Crystal structure of the twinned tetramethylurea adduct of 2-phenyl-1,3-dioxa-2-borolane-4,5-dione

The title compound crystallizes in the monoclinic space groupP2₁/c. Twinning occurs between domains sharing thehk0 zone. The indices of imprecise intensity data were interpreted successfully. A subset of these data could be corrected and used in structure determination together with single-crystal intensity data of the predominant domain, whereas the remaining superposition data were excluded from refinement. Structure solution converged at satisfactory values ofR=0.082,R _w=0.074. The structure consists of isolated Lewis acid base adducts.     

Two ammonium tetrachloridoaluminate salts: how a twinned orthorhombic structure emulates a trigonal crystal system

We have determined the crystal structures of two tetrachloridoaluminate salts. Tetrabutylammonium tetrachloridoaluminate benzene hemisolvate, (C₁₆H₃₆N)[AlCl₄]·0.5C₆H₆, (I), crystallizes with discrete cations, anions and solvent molecules. The benzene molecule is located on a centre of inversion. The structure of the benzene‐free polymorph has been determined previously. Tetraethylammonium tetrachloridoaluminate, (C₈H₂₀N)[AlCl₄], (II), also crystallizes with discrete cations and anions, and forms crystals which appear trigonal but are actually orthorhombic. With the additional reflections of the second and third domains of this nonmerohedral twin, a trigonal lattice is emulated, although the correct crystal system is orthorhombic.     

Unit-cell intergrowth of pyrochlore and hexagonal tungsten bronze structures in secondary tungsten minerals

Structural relations between secondary tungsten minerals with general composition A_x[(W,Fe)(O,OH)₃]_·yH₂O are described. Phyllotungstite (A=predominantly Ca) is hexagonal, , , space group P6₃/mmc. Pittongite, a new secondary tungsten mineral from a wolframite deposit near Pittong in Victoria, southeastern Australia (A=predominantly Na) is hexagonal, , , space group P-6m2. The structures of both minerals can be described as unit-cell scale intergrowths of (111)_py pyrochlore slabs with pairs of hexagonal tungsten bronze (HTB) layers. In phyllotungstite, the (111)_py blocks have the same thickness, 6 Å, whereas pittongite contains pyrochlore blocks of two different thicknesses, 6 and 12 Å. The structures can alternatively be described in terms of chemical twinning of the pyrochlore structure on (111)_py oxygen planes. At the chemical twin planes, pairs of HTB layers are corner connected as in hexagonal WO₃.     

How Much Water Does Calcined Gypsum Contain?

Ordered water : Gypsum has been used for construction for millennia. The structure and water content of calcined gypsum, CaSO₄?0.5 H₂O, has been under discussion until now: single‐crystal structure analysis (see picture: S yellow, Ca gray, O blue, H red) provides an ordered model that is confirmed by DFT calculations.

     

Establishing the microstructure-strengthening correlation in severely deformed surface of titanium

Surface nanostructuring of engineering materials can be utilised to enhance materials performance for various applications. The aim of this work was to investigate the evolution of microstructure and its correlation with strengthening mechanisms in nanocrystalline commercially pure titanium (cp-Ti) produced by surface mechanical attrition treatment (SMAT). The individual contributions of dislocation slip and twining as the deformation mechanisms during SMAT have been quantified using X-ray line profile analysis and corroborated with transmission electron microscopy and electron backscattered diffraction techniques. It is found that twining is operative only in the early stages of deformation. The absence of twin–twin intersections suggests that twining is not directly responsible for the initial refinement of grain size. Dislocation slip is the major deformation mode, which leads to the refinement of the microstructure by forming low-angle lamellar boundaries. Continuous dynamic recrystallisation is demonstrated to be the mechanism of nanocrystallisation in cp-Ti using detailed microscopic analysis. In contrast to previous studies, which have neglected the contribution of Taylor strengthening, it is observed that a combination of Hall–Petch and Taylor relationships can explain the strength only if separate set of parameters K (Hall–Petch constant) and α (geometrical factor in Taylor relationship) are used for the nanocrystalline surface and severely deformed sub-surface of cp-Ti. Taken together, this work provides new insights into the underlying mechanisms for engineering nanocrystalline materials.     

Effect of initial orientation on the tensile properties of commercially pure titanium

Effect of crystallographic texture on uniaxial tensile deformation of commercially pure titanium was studied using in situ as well as post-mortem electron backscatter diffraction and elastoplastic self-consistent simulations. Correlation of mechanical properties and strain hardening response with deformation micromechanisms like different modes of slip and twinning was established. Tensile specimens were machined along rolling direction in the plane perpendicular to normal and transverse direction (sample A and C, respectively) as well as along transverse direction in the plane normal to rolling direction (sample B) to obtain different initial texture from cold rolled and annealed plate of commercially pure titanium. Sample B showed higher strength but lower strain hardening rate and ductility than the orientations A and C. It showed extension twinning with lateral thickening while the other samples showed coexistence of extension and contraction twinning. Schmid factor accounted for most of the observed twinning although some contraction twinning in sample A is attributed to the effect of internal stresses. A combination of in situ tensile test in a field emission gun scanning electron microscope with electron backscatter diffraction facility and elastoplastic self-consistent simulations aid in obtaining high-fidelity Voce hardening parameters for different slip and twinning systems in commercially pure titanium. The variation in tensile properties can be explained on the basis of propensity of twinning which tends to provide strain hardening at lower strain but contributes to failure at higher strain.