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This paper presents an investigation of the limitations and optimisation of energy dispersive X-ray (EDX) tomography within the scanning transmission electron microscope, focussing on application of the technique to characterising the 3D elemental distribution of bimetallic AgAu nanoparticles. The detector collection efficiency when using a standard tomography holder is characterised using a tomographic data set from a single nanoparticle and compared to a standard low background double tilt holder. Optical depth profiling is used to investigate the angles and origin of detector shadowing as a function of specimen field of view. A novel time-varied acquisition scheme is described to compensate for variations in the intensity of spectrum images at each sample tilt. Finally, the ability of EDX spectrum images to satisfy the projection requirement for nanoparticle samples is discussed, with consideration of the effect of absorption and shadowing variations.

Energy-dispersive X-ray (EDX) spectroscopy in the scanning transmission electron microscope (STEM) has been used to demonstrate the presence of size-dependent compositional variation for L1 2 -structured Ni 3 Al-type gamma-prime (γ′) precipitates within a commercial RR1000 Ni-based superalloy. This semi-quantitative elemental analysis has been achieved using electrochemical extraction of the γ′ precipitates from the γ matrix. The applicability of this approach to size-dependent compositional analysis of precipitates was confirmed by a comparison of the size distribution for the extracted precipitates with those present in traditional electropolished foil specimens in the size range 20–250 nm. By applying suitable thickness-dependent absorption-corrections we have demonstrated that the composition of γ′ precipitates in our material depends on the size of the precipitate in the range of 5 nm to 3 μm. In particular, the Al content was observed to increase in smaller γ′ precipitates while Ti and Ta contents are constant for all sizes of precipitate. Hf was observed to be present only in the largest precipitates. This type of local compositional information provides invaluable input to assess the accuracy of microstructural modelling for these complex alloys and provides new evidence supporting the importance of anti-site diffusion.

We report on the observability of valence bonding effects in aberration-corrected high resolution electron microscopy (HREM) images along the [0 1 0] projection of the mineral Forsterite (Mg 2 SiO 4 ). We have also performed exit wave restorations using simulated noisy images and have determined that both the intensities of individual images and the modulus of the restored complex exit wave are most sensitive to bonding effects at a level of 25% for moderately thick samples of 20–25 nm. This relatively large thickness is due to dynamical amplification of bonding contrast arising from partial de-channeling of 1s states. Simulations also suggest that bonding contrast is similarly high for an un-corrected conventional electron microscope, implying an experimental limitation of signal to noise ratio rather than spatial resolution.

Aberration corrected Transmission Electron Microscope (TEM) images can currently resolve information at significantly better than 0.1 nm. Aberration corrected imaging conditions seek to optimize the transfer of high-resolution information but in doing so they prevent the transfer of low spatial frequency information. To recover low spatial frequency information, aberration corrected images must be acquired at a large defocus which compromises high spatial frequency information transfer. In this paper we present two a posteriori solutions to this problem in which the information bandwidth in an exit wave reconstruction is increased. In the first we reconstruct the electron exit wavefunction from two focal series datasets, with different, uniform focal steps, experimentally demonstrating that the width of the transfer interval can be extended from 0.2 nm −1 (∼5 nm) to better than 10 nm −1 (0.1 nm). In the second we outline the use of a focal series recorded with a non-uniform focal step to recover a wider range of spatial frequencies without the need for a large number of images. Using simulated data we show that using this non-uniform focal step the spatial frequency interval for a five image data set may be increased to between 0.25 nm −1 (4 nm) and 8.3 nm −1 (0.12 nm) compared to between 0.74 nm −1 (1.4 nm) and 8.3 nm −1 (0.12 nm) for the standard focal series geometry.

The convergent beam electron diffraction (CBED) patterns of twisted bilayer samples exhibit interference patterns in their CBED spots. Such interference patterns can be treated as off-axis holograms and the phase of the scattered waves, meaning the interlayer distance can be reconstructed. A detailed protocol of the reconstruction procedure is provided in this study. In addition, we derive an exact formula for reconstructing the interlayer distance from the recovered phase distribution, which takes into account the different chemical compositions of the individual monolayers. It is shown that one interference fringe in a CBED spot is sufficient to reconstruct the distance between the layers, which can be practical for imaging samples with a relatively small twist angle or when probing small sample regions. The quality of the reconstructed interlayer distance is studied as a function of the twist angle. At smaller twist angles, the reconstructed interlayer distance distribution is more precise and artefact free. At larger twist angles, artefacts due to the moire structure appear in the reconstruction. A method for the reconstruction of the average interlayer distance is presented. As for resolution, the interlayer distance can be reconstructed by the holographic approach at an accuracy of ± 0 . 5 A, which is a few hundred times better than the intrinsic z -resolution of diffraction limited resolution, as expressed through the spread of the measured k -values. Moreover, we show that holographic CBED imaging can detect variations as small as 0 . 1 A in the interlayer distance, though the quantitative reconstruction of such variations suffers from large errors.

Focused ion beam (FIB) milling has evolved to be one of the most important Transmission Electron Microscope (TEM) site specific sample preparation techniques. However, this technique still poses challenges, such as the structural damage and potential curtaining issues often observed for thin TEM lamella. These artefacts can negatively affect the TEM analysis results. In particular, structures such as internal cracks and pores in FIB prepared TEM samples can often be damaged during sample preparation. This is commonly regarded as an unavoidable problem, even though microstructurally intact thin lamellae TEM samples are widely needed for the investigation of crack tips or pore morphologies in many different materials. This presents a strong driver for the development of innovative methods to overcome damage and curtaining issues during FIB sample preparation. Here we report on a new methodology developed to protect internal cracks and pores from ion beam damage. Our proposed method also mitigates curtaining issues, which often make TEM analysis more difficult. This method uses the FIB to sputter and redeposit material onto the edges of any cracks or pores in order to fill these features in-situ prior to lamella thinning. Case studies showcasing this method are presented, demonstrating the approach on a modular pure iron sample and on a porous laser treated Al/B4C composite sample. Our proposed ‘filling’ method has demonstrated a two key benefits; it preserves the integrity of the edges of any cracks and pores and it reducing curtaining. The results also demonstrate that this technique can be an alternative to conventional Gas Injection System (GIS) deposition for protecting the external top surface.