Mark A. Beno

Structure of the single‐phase high‐temperature superconductor YBa2Cu3O7−δ

We have determined the crystal structure of the single‐phase stoichiometric high‐temperature superconductor in the Y‐Ba‐Cu‐O system using high‐resolution neutron powder diffraction. This compound has an orthorhombic structure with space group Pmmm and lattice constants a=3.8231 A, b=3.8864 A, and c=11.6807 A. The structure consists of ‘‘dimpled’’ CuO2 layers in the a‐b planes loosely bonded by one‐dimensional fencelike square‐planar CuO3 chains in the b‐c planes.

Structure and superconductivity of HgBa2CuO4+δ

Abstract We have used neutron powder diffraction to investigate the defect structure of HgBa 2 CuO 4+δ . An interstitial oxygen defect in the Hg plane is the primary doping mechanism. A superconducting transition temperature, T c onset , of 95 K is achieved when ≈0.06 oxygen atoms per formula unit are incorporated at this site by annealing the sample at 500°C in pure oxygen. Annealing in argon at 500°C lowers the oxygen content in this site to ≈0.01 and results in a T c of 59 K. The neutron powder diffraction data give evidence for a second defect in the Hg plane which we conclude involves the substitution of copper for about 8% of the mercury and the incorporation of additional oxygen (≈0.1 atoms per formula unit), presumably bonded to the copper defects. In the present samples, the concentration of this defect does not vary with synthesis conditions and its contribution to doping is, therefore, unclear. The structure of the compound is the same at room temperature and superconducting temperatures.

A dedicated powder diffraction beamline at the Advanced Photon Source: Commissioning and early operational results

A new dedicated high-resolution high-throughput powder diffraction beamline has been built, fully commissioned, and opened to general users at the Advanced Photon Source. The optical design and commissioning results are presented. Beamline performance was examined using a mixture of the NIST Si and Al(2)O(3) standard reference materials, as well as the LaB6 line-shape standard. Instrumental resolution as high as 1.7 x 10(-4) (DeltaQQ) was observed.

A twelve-analyzer detector system for high-resolution powder diffraction.

A dedicated high-resolution high-throughput X-ray powder diffraction beamline has been constructed at the Advanced Photon Source (APS). In order to achieve the goals of both high resolution and high throughput in a powder instrument, a multi-analyzer detector system is required. The design and performance of the 12-analyzer detector system installed on the powder diffractometer at the 11-BM beamline of APS are presented.

Structure, doping and superconductivity in HgBa2CaCu2O6+δ (Tc ⩽ 128 K)

Abstract We have studied the defect structure and superconducting propertiess of HgBa2CaCu2O6+δ by neutron powder diffraction, AC susceptibility and DC resistivity. An as-synthesized sample has an onset Tc of 128 K, the highest yet reported for this material. The critical temperature decreases slightly (126 K) after oxygenation, and drops to 92 K after reduction in flowing argon. Neutron diffraction data give evidence that the primary doping mechanism in this material is provided by oxygen atoms in an interstitial position, similar to the case of the one-layer compound HgBa2CuO4+δ. The occupancy of this site varies from 0.08 (1) for the argon-reduced sample to 0.22 (1) for the oxygenated sample. Unlike the case of the one-layer compound, no evidence of an additional defect site was found in these samples. HgBa2CaCu2O6+δ has remarkably long copper-apical oxygen distances and almost perfectly flat CuO2 planes.

Electronic and magnetic properties of rare-earth ions in REBa2Cu3O7-x (RE=Dy, Ho, Er)☆

Abstract Heat capacity, resistivity, and magnetic susceptability data have been obtained for the compounds REBa2Cu3O7-x, where RE = Dy, Ho or Er. Neutron diffraction data on the Ho compound show a structure identical to that of YBa2Cu3O7-x. Magnetic transitions are observed at Tm=0.95, 0.17 and 0.59 K for Dy, Ho and Er compounds, respectively. It is argued that these are due predominantly to dipolar interactions. Resistivity data show that the magnetic state is coexistent with superconductivity in all cases. From the heat capacity data, the degeneracies of the crystal field ground states are determined, and estimates are given for the magnetic moment in the ground state and the energy separation of the first excited crystal field state.

An energy dispersive x-ray absorption spectroscopy beamline, X6A, at NSLS

An energy dispersive x‐ray absorption spectroscopy instrument has been built at the X6A beam port of the x‐ray ring at the National Synchrotron Light Source (NSLS). This instrument allows the collection of extended x‐ray‐absorption fine structure and/or x‐ray absorption near‐edge structure spectra for many elements on the millisecond time scale. The beamline employs a four‐point crystal bender and a rectangular Si 220 crystal to access incident energies between 6.5 and 21 keV. Because the polychromator focuses the synchrotron beam to a narrow 100‐μm line, this experimental apparatus is ideal for x‐ray absorption spectroscopy experiments in special environments such as at high pressures, for in situ experiments, and/or for very small samples. In this manuscript we will describe the instrument design and present data with which to evaluate the instrument. This beamline is available through the NSLS user proposal system.

Levitation apparatus for structural studies of high temperature liquids using synchrotron radiation

A new levitation apparatus coupled to a synchrotron-derived x-ray source has been developed to study the structure of liquids at temperatures up to 3000 K. The levitation apparatus employs conical nozzle levitation using aerodynamic forces to stably position solid and liquid specimens at high temperatures. A 270 W CO2 laser was used to heat the specimens to desired temperatures. Two optical pyrometers were used to record the specimen temperature, heating curves, and cooling curves. Three video cameras and a video recorder were employed to obtain and record specimen views in all three dimensions. The levitation assembly was supported on a three-axis translation stage to facilitate precise positioning of the specimen in the synchrotron radiation beam. The levitation system was enclosed in a vacuum chamber with Be windows, connections for vacuum and gas flow, ports for pyrometry, video, and pressure measurements. The vacuum system included automatic pressure control and multi-channel gas flow control. A phos...

Structural Characterization and Band Electronic Structure of α-(BEDT-TTF)2I3 below its 135 K Phase Transition

Abstract The nature of the 135 K metal-insulator (MI) transition in α-(BEDT-TTF)2l3, abbreviated α-(ET)2l3, was examined by determining the crystal structures above (298 K) and below (120 K) the phase transition and also by calculating the band electronic structures at both temperatures. This study demonstrates that both the crystal and band electronic structures of α-(ET)2l3 change only slightly upon passing through the MI transition. Within each sheetlike network of ET radical cations, the magnitudes of interactions between adjacent pairs of ET molecules (i-j) above and below the MI transition temperature (T MI) were evaluated by calculating their interaction energies, β ij = ⟨Ψ, H off|Ψ⟩, where Ψ1); and Ψ1 are the HOMOs of ET molecules i and j, respectively. The band electronic structures calculated by using single-zeta Slater type orbitals show that α-(ET)2l3 is a semiconductor with band gaps of 13 meV (298 K) and 35 meV (120 K). Thus, within the one-electron model, the apparently metallic properties...

Charge-Transfer Salts Derived from the New Electron-Donor Molecule BEDO-TTF: ESR, Superconductivity and Electrical Properties, and Crystal and Band Electronic Structure

Abstract Charge transfer salts of bis(ethylenedioxy)tetrathiafulvalene, BEDO-TTF, namely (BEDO-TTF)2AuBr2, and charge transfer salts (BEDO-TTF)mXn where X− is I3, AuI2 −, Au(CN)2−, ClO4 −, BrO4 −, BF4 −, PF6 −, AsF6 −, NO3 −, C(CN)3 −, and HgBr3− have been synthesized. The AuBr2− salt is the first BEDO-TTF salt to be structurally characterized. Crystallographic investigations of several of the other (BEDO-TTF)mXn salts have shown that (with the exception of the I3− salt) these new synmetals are structurally very similar to (BEDO- TTF)2AuBr2. Therefore, a 2:1 stoichometry is expected for BEDO-TTF salts. The observation of similar ESR linewidths for all the BEDO-TTF salts reinforces this conclusion. While (BEDO-TTF)2PF6 is semiconducting and the AuBr2−, Au(CN)2−, and ClO4− salts are metallic only near room temperature and semiconducting at low temperatures, (BEDO-TTF)2AuI2 shows metallic conductivity to low temperatures. RF penetration depth measurements on crystals derived from BEDO-TTF/KSCN/CuSCN show the...