The physical properties of polycrystalline materials depend on their microstructure, which is the nano- to centimeter scale arrangement of phases and defects in their interior. Such microstructure depends on the shape, crystallographic phase and orientation, and interfacing of the grains constituting the material. This article presents a new non-destructive 3D technique to study centimeter-sized bulk samples with a spatial resolution of hundred micrometers: time-of-flight three-dimensional neutron diffraction (ToF 3DND). Compared to existing analogous X-ray diffraction techniques, ToF 3DND enables studies of samples that can be both larger in size and made of heavier elements. Moreover, ToF 3DND facilitates the use of complicated sample environments. The basic ToF 3DND setup, utilizing an imaging detector with high spatial and temporal resolution, can easily be implemented at a time-of-flight neutron beamline. The technique was developed and tested with data collected at the Materials and Life Science Experimental Facility of the Japan Proton Accelerator Complex (J-PARC) for an iron sample. We successfully reconstructed the shape of 108 grains and developed an indexing procedure. The reconstruction algorithms have been validated by reconstructing two stacked Co-Ni-Ga single crystals, and by comparison with a grain map obtained by post-mortem electron backscatter diffraction (EBSD).
A coupled diffusion-deformation, multiphase field model for elastoplastic materials is presented. The equations governing the evolution of the phase fields and the molar concentration field are derived in a thermodynamically consistent way using microforce balance laws. As an example of its capabilities, the model is used to study the growth of the intermetallic compound (IMC) Cu 6 Sn 5 during room-temperature aging. This IMC is of great importance in, e.g., soldering of electronic components. The model accounts for grain boundary diffusion between IMC grains and plastic deformation of the microstructure. A plasticity model with hardening, based on an evolving dislocation density, is used for the Cu and Sn phases. Results from the numerical simulations suggest that the thickness of the IMC layer increases linearly with time and that the morphology of the IMC gradually changes from scallop-like to planar, consistent with previous experimental findings. The model predicts that plastic deformation occurs in both the Cu and the Sn layers. Furthermore, the mean value of the biaxial stress in the Sn layer is found to saturate at a level of −8 MPa to −10 MPa during aging. This is in good agreement with experimental data.
The formation of titanium aluminides in Ti-Al elemental powder mixtures containing 25, 50 and 75 at.% Al, has been studied using differential scanning calorimetry (DSC). Phase evolution in the mixture was followed by heating the compacted samples up to 1273 K at 7.5 and 15 K min -1 . The cooled samples were characterized using X-ray diffraction, scanning electron microscopy and energy-dispersive spectroscopy. The results showed that the primary combustion product in all the samples was TiAl 3 , and the combustion reaction occurred below the melting point of aluminum only in Ti-rich samples. In Alrich samples (75 at.% Al), TiAl 3 was obtained as a porous, single-phase product after combustion. In samples containing 25 and 50 at.% Al, the combustion reaction was incomplete and the unreacted titanium particles were covered by a layer of TiAl 3 . In these samples, other intermetallic compounds such as TiAl 2 , TiAl and Ti 3 Al were observed to form upon heating beyond the combustion peak and are attributed to the solid-state reaction between unreacted titanium and TiAl 3 . Heating the samples with 25 at.% Al to 1273 K for an hour led to the formation of a homogenous Ti 3 Al product, while a multiphase product with a dominant TiAl phase was observed in samples containing 50 at.% Al. Calculations based on DSC data show that the formation of TiAl 3 through the reaction between solid titanium and molten aluminum is associated with an apparent activation energy of 195 ± 20 kJ mol -1 and an enthalpy of -114 ± 5 kJ mol -1 .
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