This paper is a study of the microstructure and other selected properties of solid-state, high-speed, rotary friction-welded tungsten and mild steel (S355) joints. Due to the high affinity of tungsten for oxygen, the welding process was carried out in a chamber with an argon protective atmosphere. Joints of suitable quality were obtained without any macroscopic defects and discontinuities. Scanning electron microscopy (SEM) was used to investigate the phase transformations taking place during the friction welding process. Chemical compositions in the interfaces of the welded joints were determined by using energy dispersive spectroscopy (EDS). The microstructure of friction welds consisted of a few zones, fine equiaxed grains (formed due to dynamic recrystallization) and ultrafine grains in the region on the steel side. A plastic deformation in the direction of the flash was visible mainly on the steel side. EDS-SEM scan line analyses across the interface did not confirm the diffusion of tungsten to iron. The nature of the friction welding dissimilar joint is non-equilibrium based on deep plastic deformation without visible diffusive processes in the interface zone. The absence of intermetallic phases was found in the weld interface during SEM observations. Mechanical properties of the friction-welded joint were defined using the Vickers hardness test and the instrumented indentation test (IIT). The results are presented in the form of a distribution in the longitudinal plane of the welded joint. The fracture during strength tests occurred mainly through the cleavage planes at the interface of the tungsten grain close to the friction surface.
The structural and luminescence properties of a new material, Ca10.5−xNix(VO4)7, formed by substitution of a fraction of calcium by nickel, are studied as a function of the Ni content (x). The powder X-ray diffraction results for the polycrystals, synthesized using a solid-state reaction method, show that in the studied temperature range (300–1150 K), the structure of the unsubstituted material (space group R3c, whitlockite--Ca3(PO4)2 structure type) is conserved up to the solubility limit, x = 0.72(2), determined on the basis of variation of unit cell size with x. The samples of nominal composition exceeding this limit contain a significant amount of the impurity phase.The structural refinements demonstrate that Ni atoms preferentially occupy the M5 site (one of the five independent Ca sites, M1–M5). The unit cell size was equally studied in the range of 300–1150 K, leading to the determination of the thermal expansion coefficients. It was found that with rising Ni content, the room temperature volumetric thermal expansion decreases from 41.80 MK−1 (x = 0.16) to 39.24 MK−1 (x = 0.66) and to 38.92 MK−1 at the solubility limit, this reduction being in line with earlier reported data for x=0. In the unit cell variation, around 800–900 K, a weak anomaly is observed, detectable most clearly for the axial ratio; it is also visible at thermal expansion coefficient temperature dependence. Substitution of Ca by Ni ions reduces the optical band gap of Ca10.5−xNix(VO4)7 from 3.56 (x = 0) to 3.29 and 3.16 eV observed for Ni-containing samples (x = 0.33 and 0.66, respectively). Observed bands in the absorption and photoluminescence spectra are assigned to electronic transitions in both VO groups and Ni2+ ions, confirming that Ni mainly occupies the M5 site. The band gap narrowing and decrease in photoluminescence intensity when the Ni concentration increases makes Ni-substituted compounds attractive for application, e.g., as photocatalysts.
The crystal structure and thermal expansion are determined for Ca 10 TM 0.5 (VO 4 ) 7 (TM = Co, Cu) orthovanadates. We find a correlation of the behavior of unit cell volume plotted against the ionic radius for these compounds and isostructural phosphates.