Atomic-scale quantification of grain boundary segregation in nanocrystalline material.

Grain boundary segregation leads to nanoscale chemical variations that can alter a material's performance by orders of magnitude (e.g., embrittlement). To understand this phenomenon, a large number of grain boundaries must be characterized in terms of both their five crystallographic interface parameters and their atomic-scale chemical composition. We demonstrate how this can be achieved using an approach that combines the accuracy of structural characterization in transmission electron microscopy with the 3D chemical sensitivity of atom probe tomography. We find a linear trend between carbon segregation and the misorientation angle ω for low-angle grain boundaries in ferrite, which indicates that ω is the most influential crystallographic parameter in this regime. However, there are significant deviations from this linear trend indicating an additional strong influence of other crystallographic parameters (grain boundary plane, rotation axis). For high-angle grain boundaries, no general trend between carbon excess and ω is observed; i.e., the grain boundary plane and rotation axis have an even higher influence on the segregation behavior in this regime. Slight deviations from special grain boundary configurations are shown to lead to unexpectedly high levels of segregation.

Three-dimensional EBSD study on the relationship between triple junctions and columnar grains in electrodeposited Co-Ni films.

Electrodeposited nanocrystalline materials are expected to have a homogeneous grain size and a narrow grain size distribution. In Co-Ni electrodeposited films, however, under certain conditions an undesired columnar grain structure is formed. Fully automated three-dimensional (3D) orientation microscopy, consisting of a combination of precise material removal by focussed ion beam and subsequent electron backscatter diffraction (EBSD) analysis, was applied to fully characterize the grain boundaries of these columnar grains in order to gain further understanding on their formation mechanisms. Two-dimensional orientation microscopy on these films indicated that the development of columnar grains could be related to the formation of low-energy triple junctions. 3D EBSD allowed us to verify this suggestion and to determine the boundary planes of these triples. The triplets are formed by grain boundaries of different quality, a coherent twin on the {1011} plane, an incoherent twin and a large-angle grain boundary. These three boundaries are related to each other by a rotation about the <1120> direction. A second particularity of the columnar grains is the occurrence of characteristic orientation gradients created by regular defects in the grain. Transmission electron microscopy was applied to investigate the character of the defects. For this purpose, a sample was prepared with the focussed ion beam from the last slice of the 3D EBSD investigation. From the TEM and 3D EBSD observations, a growth mechanism of the columnar grains is proposed.

EBSD as a tool to identify and quantify bainite and ferrite in low-alloyed Al-TRIP steels.

Bainite is thought to play an important role for the chemical and mechanical stabilization of metastable austenite in low-alloyed TRIP steels. Therefore, in order to understand and improve the material properties, it is important to locate and quantify the bainitic phase. To this aim, electron backscatter diffraction-based orientation microscopy has been employed. The main difficulty herewith is to distinguish bainitic ferrite from ferrite because both have bcc crystal structure. The most important difference between them is the occurrence of transformation induced geometrically necessary dislocations in the bainitic phase. To determine the areas with larger geometrically necessary dislocation density, the following orientation microscopy maps were explored: pattern quality maps, grain reference orientation deviation maps and kernel average misorientation maps. We show that only the latter allow a reliable separation of the bainitic and ferritic phase. The kernel average misorientation threshold value that separates both constituents is determined by an algorithm that searches for the smoothness of the boundaries between them.

On the formation mechanisms, spatial resolution and intensity of backscatter Kikuchi patterns.

The present paper is divided into two main sections. In the first, the formation mechanisms of backscatter Kikuchi patterns (BKP) are discussed on the basis of measurements on the sharpness of Kikuchi lines and on the spatial, that means the lateral and depth resolution of the technique. We propose that thermal diffuse scattering is the important incoherent scattering mechanism involved in pattern formation. This mechanism is not considered in the classical description of the origin of backscattered electrons in the scanning electron microscope (SEM) which is why there is in some important points no agreement between classical Monte-Carlo-type electron trajectory simulations and experimental results. We assume that the energy spectrum of the backscattered electrons shows, similar to the spectra in transmission electron microscopy, a sharp zero-loss peak. In the second section, we discuss the intensity of Kikuchi bands in BKP. It is shown that the kinematical theory gives-of course-not the correct intensities, but that these intensities are, on the other hand, not too far off the experimental ones. We subsequently introduce a simple intensity correction procedure that is based on the two-beam dynamical theory, originally proposed by Blackman for transmission electron diffraction patterns. It is shown by examples of diffraction patterns of niobium and silicon that this procedure leads to satisfying results, once two unknown variables (a universal constant and the exit depth of the electrons) have been empirically fit. It is assumed that in the future, this correction will improve the possibilities of phase identification by backscatter Kikuchi diffraction patterns.