X-Ray powder diffraction study of structural phase transitions in (Ba0.5Sr0.5)PbO3 perovskite

Study of structural properties of (Ba_0.5Sr_0.5)PbO₃ has been carried out in a wide temperature range from 10 to 1223 K using the X-ray powder diffraction technique. Two temperature-induced structural phase transitions at 948 and 1198 K have been found. For polycrystallines the XPS and electrical resistivity measurements have been performed.     

Alkyne oligomerization catalyzed by molybdenum(0) complexes

Three new molybdenum(0) complexes, [Mo(CO)₃(Hpz)₃] (1), [Mo(CO)₂(Hpz)₂(DMAD)₂] (2), (DMAD=dimethyl acetylenedicarboxylate) and [Mo(CO)₃(1-Me-imidazole)₃] (3) were synthesized and characterized. Their activity and selectivity in alkyne cyclotrimerization and co-trimerization reactions was investigated. The molecular structures of 1 and 2 have been determined by unconventional powder and standard single-crystal diffraction methods, respectively. 1 consists of a pseudo-octahedral complex of C₃ symmetry, with the ligands in fac disposition; complex 2, of idealized C₂ symmetry, is obtained by substitution of one CO and one pyrazole in 1 by two DMAD ligands, and shows the rare trans configuration of π-bound acetylenic moieties.     

Magnetic alignment in nominally non-magnetic hexagonal metal hydrides: NMR

Powders of three hexagonal metal-hydrides or -deuterides are found to align in 4.4–8.3 T magnetic fields used for NMR. The field-alignment is unexpected, since all three systems have very small susceptibilities, as demonstrated by sharp NMR lines. The extent of alignment runs from nearly complete to barely detectable in ZrBe₂(H,D)_x, LuD₃, and YD₃, respectively. The preferred alignment direction in ZrBe₂(H,D)_x is with the crystallites’ c-axis perpendicular to B, while the c-axis and B tend to be parallel in LuD₃ and YD₃. The susceptibilities χ_|| and χ are determined from bulk magnetization measurements in aligned ZrBe₂H_1.4 powder. The alignment must be considered for proper analysis of NMR spectra in these and related materials.     

Powder MAS NMR lineshapes of quadrupolar nuclei in the presence of second-order quadrupole interaction

We derive a complete analytical solution for the powder magic angle spinning (MAS) nuclear magnetic resonance (NMR) lineshape in the presence of second-order quadrupole interaction, considering a radiofrequency (rf) pulse of finite width, a finite MAS frequency, and a non-zero asymmetry parameter. I_x is calculated using two approaches. The first applies time-dependent perturbation theory in the presence of the rf pulse and stationary perturbation theory (SPT) in its absence. The second is based on the Magnus expansion of the density matrix in the interaction representation during the pulse and SPT in its absence. We solve the problem in the laboratory frame using the properties of the Fourier transform and spin operators. Diagonalisation is not required. Both approaches agree well with each other under all conditions and also with the transition probability approach for the central transition. The Magnus expansion exists at all times and the effect of the non-secular terms is negligible. We describe an analytical method of averaging I_x over the Euler angles and simulate the ¹¹B MAS NMR lineshapes for crystalline and vitreous B₂O₃. A critical analysis is given of all earlier calculations of the MAS NMR lineshape.     

Porosity, mechanical properties, residual stresses of supersonic plasma-sprayed Ni-based alloy coatings prepared at different powder feed rates

The aim of this paper was to investigate the effect of powder feed rate (PFR) on the microstructure and mechanical properties of the supersonic plasma-sprayed Ni-Cr-B-Si-C coatings. The microstructure, porosity and mechanical properties of the coatings and the residual stresses at the coating surfaces were experimentally determined. Results showed that the variations of porosity, elastic moduli and micro-hardness of the coatings followed Weibull distribution. From the statistical trend, the porosity of the coating increased with increasing PFR. However, the elastic modulus and the micro-hardness of the coating decreased and reached local minima and then increased with increasing PFR. Elastic modulus could be generally considered to be an increasing function of micro-hardness. The mean value of the elastic modulus of the coating calculated from Weibull plot was almost proportional to the square root of the mean value of the micro-hardness of the coating. Moreover, with increasing PFR, the residual stress at the coating surface, which was mainly governed by the elastic modulus of the coating, decreased to a local minimum and then increased.     

Synthesis of silicated hydroxyapatite Ca10(PO4)6−x(SiO4)x(OH)2−x

The preparation of silicated hydroxyapatite Ca₁₀(PO₄)_6−x(SiO₄)_x(OH)_2−x (SiHA) with 0?x?2 was investigated using a wet precipitation method followed by a heat treatment. X-ray diffraction and Rietveld refinement, Fourier transformed IR (FTIR) spectroscopy, elemental analyses, transmission electron microscopy and thermal analyses were used to characterize the samples. The raw materials were composed of a partially silicated and carbonated apatite and a secondary minor phase containing the excess silicon. Single phase silicated hydroxyapatites, with 0?x?1, could be synthesized after a thermal treatment of the raw powders above 700 °C. The presence of carbonate groups in the raw apatite played an important role in the incorporation of silicates during heating. From the different results, the mechanisms of formation of SiHA are discussed.     

X-ray structural study of intermetallic alloys RT2Si and RTSi2 (R=rare earth, T=noble metal)

Two series of intermetallic alloys, RT₂Si and RTSi₂, have been synthesized from stoichiometric compositions. The crystal structures of EuPt_1+xSi_2−x (CeNiSi₂-type), CeIr₂Si (new structure type), YbPd₂Si and YbPt₂Si (both YPd₂Si-type) have been elucidated from X-ray single crystal CCD data, which were confirmed by XPD experiments. The crystal structures of LaRh₂Si and LaIr₂Si (CeIr₂Si-type), {La,Ce,Pr,Nd}AgSi₂ (all TbFeSi₂-type), and EuPt₂Si (inverse CeNiSi₂-type) were characterized by XPD data. RT₂Si/RTSi₂ compounds were neither detected in as-cast alloys Sc₂₅Pt₅₀Si₂₅, Eu₂₅Os₂₅Si₅₀ and Eu₂₅Rh₂₅Si₅₀ nor after annealing at 900 °C. Instead, X-ray single crystal data prompted Eu₂Os₃Si₅ (Sc₂Fe₃Si₅-type) and EuRh_2+xSi_2−x (x=0.04, ThCr₂Si₂-type) as well as a new structure type for Sc₂Pt₃Si₂ (own type).     

傅里叶变换红外光谱法研究核辐照对三七总皂苷粉成分的影响

采用傅里叶变换红外光谱(卷积谱)法对经不同剂量y-射线核辐照的三七总皂苷粉进行了对比研究.辐照剂量不高于9kGy时,三七总皂苷粉样品的化学成分几乎没有发生变化;三七总皂苷粉样品经15kGy及以上的辐照剂量辐照后,可能产生新的化学成分;经21kGy的剂量辐照,三七总皂苷粉产生了人参、三七粉所含的普通成分(非三七总皂苷成分...     

A new ferromagnetic hysteresis model for soft magnetic composite materials

A new ferromagnetic hysteresis model for soft magnetic composite materials based on their specific properties is presented. The model relies on definition of new anhysteretic magnetization based on the Cauchy-Lorentz distribution describing the maximum energy state of magnetic moments in material. Specific properties of soft magnetic composite materials (SMC) such as the presence of the bonding material, different sizes and shapes of the Fe particles, level of homogeneity of the Fe particles at the end of the SMC product treatment, and achieved overall material density during compression, are incorporated in both the anhysteretic differential magnetization susceptibility and the irreversible differential magnetization susceptibility. Together they form the total differential magnetization susceptibility that defines the new ferromagnetic hysteresis model. Genetic algorithms are used to determine the optimal values of the proposed model parameters. The simulated results show good agreement with the measured results.     

Investigations on the growing, cracking and spalling of oxides scales of powder metallurgy Rene95 nickel-based superalloy

The surface and cross-sectional morphologies of powder metallurgy (PM) Rene95 nickel-based superalloy after 100 h oxidation in the temperature range of 700-1100 °C were investigated. It is shown that oxides nucleate first on the surface of the alloy and form an oxides scale. Afterwards, oxides scale endures decohesion, rumpling, cracking and finally spalling owing to the weak cohesive strength of the scale/alloy interface. The XRD and EDS analyses confirmed that the oxides scale of PM Rene95 superalloy is mainly composed by Cr₂O₃ at 800 °C and NiCr₂O₄ is the main spinel at 1100 °C. The subsequent analysis of internal stress verified that cracking and spalling are caused by growth stress and promoted by thermal stress. On these bases, improvement of the cohesive strength of the scale/alloy interface is considered to be the main way to increase the oxidation resistance of PM Rene95 superalloy.