A set of hot rolled 7xxx aluminum alloys with modification of processing conditions were analyzed on their fatigue life time as well as the internal microstructure using 3D computed X-ray tomography with a lab scale scanner and optical microscopy. It is shown that for conventional hot rolling conditions many large (>300μm) casting pores were retained in the material. With modifications of the rolling conditions the size and density distribution of the retained casting pores were significantly reduced, leading to greatly improved fatigue life times.

Hierarchically porous materials are of interest in a wide range of applications. If the materials are electronic, or ionic conductors, such materials are of interest as electrodes for use in fuel cells. Using hierarchically porous silica as templates, we have demonstrated the formation of hierarchically porous metal and metal oxide structures. Through the control of the synthesis conditions, we have produced partial replicas ca. 1 cubic centimeter in volume, in which two macroporous networks are separated by a nanoporous membrane. The macroporous network in the silica template is known to be bicontinuous. Our underlying model predicts that the second, induced, macroporous network should be similarly bicontinuous.

Micrometer resolution X-ray tomography of the whole sample confirms that the synthesis produces one bicontinuous macroporous network, and is consistent with the existence of a second set of macropores. Preliminary experiments were carried out using FIB/SEM serial tomography to image the second macropore network, however, the length scale of the structures is such that this approach it is unable to firmly establish that the second macropore network is bicontinuous throughout the entire sample volume.

In this contribution, we report on a numerical study demonstrating how to realize Electrostatic Force Microscopy (EFM) tomography. Based on the Equivalent Charge Method, both force and force gradient between a buried object (or trapped charges) and the Atomic Force Microscope tip are calculated. The main idea is to scan the sample at different tip sample distances and obtain the position and charge value of the object using reconstruction algorithms. The quantitative analysis here presented is a first step toward tomography for samples presenting “dilute” point charges creating non correlated signals by the interpretation of EFM signals. Lateral resolution, sensitivity (i.e. ability to detect an object), performance and limitations of EFM are also discussed in the paper.

3D x-ray diffraction contrast tomography (DCT) is a non-destructive technique for the determination of grain shape and crystallography in polycrystalline bulk materials. Using this technique, a strontium titanate specimen was repeatedly measured between annealing steps.. A systematic analysis of the growth history of selected grains before and after the ex-situ annealing step allows to extract the topological and morphological changes during grain growth. Furthermore, misorientation as well as interface orientation information of the microstructure reconstructions have been determined. The interface normal distribution clearly shows a preference for (100) oriented interfaces in the selected grains when annealed at 1600°C. This observation can be connected to existent interfacial energy estimations resulting from capillarity vector reconstructions.

The presence of elongation, streak and blurring artifacts in tomograms recorded under a missing wedge of rotation angles presents a major challenge for the quantitative analysis of tomographic image data. We show that the missing wedge artifacts of standard reconstruction algorithms may be reduced by the innovative reconstruction technique DIRECTT. For the comparison of missing wedge artifacts we apply techniques from spatial statistics, which have been specifically designed to investigate the shape of phase boundaries in tomograms.

In this report, a method is discussed to perform successive milling on yttria-stabilized zirconia (YSZ), NiO-YSZ and Ni-alloy at the intervals of 85 nm 50 nm and 100 nm, respectively using a focused ion beam (FIB) followed by electron backscatter diffraction (EBSD) analysis on each slice. The EBSD data is then reconstructed to generate 3D volume. The 3D-EBSD band quality data is superimposed on inverse pole figure (IPF) grain orientation analysis to get a correlation with quality of band indexing. For the NiO-YSZ case, grain orientations and band quality factors were matched for grains ∼250 nm diameters producing a high resolution 3D-EBSD data. For this case, a pore space in 3D volume was visible due to nanocrystalline NiO-YSZ grain network. The advantages of 3D EBSD are discussed in the context of its applications to SOFC research community.

Zirconium alloys have been used as fuel cladding and structural fuel assembly components in nuclear reactors since the 1950s, and show a characteristic variation in oxidation rate and layered crack morphology during aqueous corrosion. It is common to associate the first phenomenon with the appearance of the second. We have used 3D serial sectioning to study the morphology and distribution of cracks in corroded ZIRLO samples at different stages of oxidation, and have shown that cracks nucleate and grow at all stages of the oxidation process not just at the kinetic transition. We have used this data to analyse the nucleation of cracks with reference to the shape of the oxide/metal interface and the distribution of second phase precipitates.

The mechanical behavior of nanocomposites is critically dependent on their structural composition. In this paper we use Focused Ion Beam (FIB) microscopy to prepare surfaces from a layered polymer nanocomposite for investigation using phase contrast atomic force microscopy (AFM). Phase contrast AFM provides mechanical information on the surface examined and, by combining with the sequential cross-sectioning of FIB, can extend the phase contract AFM into three dimensions.

We review the progress in the electron tomography of dislocation microstructures in the transmission electron microscope (TEM). Dislocation contrast is visible both in conventional TEM and scanning TEM (STEM) modes and, despite the complicated intensity variations, dislocation contrast can be isolated using computational filtering techniques prior to reconstruction. We find that STEM annular dark-field (STEM-ADF) imaging offers significant advantages in terms of dislocation contrast and background artifacts. We present several examples, both in semiconducting and metallic systems, illustrating the properties of 3D dislocations. We present the high-angle triple-axis (HATA) specimen holder where the diffraction condition can be chosen at will and dislocation tomograms of multiple reflections can be combined. 3D dislocations are analyzed in terms of dislocation density and dislocation nodal structures. Several avenues of study are suggested that may exploit the 3D dislocation data.

Focused ion beam (FIB) milling coupled with scanning electron microscopy (SEM) on the same platform enables 3D microstructural analysis of structures using FIB for serial sectioning and SEM for imaging. Since FIB milling is a destructive technique, the acquisition of multiple signals from each slice is desirable. The feasibility of collecting both an inlens backscattered electron (BSE) signal and an inlens secondary electron (SE) simultaneously from a single scan of the electron beam from each FIB slice is demonstrated. The simultaneous acquisition of two different SE signals from two different detectors (inlens vs. Everhart-Thornley (ET) detector) is also possible. Obtaining multiple signals from each FIB slice with one scan increases the acquisition throughput. In addition, optimization of microstructural and morphological information from the target is achieved using multi-signals. Examples of multi-signal FIB/SEM tomography from a dental implant will be provided where both material contrast from the bone/ceramic coating/Ti substrate phases and porosity in the ceramic coating will be characterized.