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Spain, I. L.

Publications and source records attributed to Spain, I. L..

Energy dispersive X-ray diffraction in the diamond anvil, high-pressure apparatus - Comparison of synchrotron and conventional X-ray sources

The use of both conventional fixed-anode X-ray sources and synchrotron radiation to carry out energy-dispersive X-ray diffraction experiments at high pressure in a diamond anvil cell, is discussed. The photon flux at the sample and at the detector for the two cases are compared and the results are presented in graphs. It is shown that synchrotron radiation experiments can be performed with nearly two orders of magnitude increase in data rate if superior detectors and detector electronics are available.

Spain, I. L.

Raman spectra of solid benzene under high pressure

Raman spectra of solid benzene have been measured at room temperature up to about 140 kbar, using the diamond anvil cell. Effort has been focused upon the lattice vibration spectra at pressures above that of phase II. It is found that a change in slopes occurs in the frequency-pressure curves at about 40 kbar. Furthermore, a new band appears above 90 kbar. These features probably correspond respectively to the II-III phase transition, which has been reported previously, and a III-IV phase transition, reported here for the first time.

Thiery, M.-M.

Simple collimator for use with diamond-anvil cells in a synchrotron beam

A simple double-slit system is described which allows a synchrotron beam to be collimated onto a small sample (approximately 150-micron diameter) in a diamond-anvil cell using remote control. The apparatus can be constructed easily and inexpensively, and allows the shutter positions to be monitored accurately using readily available electronic equipment. A desirable feature of the collimator is the relatively small time needed for adjustment.

Spain, I. L.

Experiments with phase transitions at very high pressure

A diamond anvil cell is described which was developed for studying hydrogen and other materials to pressure above 100 PGa, including measurements at low temperature. The benefits of X-ray diffraction using synchrotron radiation and using a fixed anode source are examined as well as the optimization of X-ray diffraction at low temperature. A Ge diode detector was incorporated into apparatus for measuring optical absorption, reflectance, and fluorescence in order to enable luminescence studies and Raman spectra were obtained. Results of experiments on Si, Ge, GaP, InAs, hydrogen, benzene, nitrogen, graphite, and the superconductor CeCu2Si2 are given.

Spain, I. L.

Experiments with phase transitions at very high pressure

Diamond cells were constructed for use to 1 Mbar. A refrigerator for cooling diamond cells was adapted for studies between 15 and 300 K. A cryostat for superconductivity studies between 1.5 to 300 K was constructed. Optical equipment was constructed for fluorescence, transmission, and reflectance studies. X-ray equipment was adapted for use with diamond cells. Experimental techniques were developed for X-ray diffraction studies using synchrotron radiation. AC susceptibility techniques were developed for detecting superconducting transitions. The following materials were studied: compressed solidified gases (Xe, Ar), semiconductors (Ge, Si, GaAs), superconductors (Nb3Ge, Nb3Si, Nb3As, CuCl), molecular crystals (I).

Spain, I. L.

Phase transitions in Group III-V and II-VI semiconductors at high pressure

The structures and transition pressures of Group III-V and II-VI semiconductors and of a pseudobinary system (Ga/x/In/1-x/Sb) have been investigated. Results indicate that GaP, InSb, GaSb, GaAs and possible AlP assume Metallic structures at high pressures; a tetragonal, beta-Sn-like structure is adopted by only InSb and GaSb. The rocksalt phase is preferred in InP, InAs, AlSb, ZnO and ZnS. The model of Van Vechten (1973) gives transition pressures which are in good agreement with measured values, but must be refined to account for the occurrence of the ionic rocksalt structure in some compounds. In addition, discrepancies between the theoretical scaling values for volume changes at the semiconductor-to-metal transitions are observed.

Yu, S. C.

Polymorphism and the crystal structures of InSb at elevated temperature and pressure

The paper presents polycrystalline X-ray diffraction data for three high-pressure phases of InSb. The study employed two types of diamond-anvil pressure cells. The X-ray diffraction parameters were recorded at different fixed pressures and temperatures on flat film. The experiment utilized Zr-filtered Mo radiation. The intensities were estimated from the X-ray photographs using a semiautomated microdensitometer.

Yu, S.-C.

High pressure phase transitions in tetrahedrally coordinated semiconducting compounds

New experimental results are reported for structural transitions at high pressure in several III-V compounds and two II-VI compounds. These data, together with earlier results, are then compared with the predictions of model calculations of Van Vechten. Experimental transition pressures are often at variance with calculated values. However, his calculation assumes that the high pressure phase is metallic, with the beta-Sn structure. The present results show that several compounds assume an ionic NaCl structure at high pressure, while others have neither the beta-Sn nor NaCl structure.

Yu, S. C.

Variable temperature pressure cell for polycrystalline X-ray studies down to 2 K - Application to Bi

A variable pressure diamond anvil cell is described for operation at temperatures continuously variable from 300 down to 2 K and controllable within 10 mK. Polycrystalline X-ray data are collected from the pressure cavity by means of either (1) standard photographic techniques, (2) diffractometer measurements, or (3) energy dispersive diffractometry. The facility has been used to examine parts of the phase diagram of Bi. Results from this study indicate that the Bi-I and Bi-III structures are retained to low temperatures; however, there is no evidence to support a structural transition from Bi-V to Bi-VIII.

Skelton, E. F.

Hall effect magnetometer

A magnetometer which uses a single crystal of bismuth selenide is described. The rhombohedral crystal structure of the sensing element is analyzed. The method of construction of the magnetometer is discussed. It is stated that the sensing crystal has a positive or negative Hall coefficient and a carrier concentration of about 10 to the 18th power to 10 to the 20th power per cubic centimeter.

Woollam, J. A.

Quantum limit studies in single-crystal and pyrolytic graphite

The occupied regions of momentum space in graphite are confined to very elongated volumes near the hexagonal Brillouin zone edges. The elongation is along the hexagonal axis (c axis) so that cross-sectional areas perpendicular to that axis are very small. Hence, when magnetic fields are applied parallel to the c axis only the n = 0 Landau levels remain below the Fermi energy for fields above 7 T (Woollam, 1971). The energy bands in graphite can be described by a set of seven parameters (McClure, 1971) (including the Fermi energy as a parameter). In a quantizing magnetic field the Landau levels are described by a secular equation determined by diagonalizing the Hamiltonian (McClure, 1960). A major unusual feature for the levels along the Brillouin zone edge is that the n = 0 Landau level for electrons is independent of magnetic field, while that for holes is field dependent.

Woollam, J. A.

Prospects for obtaining metallic hydrogen with spherical presses

Description of a split-sphere apparatus modified for use at low temperature and affording a possible method for compressing molecular hydrogen to a pressure in excess of 1 Mbar and for converting it to the metallic state. The construction costs of the apparatus are relatively low and the amount of liquid helium required for low-temperature operation is readily obtainable with modern liquefiers.

Spain, I. L.

Properties of crystalline bismuth selenide and its use as a Hall effect magnetometer

Single crystals of n-type Bi2Se3 grown by the Bridgman technique are found to make excellent Hall effect magnetometers. Plots of Hall resistivity sub yx against magnetic field B to 10 tesla are linear to within 1 percent. Furthermore, the slope of the sub yx against B curve varies by about 1 percent in the region 1.1 to 35 K and by less than 20 percent in the region 1.1 to 300 K. Analysis of galvanomagnetic measurements indicate the samples have semimetallic densities of approximately 10 to the 25th power/cu cm, with two band conduction and near carrier compensation. Reflectivity measurements suggest a band gap of approximately 0.08 eV for the samples. The temperature dependence of mobility is also measured. A series of 50 direct immersions into liquid helium and liquid nitrogen demonstrate the reliability of Bi2Se3 magnetometers for cryogenic use.

Wollam, J. A.

Mobility in single crystal Bi2Se3.

Galvanomagnetic effects are measured in p-type Bi2Se3 in magnetic fields to 8 tesla. Both Hall and conductivity mobilities are determined between 4.2 and 300 K. Carrier compensation, as well as nearly equal electron and hole mobilities are found in samples with approximately 10 to the 25th power per cu m 3 total carrier concentration.

Woollam, j. A.

Quantum limit studies in single crystal and pyrolytic graphite

The occupied regions of momentum space in graphite are confined to elongated volumes near the hexagonal Brillouin zone edges. The elongation is along the hexagonal axis (c-axis), so that cross sectional areas perpendicular to that axis are very small. When magnetic fields are applied parallel to the c-axis, only the n = 0 Landau levels remain below the Fermi energy for fields above 7 tesla. The energy bands in graphite can be described by a set of seven parameters (including the Fermi energy as a parameter). In a quantizing magnetic field the Landau levels are described by a secular equation determined by diagonalizing the Hamiltonian. A major feature for the levels along the Brillouin zone edge is that the n = 0 Landau level for electrons is independent of magnetic field, while that for holes is field-dependent.

Woollam, J. A.

Magnetometer uses bismuth-selenide

Characteristics of bismuth-selenide magnetometer are described. Advantages of bismuth-selenide magnetometer over standard magnetometers are stressed. Thermal stability of bismuth-selenide magnetometer is analyzed. Linearity of output versus magnetic field over wide range of temperatures is reported.

Woollman, J. A.