Shaping the lens of the atom probe: fabrication of site specific, oriented specimens and application to grain boundary analysis

The random sampling provided by classical atom probe sample preparation methods is one of the major factors limiting the types of problems that can be addressed using this powerful technique. A focused ion beam enables not only site-specific preparation, but can also be used to give the specimen, which acts as the lens in an atom probe experiment, a specific shape. In this paper we present a technique that uses low accelerating voltages (10 and 5 kV) in the focused ion beam (FIB) to reproducibly produce specimens with selected grain boundaries <100 nm from the tip at any desired orientation. These tips have a high rate of successfully running in the atom probe and no Ga contamination within the region of interest.This technique is applied to the analysis of grain boundaries in a high purity iron wire and a strip-cast steel. Lattice resolution is achieved around the boundary in certain areas. Reconstruction of these datasets reveals the distribution of light and heavy elements around the boundary. Issues surrounding the uneven distribution of certain solute elements as a result of field-induced diffusion are discussed.     

Fabrication and characterization of APT specimens from high dose heavy ion irradiated materials

The next generations of advanced energy systems will require materials that can withstand high doses of irradiation at elevated temperatures. Therefore, a methodology has been developed for the fabrication of high-dose ion-irradiated atom probe tomography specimens at a specific dose with the use of a focused ion beam milling system. The method also enables the precise ion dose of the atom probe tomography specimen to be estimated from the local concentration of the implanted ions. The method has been successfully applied to the characterization of the distribution of nanoclusters in a radiation-tolerant 14YWT nanostructured ferritic steel under ion irradiation to doses up to 400 displacements per atom.     

Broadening the applications of the atom probe technique by ultraviolet femtosecond laser

Laser assisted field evaporation using ultraviolet (UV) wavelength gives rise to better mass resolution and signal-to-noise ratio in atom probe mass spectra of metals, semiconductors and insulators compared to infrared and green lasers. Combined with the site specific specimen preparation techniques using the lift-out and annular Ga ion milling in a focused ion beam machine, a wide variety of materials including insulating oxides can be quantitatively analyzed by the three-dimensional atom probe using UV laser assisted field evaporation. After discussing laser irradiation conditions for optimized atom probe analyses, recent atom probe tomography results on oxides, semiconductor devices and grain boundaries of sintered magnets are presented.     

The remote electron beam-induced current analysis of grain boundaries in semiconducting and semi-insulating materials

When no charge collecting p-n junction or Schottky barrier is present in the specimen, but two contacts are applied, conductive mode scanning electron microscope (SEM) observations known as remote electron beam-induced current (REBIC) can be made. It was described as "remote" EBIC because the contacts to the specimen can lie at macroscopic distances from the beam impact point. In recent years, REBIC has been found to be useful not only for studies of grain boundaries in semiconducting silicon and germanium, but also in semi-insulating materials such as the wider bandgap II-VI compounds and electroceramic materials like varistor ZnO and positive temperature coefficient resistor (PTCR) BaTiO3. The principles of this method are outlined. Accounts are given of the five forms of charge collection and resistive contrast that appear at grain boundaries (GBs) in REBIC micrographs. These are (1) terraced contrast due to high resistivity boundary layers, (2) peak and trough (PAT) contrast due to charge on the boundary, (3) reversible contrast seen only under external voltage bias due to the beta-conductive effect in a low conductivity boundary layer, (4) dark contrast due to enhanced recombination, and (5) bright contrast apparently due to reduced recombination. For comparison, the results of the extensive EBIC studies of GBs in Si and Ge are first outlined and then the results of recent REBIC grain boundary studies in both semiconducting and semi-insulating materials are reviewed.     

A direct and quantitative image of the internal nanostructure of nonordered porous monolithic carbon using FIB nanotomography

A direct study of the shape, size and connectivity of nonordered pores in carbon materials is particularly challenging. A new method that allows direct three-dimensional (3D) investigations of mesopores in monolithic carbon materials and quantitative characterization of their physical properties (surface area and pore size distribution) is reported. Focused ion beam (FIB) nanotomography technique is performed by combination of focused ion beam and scanning electron microscope. Porous monolithic carbon is produced by carbonization of a resorcinol-formaldehyde gel in the presence of a cationic polyelectrolyte as a pore stabilizer.     

Atomic-scale redistribution of Pt during reactive diffusion in Ni (5% Pt)–Si contacts

The NiSi silicide that forms by reactive diffusion between Ni and Si active regions of nanotransistors is used nowadays as contacts in nanoelectronics because of its low resistivity. Pt is added to the Ni film in order to stabilise the NiSi phase against the formation of the high-resistivity NiSi₂ phase and agglomeration.     

Tomography of insulating biological and geological materials using focused ion beam (FIB) sectioning and low-kV BSE imaging

Tomography in a focused ion beam (FIB) scanning electron microscope (SEM) is a powerful method for the characterization of three-dimensional micro- and nanostructures. Although this technique can be routinely applied to conducting materials, FIB–SEM tomography of many insulators, including biological, geological and ceramic samples, is often more difficult because of charging effects that disturb the serial sectioning using the ion beam or the imaging using the electron beam. Here, we show that automatic tomography of biological and geological samples can be achieved by serial sectioning with a focused ion beam and block-face imaging using low-kV backscattered electrons. In addition, a new ion milling geometry is used that reduces the effects of intensity gradients that are inherent in conventional geometry used for FIB–SEM tomography.