Irradiation of reactor pressure vessel (RPV) steels causes the formation of nanoscale microstructural features (termed radiation damage), which affect the mechanical properties of the vessel. A key tool for characterizing these nanoscale features is atom probe tomography (APT), due to its high spatial resolution and the ability to identify different chemical species in three dimensions. Microstructural observations using APT can underpin development of a mechanistic understanding of defect formation. However, with atom probe analyses there are currently multiple methods for analyzing the data. This can result in inconsistencies between results obtained from different researchers and unnecessary scatter when combining data from multiple sources. This makes interpretation of results more complex and calibration of radiation damage models challenging. In this work simulations of a range of different microstructures are used to directly compare different cluster analysis algorithms and identify their strengths and weaknesses.

Radiation induced clustering affects the mechanical properties, that is the ductile to brittle transition temperature (DBTT), of reactor pressure vessel (RPV) steel of nuclear power plants. The combination of low Cu and high Ni used in some RPV welds is known to further enhance the DBTT shift during long time operation. In this study, RPV weld samples containing 0.04 at% Cu and 1.6 at% Ni were irradiated to 2.0 and 6.4×1023 n/m2 in the Halden test reactor. Atom probe tomography (APT) was applied to study clustering of Ni, Mn, Si, and Cu. As the clusters are in the nanometer-range, APT is a very suitable technique for this type of study. From APT analyses information about size distribution, number density, and composition of the clusters can be obtained. However, the quantification of these attributes is not trivial. The maximum separation method (MSM) has been used to characterize the clusters and a detailed study about the influence of the choice of MSM cluster parameters, primarily on the cluster number density, has been undertaken.

Emulsion polymer isocyanate (EPI) and urea-formaldehyde (UF) were selected as typical resin systems to investigate the microstructure of wood–adhesive interphases by fluorescence microscopy (FM) and confocal laser scanning microscopy (CLSM). Further, a quantitative micromechanical analysis of the interphases was conducted using nanoindentation. The FM results showed that the UF resin could penetrate the wood to a greater extent than the EPI resin, and that the average penetration depth for these two resin systems was higher in the case of latewood. CLSM allowed visualization of the resin distribution with contrasting colors, showing that the EPI resin could not penetrate the cell wall, whereas UF resin could enter the cell walls. The micromechanical properties of the cell walls were almost unaffected by EPI penetration but were significantly affected by UF penetration, especially in the first cell wall from the glueline. This further confirmed that only cell walls with resin penetration can improve the mechanical properties of the interphase regions.

Improved understanding of the interactions between solutes and the austenite/ferrite interface can benefit modeling of ferrite growth during austenite decomposition, as the transformation kinetic is significantly affected by solutes that influence interface mobility. Solute-interface interactions dominate solute segregation at the interface in binary systems, but in multi-component alloys, solute–solute interactions may also affect segregation. In this study, interface segregation in Fe–Mn–N is examined and compared with Fe–Mn–C, to reveal the extent to which C affects the segregation of Mn. Atom probe tomography (APT) is well-suited to analyze solute concentrations across the interface, as this technique combines high spatial resolution and compositional sensitivity. Measurements of Mn show that segregation is only observed for Fe–Mn–C. This demonstrates that Mn segregation is primarily driven by an affinity for C, which also segregates to the interface. However, the measurement of N in steels by APT may be affected by a variety of experimental factors. Therefore, in verifying the Fe–Mn–N result, systematic examination is conducted on the influence of pulsing method (voltage versus laser), sample preparation (ion milling versus electropolishing), and vacuum storage on the measured N concentration. Both laser pulsing and focused ion beam sample preparation are observed to decrease the apparent N concentration.

This study applies atom probe tomography (APT) to analyze the oxide scales formed on model NiAlCr alloys doped with Hf, Y, Ti, and B. Due to its ability to measure small amounts of alloying elements in the oxide matrix and its ability to quantify segregation, the technique offers a possibility for detailed studies of the dopant’s fate during high-temperature oxidation. Three model NiAlCr alloys with different additions of Hf, Y, Ti, and B were prepared and oxidized in O2 at 1,100°C for 100 h. All specimens showed an outer region consisting of different spinel oxides with relatively small grains and the protective Al2O3-oxide layer below. APT analyses focused mainly on this protective oxide layer. In all the investigated samples segregation of both Hf and Y to the oxide grain boundaries was observed and quantified. Neither B nor Ti were observed in the alumina grains or at the analyzed interfaces. The processes of formation of oxide scales and segregation of the alloying elements are discussed. The experimental challenges of the oxide analyses by APT are also addressed.

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.

The functional properties of the high-temperature superconductor Y1Ba2Cu3O7−δ (Y-123) are closely correlated to the exact stoichiometry and oxygen content. Exceeding the critical value of 1 oxygen vacancy for every five unit cells (δ>0.2, which translates to a 1.5 at% deviation from the nominal oxygen stoichiometry of Y7.7Ba15.3Cu23O54−δ) is sufficient to alter the superconducting properties. Stoichiometry at the nanometer scale, particularly of oxygen and other lighter elements, is extremely difficult to quantify in complex functional ceramics by most currently available analytical techniques. The present study is an analysis and optimization of the experimental conditions required to quantify the local nanoscale stoichiometry of single crystal yttrium barium copper oxide (YBCO) samples in three dimensions by atom probe tomography (APT). APT analysis required systematic exploration of a wide range of data acquisition and processing conditions to calibrate the measurements. Laser pulse energy, ion identification, and the choice of range widths were all found to influence composition measurements. The final composition obtained from melt-grown crystals with optimized superconducting properties was Y7.9Ba10.4Cu24.4O57.2.

We study the effects of Dy, Nb, and Ga additions on the microstructure and magnetic properties of Nd2Fe14B/α-Fe nanocomposites. Dy, Nb, and Ga additions inhibit the growth of the soft magnetic α-Fe phase. Dy and Nb additions are able to refine the microstructure, whereas Ga addition plays only a minor role in prohibiting crystal growth. The magnetic properties are sensitive to Dy, Nb, and Ga additions. The Dy-containing alloy enhances the intrinsic coercivity of 872 kA/m because Dy partially replaces Nd, forming (Nd, Dy)2Fe14B. Nb addition refines the microstructure, and consequently increases the exchange coupling between magnetic grains. The Nd9.5Fe75.4Co5Zr3B6.5Ga0.6 alloy exhibits the highest remanence (0.92 T) due to Ga addition.