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The composition of carbides in steel, measured by atom probe tomography, can be influenced by limitations in the ion detector system. When carbides are analyzed, many ions tend to field evaporate from the same region of the specimen during the same laser or voltage pulse. This results in a so-called multiple event, meaning that several ions impact the detector in close proximity both in time and space. Due to a finite detector dead-time not all ions can be detected, a phenomenon known as detector pile-up. The evaporation behavior of carbon is often different than the evaporation behavior of metals when analyzing alloy carbides, leading to preferential loss of carbon ions, and a measured carbon concentration below the expected value. This effect becomes stronger as the overall detection efficiency gets higher. Here, the detection efficiency was deliberately reduced by inserting a grid into the flight-path, which resulted in a higher and more correct carbon concentration, accompanied by an increase in the statistical uncertainty.
The microstructure and distribution of the elements have been studied in thin films of a near-equimolar CrNbTaTiW high entropy alloy (HEA) and films with 8 at.% carbon added to the alloy. The films were deposited by magnetron sputtering at 300°C. X-ray diffraction shows that the near-equimolar metallic film crystallizes in a single-phase body centered cubic (bcc) structure with a strong (110) texture. However, more detailed analyses with transmission electron microscopy (TEM) and atom probe tomography (APT) show a strong segregation of Ti to the grain boundaries forming a very thin Ti–Cr rich interfacial layer. The effect can be explained by the large negative formation enthalpy of Ti–Cr compounds and shows that CrNbTaTiW is not a true HEA at lower temperatures. The addition of 8 at.% carbon leads to the formation of an amorphous structure, which can be explained by the limited solubility of carbon in bcc alloys. TEM energy-dispersive X-ray spectroscopy indicated that all metallic elements are randomly distributed in the film. The APT investigation, however, revealed that carbide-like clusters are present in the amorphous film.
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.
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.
Atom-probe tomography (APT) is in the midst of a dynamic renaissance as a result of the development of well-engineered commercial instruments that are both robust and ergonomic and capable of collecting large data sets, hundreds of millions of atoms, in short time periods compared to their predecessor instruments. An APT setup involves a field-ion microscope coupled directly to a special time-of-flight (TOF) mass spectrometer that permits one to determine the mass-to-charge states of individual field-evaporated ions plus their x-, y-, and z-coordinates in a specimen in direct space with subnanoscale resolution. The three-dimensional (3D) data sets acquired are analyzed using increasingly sophisticated software programs that utilize high-end workstations, which permit one to handle continuously increasing large data sets. APT has the unique ability to dissect a lattice, with subnanometer-scale spatial resolution, using either voltage or laser pulses, on an atom-by-atom and atomic plane-by-plane basis and to reconstruct it in 3D with the chemical identity of each detected atom identified by TOF mass spectrometry. Employing pico- or femtosecond laser pulses using visible (green or blue light) to ultraviolet light makes the analysis of metallic, semiconducting, ceramic, and organic materials practical to different degrees of success. The utilization of dual-beam focused ion-beam microscopy for the preparation of microtip specimens from multilayer and surface films, semiconductor devices, and for producing site-specific specimens greatly extends the capabilities of APT to a wider range of scientific and engineering problems than could previously be studied for a wide range of materials: metals, semiconductors, ceramics, biominerals, and organic materials.
This article summarizes findings from our previous investigations and
recent studies concerning precipitation in a maraging steel of type
13Cr-9Ni-2Mo-2Cu (at.%) with small additions of Ti (1 at.%) and Al (0.7
at.%). The material was investigated after aging at 475°C up to 400
h using both conventional and three-dimensional atom-probe analyses.
The process of phase decomposition in the steel proved to be
complicated. It consisted of precipitation of several phases with
different chemistry. A Cu-rich phase was first to precipitate and Mo
was last in the precipitation sequence. The influence of the complex
precipitation path on the material properties is discussed. The
investigation clearly demonstrated the usefulness of the applied
techniques for investigation of nanoscale precipitation. It is also
shown that, complementary methods (such as TEM and EFTEM) giving
structural and chemical information on a larger scale must be applied
to explain the good properties of the steel after prolonged aging.