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In response to the requirements imposed by the COVID-19 pandemic in 2020, we developed a remote learning undergraduate workshop for 44 students at the University of Newcastle by embedding scanning electron microscope (SEM) images of Maratus (Peacock) spiders into the MyScope Explore environment. The workshop session had two main components: 1) to use the online MyScope Explore tool to virtually image scales with structural color and pigmented color on Maratus spiders; 2) to join a live SEM session via Zoom to image an actual Maratus spider. In previous years, the undergraduate university students attending this annual workshop would enter the Microscopy Facility at the University of Newcastle to image specimens with SEM; however, in 2020 the Microscopy Facility was closed to student visitors, and this virtual activity was developed in order to proceed with the educational event. The program was highly successful and constitutes a platform that can be used in the future by universities for teaching microscopy remotely.
Current reconstruction methodologies for atom probe tomography (APT) contain serious geometric artifacts that are difficult to address due to their reliance on empirical factors to generate a reconstructed volume. To overcome this limitation, a reconstruction technique is demonstrated where the analyzed volume is instead defined by the specimen geometry and crystal structure as determined by transmission electron microscopy (TEM) and diffraction acquired before and after APT analysis. APT data are reconstructed using a bottom-up approach, where the post-APT TEM image is used to define the substrate upon which APT detection events are placed. Transmission electron diffraction enables the quantification of the relationship between atomic positions and the evaporated specimen volume. Using an example dataset of ZnMgO:Ga grown epitaxially on c-plane sapphire, a volume is reconstructed that has the correct geometry and atomic spacings in 3D. APT data are thus reconstructed in 3D without using empirical parameters for the reverse projection reconstruction algorithm.
Covering a broad optical spectrum, ternary InxGa1−xAs nanowires, grown by bottom-up methods, have been receiving increasing attention due to the tunability of the bandgap via In composition modulation. However, inadequate knowledge about the correlation between growth and properties restricts our ability to take advantage of this phenomenon for optoelectronic applications. Here, three different InGaAs nanowires were grown under different experimental conditions and atom probe tomography was used to quantify their composition, allowing the direct observation of the nanowire composition associated with the different growth conditions.
In this work, we demonstrate a new system for the examination of gas interactions with surfaces via atom probe tomography. This system provides capability of examining the surface and subsurface interactions of gases with a wide range of specimens, as well as a selection of input gas types. This system has been primarily developed to aid the investigation of hydrogen interactions with metallurgical samples, to better understand the phenomenon of hydrogen embrittlement. In its current form, it is able to operate at pressures from 10−6 to 1000 mbar (abs), can use a variety of gasses, and is equipped with heating and cryogenic quenching capabilities. We use this system to examine the interaction of hydrogen with Pd, as well as the interaction of water vapor and oxygen in Mg samples.
Understanding oxide–metal interfaces is crucial to the advancement of materials and components for many industries, most notably for semiconductor devices and power generation. Atom probe tomography provides three-dimensional, atomic scale information about chemical composition, making it an excellent technique for interface analysis. However, difficulties arise when analyzing interfacial regions due to trajectory aberrations, such as local magnification, and reconstruction artifacts. Correlative microscopy and field simulation techniques have revealed that nonuniform evolution of the tip geometry, caused by heterogeneous field evaporation, is partly responsible for these artifacts. Here we attempt to understand these trajectory artifacts through a study of the local evaporation field conditions. With a better understanding of the local evaporation field, it may be possible to account for some of the local magnification effects during the reconstruction process, eliminating these artifacts before data analysis.
Correlative microscopy approaches offer synergistic solutions to many research problems. One such combination, that has been studied in limited detail, is the use of atom probe tomography (APT) and transmission Kikuchi diffraction (TKD) on the same tip specimen. By combining these two powerful microscopy techniques, the microstructure of important engineering alloys can be studied in greater detail. For the first time, the accuracy of crystallographic measurements made using APT will be independently verified using TKD. Experimental data from two atom probe tips, one a nanocrystalline Al–0.5Ag alloy specimen collected on a straight flight-path atom probe and the other a high purity Mo specimen collected on a reflectron-fitted instrument, will be compared. We find that the average minimum misorientation angle, calculated from calibrated atom probe reconstructions with two different pole combinations, deviate 0.7° and 1.4°, respectively, from the TKD results. The type of atom probe and experimental conditions appear to have some impact on this accuracy and the reconstruction and measurement procedures are likely to contribute further to degradation in angular resolution. The challenges and implications of this correlative approach will also be discussed.
The application of atom probe tomography to the study of minerals is a rapidly growing area. Picosecond-pulsed, ultraviolet laser (UV-355 nm) assisted atom probe tomography has been used to analyze trace element mobility within dislocations and low-angle boundaries in plastically deformed specimens of the nonconductive mineral zircon (ZrSiO4), a key material to date the earth’s geological events. Here we discuss important experimental aspects inherent in the atom probe tomography investigation of this important mineral, providing insights into the challenges in atom probe tomography characterization of minerals as a whole. We studied the influence of atom probe tomography analysis parameters on features of the mass spectra, such as the thermal tail, as well as the overall data quality. Three zircon samples with different uranium and lead content were analyzed, and particular attention was paid to ion identification in the mass spectra and detection limits of the key trace elements, lead and uranium. We also discuss the correlative use of electron backscattered diffraction in a scanning electron microscope to map the deformation in the zircon grains, and the combined use of transmission Kikuchi diffraction and focused ion beam sample preparation to assist preparation of the final atom probe tip.
Atom probe is a powerful technique for studying the composition of nano-precipitates, but their morphology within the reconstructed data is distorted due to the so-called local magnification effect. A new technique has been developed to mitigate this limitation by characterizing the distribution of the surrounding matrix atoms, rather than those contained within the nano-precipitates themselves. A comprehensive chemical analysis enables further information on size and chemistry to be obtained. The method enables new insight into the morphology and chemistry of niobium carbonitride nano-precipitates within ferrite for a series of Nb-microalloyed ultra-thin cast strip steels. The results are supported by complementary high-resolution transmission electron microscopy.
Atom probe tomography (APT) provides three-dimensional analytical imaging of materials with near-atomic resolution using pulsed field evaporation. The processes of field evaporation can cause atoms to be placed at positions in the APT reconstruction that can deviate slightly from their original site in the material. Here, we describe and model one such process—that of preferential retention of solute atoms in multicomponent systems. Based on relative field evaporation probabilities, we calculate the point spread function for the solute atom distribution in the “z,” or in-depth direction, and use this to extract more accurate solute concentration profiles.
Transmission electron microscope samples of two types of metal matrix composites were prepared using both traditional thinning methods and the more novel focused ion beam miller. Electropolishing methods were able to produce, very rapidly, thin foils where the matrix was electron transparent, but the ceramic reinforcement particles remained unthinned. Thus, it was not possible in these foils to study either the matrix-reinforcement interface or the microstructure of the reinforcement particles themselves. In contrast, both phases in the composites prepared using the focused ion beam miller thinned uniformly. The interfaces in these materials were clearly visible and the ceramic reinforcement was electron transparent. However, microstructural artifacts associated with ion beam damage were also observed. The extent of these artifacts and methods of minimizing their effect were dependent on both the materials and the milling conditions used.
The focused ion beam miller (FIB) has been widely used in the semiconductor industry for many years, but only recently has its potential as a tool for materials science been recognised. The FIB uses a highly energetic beam of gallium ions to sputter material such that it can precisely section, as well as image, areas of interest. The FIB can be used to create crosssections, which can be examined in the FIB or in a scanning electron microscope (SEM). Cross sections can be made from delicate samples or samples in which a specific area needs to be viewed, for example to check the thickness of coatings or for failure analysis.
The FIB may also be used to prepare transmission electron microscope (TEM) specimens . Extremely site-specific thin areas may be prepared with high positional accuracy from heterogeneous samples such as composites or layered structures.
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