((O 1 1 ) and (111) PLZT) structures were found, which influenced the stored energy density. Electric field induced antiferroelectric to ferroelectric (AFE—>FE) phase transitions were found to have a large reversible energy density of up to 30J/cm 3 . With increasing temperature, an AFE to relaxor ferroelectric (AFE—>RFE) transition was found. The RFE phase exhibited lower energy loss, and an improved energy storage efficiency. Here, the results are discussed from the perspective of crystal structure, dielectric phase transitions, and energy storage characteristics.

25 ENERGY STORAGE↗

Lead halide perovskites: Crystal-liquid duality, phonon glass electron crystals, and large polaron formation

Lead halide perovskites have been demonstrated as high performance materials in solar cells and light-emitting devices. These materials are characterized by coherent band transport expected from crystalline semiconductors, but dielectric responses and phonon dynamics typical of liquids. This “crystal-liquid” duality implies that lead halide perovskites belong to phonon glass electron crystals, a class of materials believed to make the most efficient thermoelectrics. We show that the crystal-liquid duality and the resulting dielectric response are responsible for large polaron formation and screening of charge carriers, leading to defect tolerance, moderate charge carrier mobility, and radiative recombination properties. Large polaron formation, along with the phonon glass character, may also explain the marked reduction in hot carrier cooling rates in these materials.

14 SOLAR ENERGY↗

Orthorhombic YBaCo{sub 4}O{sub 8.4} crystals as a result of saturation of hexagonal YBaCo{sub 4}O{sub 7} crystals with oxygen

Hexagonal YBaCo{sub 4}O{sub 7} crystals (sp. gr. P6{sub 3}mc, a{sub h} = 6.3058(4) Å, c{sub h} = 10.2442(7) Å, Z = 2) are saturated with oxygen to the YBaCo{sub 4}O{sub 8.4} composition and studied by X-ray diffraction (XRD) analysis. The saturation is completed by a structural first-order phase transition to orthorhombic crystals (sp. gr. Pbc2{sub 1}, a{sub o} = 31.8419(2) Å, b{sub o} = 10.9239(5) Å, c{sub o} = 10.0960(5) Å, Z = 20). The connection of two lattices is expressed in terms of the action of matrix (500/120/001) on the hexagonal basis. Five structural fragments of the same type but with different degrees of order alternate along the long axis of the oxygen-saturated orthorhombic structure. The XRD data on single crystals differ from the results obtained by other researchers on ceramic samples; possible causes of these differences are discussed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Synthesis, crystal structure refinement, and nonlinear-optical properties of CaB{sub 3}O{sub 5}(OH): Comparative crystal chemistry of calcium triborates

Calcium triborate CaB{sub 3}O5(OH) obtained by hydrothermal synthesis in the Ca(OH){sub 2}–H{sub 3}BO{sub 3}–Na{sub 2}CO{sub 3}–KCl system is studied by single-crystal X-ray diffraction. The parameters of the orthorhombic unit cell are as follows: a = 13.490(1), b = 6.9576(3), and c = 4.3930(2) Å; V = 412.32(3) Å{sup 3} and space group Pna2{sub 1}. The structure is refined in the anisotropic approximation of the atomic displacement parameters to R = 4.28% using 972 vertical bar F vertical bar > 4σ(F). It is confirmed that the crystal structure of Ca triborate CaB{sub 3}O{sub 5}(OH) is identical to that described earlier. The hydrogen atom is localized. An SHG signal stronger than that of the quartz standard is registered. The phase transition of calcium triborate into calciborite is found on heating. The comparative crystal-chemical analysis of a series of borates with the general chemical formula 2CaO · 3B{sub 2}O{sub 3} · nH{sub 2}O (n = 0–13) with the constant CaO: B{sub 2}O{sub 3}= 2: 3 ratio and variable content of water is performed.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Surface-spike growth on NiBr sub 2 crystals - A VLS mode of crystal growth.

Droplets associated with surface-spike growth of crystals of NiBr 2 by sublimation have been analyzed and found to contain Cu, Co, Mn, and Fe in addition to Ni and Br. These elements exist in the bulk of the original charge material in concentrations that are several orders of magnitude lower than that in the droplets. During crystal growth by sublimation the impurities collect on the surface of growing crystals, until sufficient concentrations are reached to cause the nucleation of a metastable liquid phase droplet. Once the liquid phase droplets have been nucleated, they may then become attached to growth steps and produce accelerated growth from these sites. Such processes occur in NiBr 2 , during growth by sublimation, at approximately 500 °C below the melting point of NiBr 2 .

Edward N Sickafus↗

Polymer crystallization in a temperature gradient field with controlled crystal growth rate

A method is described for studying the influence of a temperature gradient on the crystallization of quiescent polymer melts. The apparatus used consists of two brass plates with embedded electrical resistance heaters and cooling coils. The crystallizations experiments were conducted by placing polymer specimens between the paltes, and manually adjusting heaters and cooling fluids for temperature control. Linear polyethylene, isotactic polyprophylene, and a high density polyethylene were used. It is concluded that the role of a temperature gradient in producing oriented crystallization is in producing conditions which lead the spherulitic growth pattern to proceed primarily in one direction. Steep gradients diminish the penetration of supercooling and favors oriented growth.

Hansen, D.↗

Measurements of the short-term stability of quartz crystal resonators: A window on future developments in crystal oscillators

Recent measurements of the inherent short-term stability of quartz crystal resonators are presented. These measurements show that quartz resonators are much more stable for times less than 1s than the best available commercial quartz oscillators. A simple model appears to explain the noise mechanism in crystal controlled oscillators and points the way to design changes which should permit more than 2 orders of magnitude improvement in their short-term stability. Calculations show that a reference signal at 1 THz, derived from frequency multiplying a 5 MHz source with the above measured crystal stability, should have an instantaneous or fast linewidth of order 1 Hz. These calculations explicitly include the noise contribution of our present multiplier chains and are briefly outlined.

Walls, F. L.↗