Small-angle subgrain boundaries emanating from dislocation pile-ups in multicrystalline silicon studied with synchrotron white-beam X-ray topography

The formation of dislocation pile-ups and related small-angle subgrain boundaries in block-cast multicrystalline silicon for photovoltaic applications has been studied by means of white-beam X-ray topography (WB-XRT). For this purpose, samples sliced perpendicular and parallel to the growth direction have been investigated in reflection and transmission geometry, respectively. During the growth process of the silicon ingot, the dislocation density increases. WB-XRT measurements revealed the formation of small-angle subgrain boundaries. The subgrains have a slightly changed orientation related to a rotation of ～0.07–0.80° around an axis parallel to the growth direction. This tilt results from the high number of dislocations forming dislocation pile-ups and walls. The spacings between dislocations in such subgrain boundaries were found to be between 297 and 28 nm. A qualitative model for the formation of dislocation pile-ups is proposed.     

Broad spectrum element-specific X-ray imaging

In this article element-specific mapping using a broad-spectrum laboratory based X-ray source is reported. Element-specific and element-exempt images of silver nitrate and di-hydrated barium chloride have been obtained from raw images collected either side of the K-edges for silver and barium. The informed positioning of filters between the source and sample narrowed the X-ray spectra, thereby enhancing the final images. For barium, samples with a barium area density of less than 8×10⁻⁵ g mm⁻² have been analysed. The system used here can be employed for mapping the distribution of elements from the middle of the second row transition metals to the light lanthanides.     

Quantitative measurement of deformation-induced martensite in 304 stainless steel by X-ray diffraction

A single X-ray diffraction scan is effectively used for identifying and evaluating deformation-induced transformation in 304 austenitic stainless steel. Variations in grain size influence surface constraint and hence the through-thickness transformation response. The initial stage of transformation in this steel is most likely dominated by –martensite formation.     

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.     

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.     

The superposition of flow stress contributions in a precipitate hardened Ni-based alloy studied by strain rate sensitivity measurements

The strain rate sensitivity of the flow stress of underaged, peakaged and overaged samples of the γ′-hardened Ni-based superalloy Inconel X-750 has been measured. The experimental data are presented in the form of Haasen plots, which help to analyze the flow stress superposition rules. It was found that a progressive increase of the slope in the Haasen plot, during Stage II of work hardening, is correlated with the increase in the γ′-precipitate size. The analysis of the results was carried out in the framework of the theory developed by Kocks, Argon and Ashby (Kocks UF, Argon AS, Ashby MF. Prog Mater Sci, 1975;19:1) for two contributions to the flow stress. It was found that the square superposition rule leads to a slight curvature but more important, it predicts an increase of the effective slope in the Haasen plots in agreement with the experimental results.     

Microstructural evolution of some MgO–TiO2 and MgO–Al2O3 powder mixtures during high-energy ball milling and post-annealing studied by X-ray diffraction

High-energy dry ball-mill and post-anneal processing were applied to synthesize MgTiO₃ and Mg₂TiO₄ single crystalline phases from the predetermined compositions of MgO–TiO₂ powder mixtures. Also, the experiments were performed to show that it is possible to prepare MgAl₂O₄ single crystalline phase from the predetermined composition of MgO–Al₂O₃ powder mixture only by employing high-energy dry ball milling, i.e. without post-annealing the milled samples. In contrast, fully developed single crystalline powders of MgTiO₃ and Mg₂TiO₄ were obtained after post-annealing the milled samples for 1 h at 900 and 1200 °C, respectively.     

Crystal structure of Nax(MoO)5(P2O7)4 studied by synchrotron X-ray diffraction

The crystal structure of sodium pentamolybdyl tetradiphosphate Na_x(MoO)₅(P₂O₇)₄ has been determined from synchrotron diffraction data collected at 293 K on two microcrystals. The compound crystallizes in a monoclinic space group I 1 1 2/a (no. 15, setting 11), with unit cell parameters a = 22.905(3), b = 23.069(2), c = 4.8537(2) Å, γ = 90.641(9)° and a = 22.898(3), b = 23.056(2), c = 4.8551(2) Å, γ = 90.82(1)°, for crystals I and II, respectively. The structure is pseudo-tetragonal, and the crystals are pseudo-merohedrally twinned by 90° rotation around the c-axis. The structure closely resembles the previously reported Li-deintercalated Mo_1.3OP₂O₇ [V.V. Lisnyak, N.V. Stus, P. Popovich, D.A. Stratiychuk, Ya. Filinchuk, V.M. Davydov, J. Alloys Compd. 360 (2003) 81–84]. Comparison of the two structures led us to conclude that the Mo₂ and Mo₃ clusters were erroneously identified in Mo_1.3OP₂O₇. A revised structure of Mo_1.3OP₂O₇ contains a fully occupied oxygen site instead of the 16% occupied Mo(2) site, thus the revised formulae for the Li-deintercalated compound is (MoO)₅(P₂O₇)₄. In both structures, the (MoO)₅(P₂O₇)₄ framework strongly resembles the one in the earlier reported Ag(MoO)₅(P₂O₇)₄, while the location of Na and Ag atoms differ.