The charge density wave transition is investigated in the bi-layer family of rare earth tritelluride RTe3 compounds (R = Sm, Gd, Tb, Dy, Ho, Er, Tm) via high resolution x-ray diffraction and electrical resistivity. The transition temperature increases monotonically with increasing lattice parameter from 244(3) K for TmTe3 to 416(3) K for SmTe3. The heaviest members of the series, R = Dy, Ho, Er, Tm, are observed to have a second transition at a lower temperature, which marks the onset of an additional CDW with wavevector almost equal in magnitude to the first, but oriented in the perpendicular direction.
A molten Al flux method was used to grow single crystals of the type I clathrate compound Ba8Al14Si31. Single-crystal neutron diffraction data for Ba8Al14Si31 were collected at room temperature using the SCD instrument at the Intense Pulsed Neutron Source, Argonne National Laboratory. Single-crystal neutron diffraction of Ba8Al14Si31 confirms that the Al partially occupies all of the framework sites (R1 = 0.0435, wR2 = 0.0687). Stoichiometry was determined by electron microprobe analysis, density measurements, and neutron diffraction analysis. Solid-state (27)Al NMR provides additional evidence for site preferences within the framework. This phase is best described as a framework-deficient solid solution Ba8Al14Si31, with the general formula, Ba(8)Al(x)Si(42-3/4x)[](4-1/4x) ([] indicates lattice defects). DSC measurements and powder X-ray diffraction data indicate that this is a congruently melting phase at 1416 K. Temperature-dependent resistivity reveals metallic behavior. The negative Seebeck coefficient indicates transport processes dominated by electrons as carriers.
A hydrogen-encapsulated inorganic clathrate, which is stable at ambient temperature and pressure, has been prepared in high yield. Na5.5(H2)2.15Si46 is a sodium-deficient, hydrogen-encapsulated, type I silicon clathrate. It was prepared by the reaction between NaSi and NH4Br under dynamic vacuum at 300 degrees C. The Rietveld refinement of the powder X-ray diffraction data is consistent with the clathrate type I structure. The type I clathrate structure has two types of cages where the guest species, in this case Na and H2, can reside: a large cage composed of 24 Si, in which the guest resides in the 6d crystallographic position, and a smaller one composed of 20 Si, in which the guest occupies the 2a position. Solid-state 23Na, 1H, and 29Si MAS NMR confirmed the presence of both sodium and hydrogen in the clathrate cages. 23Na NMR shows that sodium completely fills the small cage and is deficient in the larger cage. The 1H NMR spectrum shows a pattern consistent with mobile hydrogen in the large cage. 29Si NMR spectrum is consistent with phase pure type I clathrate framework. Elemental analysis is consistent with the stoichiometry Na5.5(H2.15)2Si46. The sodium occupancy was also examined using spherical aberration (Cs) corrected scanning transmission electron microscopy (STEM). The high-angle annular dark-field (HAADF) STEM experimental and simulated images indicated that the Na occupancy of the large cage, 6d sites, is less than 2/3, consistent with the NMR and elemental analysis.
Single crystals of EuGa 2 Pn 2 (Pn=P, As) were grown from a molten Ga flux and characterized by single-crystal X-ray diffraction at 100(1) K. They are isostructural and crystallize in a new structure type (monoclinic, P2/m, a = 9.2822(9) Å , b=3.8967(4) Å , c=12.0777(11) Å , β=95.5220(10)°, R1 = 0.0148, wR2 = 0.0325 (EuGa 2 P 2 ) and a = 9.4953(7) Å , b = 4.0294(3) Å , c = 12.4237(9) Å , β = 95.3040(10)°, R1 = 0.0155, wR2 = 0.0315 (EuGa 2 As 2 )). The structures consist of alternating layers of two-dimensional Ga 2 Pn 2 anions and Eu cations. The anion layers are composed of Ga 2 Pn 6 staggered, ethane-like moieties having a rare Ga-Ga bonding motif; these moieties are connected in a complex fashion by means of shared Pn atoms. Both structures show small residual electron densities that can be modeled by adding a Eu atom and removing two bonded Ga atoms, resulting in structures (<2%) where most of the atoms are the same, but there is a difference in bonding that leads to one-dimensional ribbons of parallel Ga 2 Pn 6 staggered, ethane-like moieties. The compounds can be understood within the Zintl formalism, but show metallic resistivity. Magnetization measurements performed on single crystals show low-temperature magnetic anisotropy as well as multiple magnetic ordering events that occur at and below 24 and 20 K for the phosphorus and arsenic analogs, respectively. The magnetic coupling between Eu ions is attributed to indirect exchange via an RKKY interaction, which is consistent with the metallic behavior. The compounds display large negative magnetoresistance of up to -80 and -30%
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