We present a specimen preparation procedure for atom-probe tomography using SemGlu from Kleindiek Nanotechnik, an adhesive that hardens under electron beam irradiation. The SemGlu adhesive is used in place of focused-ion-beam-induced deposition of organo-metallic Pt, W, or C to form a bond between the sample and the substrate during the specimen preparation procedure. We demonstrate the utility of this adhesive-based specimen preparation technique with a correlated atom-probe tomography-scanning transmission electron microscopy study of the iron-nickel alloy kamacite (ferrite, ɑ-iron) in the Bristol iron meteorite and two steel specimens.

The influence of W on the temporal evolution of γ′ precipitation toward equilibrium in a model Ni-Al-Cr alloy is investigated by three-dimensional atom-probe (3DAP) microscopy and transmission electron microscopy (TEM). We report on the alloys Ni-10 Al-8.5 Cr (at.%) and Ni-10 Al-8.5 Cr-2 W (at.%), which were aged isothermally in the γ + γ′ two-phase field at 1073 K, for times ranging from 0.25 to 264 h. Spheroidal-shaped γ′ precipitates, 5–15 nm diameter, form during quenching from above the solvus temperature in both alloys at a high number density (∼1023 m−3). As γ′ precipitates grow with aging at 1073 K, a transition from spheriodal- to cuboidal-shaped precipitates is observed in both alloys. The elemental partitioning and spatially resolved concentration profiles across the γ′ precipitates are obtained as a function of aging time from three-dimensional atom-by-atom reconstructions. Proximity histogram concentration profiles (Hellman et al., 2000) of the quaternary alloy demonstrate that W concentration gradients exist in γ′ precipitates in the as-quenched and 0.25-h aging states, which disappear after 1 h of aging. The diffusion coefficient of W in γ′ is estimated to be 6.2 × 10−20 m2 s−1 at 1073 K. The W addition decreases the coarsening rate constant, and leads to stronger partitioning of Al to γ′ and Cr to γ.

A Mo-rich precipitate in an Fe-rich matrix and the heterophase interface bounding the precipitate have been examined on an atomic scale by three-dimensional atom-probe (3DAP) microscopy and transmission electron microscopy (TEM). The Mo-rich precipitate was generated by isothermal solid-state decomposition at 500°C of an Fe-15 at.% Mo-5 at.% V alloy. After this heat treatment, TEM reveals a characteristic modulated strain contrast structure. The precipitate has a composition of Mo-13.0 at.% Fe-4.9 at.% V as measured by 3DAP microscopy. The alloy decomposes at a nearly constant 5 at.% V, constituting a metastable tie-line between Fe-rich and Mo-rich bcc solid solutions. The formation of the equilibrium intermetallic phases is kinetically impeded. A local vanadium enrichment of 21 at.% is detected at the interface of the precipitate in a matrix region about 0.27 nm or 1–2 atomic layers in thickness. The corresponding value of the Gibbsian interfacial excess of vanadium is 3.3 ± 1.3 nm−2.

The three-dimensional (3D) atom-probe technique produces a reconstruction of the elemental chemical identities and three-dimensional positions of atoms field evaporated from a sharply pointed metal specimen, with a local radius of curvature of less than 50 nm. The number of atoms collected can be on the order of one million, representing an analysis volume of approximately 20 nm × 20 nm × 200 nm (80,000 nm3). This large amount of data allows for the identification of microstructural features in a sample, such as grain or heterophase boundaries, if the feature density is large enough. Correlation of the measured atomic positions with these identified features results in an atom-by-atom description of the chemical environment of crystallographic defects. This article outlines a data compilation technique for the generation of composition profiles in the vicinity of interfaces in a geometrically independent way. This approach is applied to quantitative determination of interfacial segregation of silver at a MgO/Cu(Ag) heterophase interface.

We are studying heterophase interfaces between molybdenum nitride precipitates and an α-iron matrix on a nanometer scale by electron and atom-probe field-ion microscopies. Fe-2 at.% Mo-0.5 at.% Sn and Fe-2 at.% Mo-0.4 at.% Sb are internally nitrided by annealing in an NH3/2 atmosphere. Nitridation at 550°C produces coherent thin platelet-shaped molybdenum nitride precipitates, while at 600°C semicoherent coarse plates and spheres also form. Segrega-tion of Sn and Sb is observed at the heterophase interfaces of only the semicoherent precipitates. The loss of coherency, that is the formation of misfit dislocations, is essential for substantial interfacial solute segregation to occur at heterophase interfaces.