Crystal structures of R2Pd2Pb (R = Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, and Lu) compounds

The crystal structures of the R₂Pd₂Pb (R=Y, La, Ce, Pr, Nd, Sm, Gd, Tb, Dy, Ho, Er, Tm, and Lu) compounds were determined using X-ray powder diffraction. The investigated compounds crystallize with Mo₂FeB₂ structure type (space group P4/mbm, Pearson code tP10). The importance of stabilization by polar intermetallic R–Pd bonding is underscored by a bonding analysis derived from electronic band structure calculations.     

Determination of the structure of UFe2Al10 compound

The atomic structure of a new ternary phase UFe₂Al₁₀ appearing in the U–Fe–Al system was determined using direct methods applied to X-ray powder diffraction data. High resolution electron microscopy combined with the methods of crystallographic image processing was used for the verification of the structural model. The UFe₂Al₁₀ phase is orthorhombic and belongs to Cmcm space group, its unit cell contains 40 Al, eight Fe, and four U atoms. The lattice parameters obtained after Rietveld refinement are: a=8.919 Å, b=10.208 Å, and c=9.018 Å. The reliability factors characterizing the Rietveld refinement procedure are: R_p=5.9%, R_wp=8.1%, and R_b=2.9%.     

Growth and dielectric properties of Ca3NbGa3Si2O14 crystals

A new langasite type single crystal Ca₃NbGa₃Si₂O₁₄ (CNGS) was grown by Czochralski (CZ) method. The structure of CNGS crystal was determined by X-ray powder diffraction, the lattice parameters were a=0.8087 ± 0.0001 nm, c=0.4974 ± 0.0002 nm, V=0.2817 ± 0.0002 nm³; The congruency of CNGS was examined by measuring the chemical composition of the grown crystal by quantitative X-ray fluorescent (XRF) analysis. The melting point of CNGS crystal was measured by using the differential scanning calorimetry (DSC). Dielectric properties of (1 1 0) wafer plate were studied in the temperature range from 298.15 to 873.15 K; the frequency dependence of dielectric loss in the frequency range 10 Hz–13 MHz was measured.     

Features of the HDDR process in R–Fe–B ferromagnetic alloys (R is a mixture of Nd, Pr, Ce, La, Dy and others)

Features of the conventional hydrogenation, disproportionation, desorption, recombination (HDDR) and solid-HDDR processes in some R–Fe–B (R is a mixture of Nd, Pr, Ce, La, Dy) ferromagnetic alloys were studied in the temperature range 20–990 °C and pressure range from 1×10⁻³ Pa to 0.1 MPa. This was carried out by means of differential thermal analysis (DTA), X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM) methods. The hydride of the initial phase is formed by heating to 115 °C. The disproportionation of the alloys occurs in the temperature range from 320 to 800 °C. Φ-phase constitutes the base of the initial alloys. Among the disproportionation products, R-hydride, -Fe and two borides (Fe₂B and R_1.1Fe₄B₄) were revealed. The initial phase in all the alloys is recovered after heating in vacuum to a temperature of 990 °C. Full hydrogen desorption occurs in two temperature ranges with the peaks at 200–320 and 630–715 °C.     

Achieving tensile superplasticity in 8 mol% Y2O3 cubic stabilized ZrO2 through the addition of intergranular silica

The addition of 5 wt.% SiO₂, a viscous second phase, to 8 mol% Y₂O₃ cubic stabilized ZrO₂ (8Y-CSZ) made superplastic 8Y-CSZ. This material had a fine grain size of 0.4 μm and exhibited deformations in tension as large as 520% at 1430 °C with a strain rate of 1.0 × 10⁻⁴ s⁻¹.     

Ba3YB3O9: phase transition and crystal structure

A new modification of the compound Ba₃YB₃O₉, β phase, has been attained through solid phase transition from phase at 1125–1134 °C. β-Ba₃YB₃O₉ crystallizes in the hexagonal space group with cell parameters a=13.0529(8) Å, c=9.5359(9) Å. The crystal structure of -Ba₃YB₃O₉ has been determined from powder X-ray diffraction (XRD) data. The refinement was carried out using the Rietveld methods and the final refinement converged with R_p=8.8%, and R_wp=11.8% with R_exp=5.65%. In its structure, the isolated [BO₃]³⁻ anionic groups are parallel to each other and distributed layer upon layer along the c-axis. The Y atoms are six-coordinated by the O atoms to form octahedra. The result of IR spectrum confirmed the existence of [BO₃]³⁻ triangular groups.     

The crystal structure and magnetic properties of the Gd6Cr4Al43 compound

The crystal structure of intermetallic compound Gd₆Cr₄Al₄₃ has been investigated by means of X-ray diffraction data (Ho₆Mo₄Al₄₃ structure type, space group P6₃/mcm, Pearson symbol hP106, a = 10.9144(7) Å, c = 17.7361(13) Å).

SQUID magnetic measurements carried out for the title compound point to the existence of two antiferromagnetic phase transitions observed at T_N1 = 19.0(1) K and T_N2 = 6.8(1) K, respectively.     

Preparation, thermal stability, and magnetic properties of Fe---Co---Zr---Mo---W---B bulk metallic glass

A bulk metallic glass (BMG) cylinder of Fe₆₀Co₈Zr₁₀Mo₅W₂B₁₅ with a diameter of 1.5 mm was prepared by copper mould casting of industrial raw materials. The amorphous state and the crystallization behavior were investigated by X-ray diffraction (XRD). The thermal stability parameters, such as glass transition temperature (T_g), crystallization temperature (T_x), supercooled liquid region (ΔT_x) between T_g and T_x, and reduced glass transition temperature T_rg (T_g/T_m) were measured by differential scanning calorimetry (DSC) to be 891, 950, 59 K, and 0.62, respectively. The crystallization process took place through a single stage, and involved crystallization of the phases -Fe, ZrFe₂, Fe₃B, MoB₂, Mo₂FeB₂, and an unknown phase, as determined by X-ray analysis of the sample annealed for 1.5 ks at 1023 K, 50 K above the DSC peak temperature of crystallization. Mössbauer spectroscopy was studied for this alloy. The spectra exhibit a broadened and asymmetric doublet-like structure that indicated paramagnetic behavior and a fully amorphous structure. -Fe was found in the amorphous matrix for a cylinder with a diameter of 2.5 mm. The success of synthesis of the Fe-based bulk metallic glass from industrial materials is important for the future progress in research and practical application of new bulk metallic glasses.     

Direct synthesis of MgCNi3 by mechanical alloying

MgCNi₃, an intermetallic compound with superconductivity, was synthesized from the Mg (or Mg₂Ni), Ni and graphite powders by mechanical alloying (MA). It is shown that the preliminary condition for the formation of MgCNi₃ is that Mg₂Ni must form in advance of MgCNi₃ in the MA process or be the starting component.     

Application of controlled and electrical discharge assisted mechanical alloying for the synthesis of nanocrystalline MgB2 superconducting compound

In this paper we present the results of our efforts to synthesize the nanocrystalline MgB₂ superconducting compound from elemental Mg and B powders by combination of controlled mechanical pre-alloying in a magneto-mill Uni-Ball-Mill 5 under shearing mode followed by electrical discharge (ED) assisted mechanical alloying (MA). There is no conclusive evidence of MgB₂ formation in the Mg-2B mixture using crystalline boron after controlled mechanical alloying (CMA) under protective argon or helium atmosphere as well as subsequent ED assisted alloying. There seems to be some XRD evidence of the strongest (1 0 1) MgB₂ peak presence in the Mg-2B mixture processed using both crystalline and amorphous boron after CMA under hydrogen as well as subsequent ED assisted alloying but this evidence is rather ambiguous. We postulate here that it is highly likely that a certain critical Mg nanograin size must be achieved before a successful reaction to form nanocrystalline MgB₂ is going to be completed. Following recent report by Gümbel et al. [Appl. Phys. Lett. 80 (2002) 2725] this critical value can be roughly estimated at 15 nm or less. Calculations of the Mg nanograin size in the present work show that only three Mg-2B powders ball milled under hydrogen meet this critical nanograin size criterion for the Mg phase. However, a massive formation of the β-MgH₂ hydride in these powders consumes the available Mg in the reaction with hydrogen which may leave inadequate concentration of Mg to form MgB₂ even though the nanograin size of Mg is sufficiently refined, say below 15 nm.     

Crystal structure and magnetic properties of ZnV2O4

We present structural and magnetic data on ZnV₂O₄ single crystals. Single crystal X-ray diffraction shows the measured crystals to be of very high quality, especially with respect to atomic order. The measured magnetic susceptibility resembles to that of a spin glass system, surprising for a translational invariant structure. The results are discussed in the framework of disorder in a magnetically frustrated lattice.     

X-ray diffraction study on formation of ErNbO4 powder

The formation of ErNbO₄ powder, prepared by calcining an Er₂O₃ (50 mol%) and Nb₂O₅ (50 mol%) powder mixture at 1100 and 1600 °C for different durations, was investigated by using X-ray diffraction. The experimental results have displayed that although the solid-state reaction had started to some extent when the mixture was pre-calcined at 1100 °C for a duration of 13 h, the two original phases Er₂O₃ and Nb₂O₅ still dominated the mixture. When the duration of the calcination reaction was increased to 120 h at the same temperature, the resultant mixture experienced a nearly complete phase transformation. Accordingly, the ErNbO₄ phase was dominant phase in the mixture. Nevertheless, a small portion of the raw powder still existed in the mixture. When the calcining temperature was elevated to 1600 °C, ErNbO₄ powder with higher purity could be obtained for a relatively much shorter duration (only up to several tens of hours). A simple formation mechanism of ErNbO₄, an elevated-temperature-assisted solid-state chemical reaction: Er₂O₃+Nb₂O₅2ErNbO₄, is suggested. In addition, the present experimental results offer important evidence for the formation of the additional phase ErNbO₄ induced in Er:LiNbO₃ crystals by vapour transport equilibration (VTE) treatment.     

LiSrGe2 and LiBaGe2: One-dimensional chains of in an unusual conformation

Two new isostructural intermetallic germanides, LiSrGe₂ and LiBaGe₂, were synthesized as single crystals from constituent elements in molten Na. They both crystallize in the space group Pnma (no. 62) with a = 7.142(1), b = 4.459(1), c = 11.550(2) Å, Z = 4, and a = 7.381(1), b = 4.617(1), c = 11.837(1) Å, Z = 4, for LiSrGe₂ and LiBaGe₂, respectively. They contain one-dimensional anionic germanide chains, , running along the a-axis. The chains are in an unusual zigzag-like conformation, with weakly alternating Ge–Ge bond lengths of 2.475(1) and 2.498(1) Å, and 2.473(1) and 2.525(1) Å, for LiSrGe₂ and LiBaGe₂, respectively. Extended Hückel calculations suggest that LiSrGe₂ is metallic: the Fermi level lies within bands having anti-bonding character.     

Effects of rapid solidification on the phase structures and electrochemical properties of a V3TiNi0.56Co0.14Nb0.047Ta0.047 alloy

The crystal structures and electrochemical properties of a V₃TiNi_0.56Co_0.14Nb_0.047Ta_0.047 alloy prepared by the melt-spinning method were studied. The rapidly solidified alloy consists of a major Vanadium-based solid solution phase and a secondary Ti₂Ni-based phase. The secondary phase exists between the dendritic arms of the major phase, showing a typical eutectic characteristic. With increasing cooling rate, the amount of the secondary phase decreases but the lattice parameters of both the major phase and the secondary phase show no obvious change. Because the disappearance of the catalytic effect of the secondary phase, the rapidly solidified alloy shows bad electrochemical properties except cycle stability.     

Ce2Ir5B2, a new structure type of ternary borides

The crystal structure of a new ternary boride Ce₂Ir₅B₂, space group , a=5.477(2) Å, c=31.518(5) Å, Z=6, V=818.79 Å, was refined down to R=0.0484, wR₂=0.1211 from single crystal X-ray diffraction data. This is the first representative of a new structure type of intermetallic compounds (an ordered variant of the binary Er₂Co₇ compound). The structure of Ce₂Ir₅B₂ is the stacking variant of the MgCu₂- and CeCo₃B₂-type slabs and belongs to the structural series with the general formula R_2+nM_4+3nX_2n (n=2).     

Crystal structure, thermal expansion and electrical properties of the new Al0.32ErGe2 compound

A new ternary compound Al_0.32ErGe₂ has been synthesized and studied from 298 K to 773 K using X-ray powder diffraction technique. Its structure has been determined at room temperature by Rietveld refinement of X-ray powder diffraction data. The ternary compound Al_0.32ErGe₂ crystallizes in the orthorhombic with the defect CeNiSi₂ structure type (space group Cmcm, a = 0.40701(2) nm, b = 1.60401(9) nm, c = 0.39240(2) nm, Z = 4 and D_calc = 8.326 g/cm³). The average thermal expansion coefficients , and of Al_0.32ErGe₂ are 1.72 × 10⁻⁵ K⁻¹, 1.11 × 10⁻⁵ K⁻¹ and 1.52 × 10⁻⁵ K⁻¹, respectively. The bulk thermal expansion coefficient is 4.35 × 10⁻⁵ K⁻¹. Electrical resistivity of Al_0.32ErGe₂ was measured between 5 K and 300 K.     

Synthesis and thermal stability of nano-crystalline vanadium disilicide

Nano-crystalline vanadium disilicide was successfully synthesized using vanadium tetrachloride and silicon as starting materials via reduction–silication route at 650 °C in the molten salt solution of magnesium chloride and sodium chloride in an autoclave. X-ray powder diffraction patterns indicated that the product was hexagonal VSi₂ (a=4.572 Å, c=6.372 Å). Transmission electron microscopy images showed that the particle size of the product was in the range of 40–60 nm in diameter. There was a strong absorption peak at 271 nm in the UV-Vis absorption spectra. The oxidation of nano-crystalline VSi₂ began to proceed at the temperature of 400 °C in air. But the product had high thermal oxidation stability below 1000 °C. It can be used as an antioxidation coating material.     

MmM5/Mg multi-layer hydrogen storage thin films prepared by dc magnetron sputtering

MmNi_3.5(CoAlMn)_1.5/Mg (here Mm denoted for mischmetal) multi-layer thin films were deposited on (0 0 1) Si substrate by direct current (dc) magnetron sputtering with dual-target. X-ray diffraction (XRD) and scanning electron microscopy analysis revealed that the microstructure of the MmNi_3.5(CoAlMn)_1.5 layer is amorphous and/or nanocrystalline and that the microstructure of the Mg layer is fine grained crystalline with preferential orientation. Phase analysis of hydrogenated and dehydrogenated MmNi_3.5(CoAlMn)_1.5/Mg multi-layer thin films proved that an apparent absorption of hydrogen in the Mg layer occurs at temperatures higher than 200 °C and that the hydrogen absorbed can be fully released at 250 °C.     

Structural, thermodynamic, and electrochemical properties of TixZr1−x(VNiCrMnCoAl)2 C14 Laves phase alloys

The crystal structure of the monoclinic phase η-Al₁₁Cr₂ of the space group C2/c, a ≈ 1.76 nm, b ≈ 3.05 nm, c ≈ 1.76 nm, β ≈ 90° [L.A. Bendersky, R.S. Roth, J.T. Ramon, D. Shechtman, Metall. Trans. A 22A (1991) 5] has been determined by single-crystal X-ray diffraction. The structure model, refined to a final R value of 0.0441, has the composition of Al_83.8Cr_16.2. a = 1.77348(10) nm, b = 3.04555(17) nm, c = 1.77344(10) nm, monoclinic angle β = 91.0520(12)°. There are 80 (66Al + 14Cr) independent atomic positions in a unit cell, of which all Cr atom sites and 8 Al atom sites have icosahedral coordination. These icosahedra are interconnected forming icosahedral chains along , (1 0 1) icosahedral layer blocks as well as a three-dimensional icosahedral structure.     

Tetragonal phase in the Mg–Ni–Sn system

Complementary metallographic and crystallographic characterisations of the Mg-rich corner of the Mg–Ni–Sn system are presented. In particular the Mg₇₅Ni₁₅Sn₁₀ phase, previously reported by Arcondo et al. [Hyperfine Interact. 66 (1991) 359] has been identified as a tetragonal phase by transmission electron microscopy and X-ray diffraction studies. The influence of this new phase, called Y-phase, on the glass forming ability of alloys with nearby composition is discussed.