Julie M. Cairney

A reproducible method for damage-free site-specific preparation of atom probe tips from interfaces

Atom probe tomography (APT) is a mass spectrometry method with atomic‐scale spatial resolution that can be used for the investigation of a wide range of materials. The main limiting factor with respect to the type of problems that can be addressed is the small volume investigated and the randomness of common sample preparation methods. With existing site‐specific specimen preparation methods it is still challenging to rapidly and reproducibly produce large numbers of successful samples from specifically selected grain boundaries or interfaces for systematic studies. A new method utilizing both focused ion beam (FIB) and transmission electron microscopy (TEM) is presented that can be used to reproducibly produce damage‐free atom probe samples with features of interest at any desired orientation with an accuracy of better than 50 nm from samples that require very little prior preparation. Microsc. Res. Tech. 2011.

Atom probe crystallography

This review addresses new developments in the emerging area of “atom probe crystallography”, a materials characterization tool with the unique capacity to reveal both composition and crystallographic structure at the atomic scale. This information is crucial for the manipulation of microstructure for the design of both structural and functional materials with optimized mechanical, electric, optoelectronic, magnetic, or superconducting properties that will find application in, for example, nanoelectronics or energy generation. The ability to extract crystallographic information from 3D atomistic reconstruction has exciting potential synergies with modern modeling techniques, blending experimental and computational methods to extend our insight.

On the multiplicity of field evaporation events in atom probe: A new dimension to the analysis of mass spectra

We introduce a filtering technique for atom probe microscopy data that is based on the multiplicity of detector events for each atom. We demonstrate that the resulting multi-dimensional mass spectra can be used to differentiate signal from noise and so the technique enhances the microscopic imaging and microanalysis capacity of atom probe in investigating the atomic-level dispersion of solutes in solid solutions. We have demonstrated this method in the analysis of C atoms in a low-alloy steel and found, somewhat unexpectedly, that the C atoms seem to participate in a surface migration prior to field evaporation. We propose that this is driven by electric field gradients. We also raise the possibility that, in some cases, the formation of complex ions prior to field evaporation may impact the detection efficiency.

Deformation-induced trace element redistribution in zircon revealed using atom probe tomography.

Trace elements diffuse negligible distances through the pristine crystal lattice in minerals: this is a fundamental assumption when using them to decipher geological processes. For example, the reliable use of the mineral zircon (ZrSiO4) as a U-Th-Pb geochronometer and trace element monitor requires minimal radiogenic isotope and trace element mobility. Here, using atom probe tomography, we document the effects of crystal–plastic deformation on atomic-scale elemental distributions in zircon revealing sub-micrometre-scale mechanisms of trace element mobility. Dislocations that move through the lattice accumulate U and other trace elements. Pipe diffusion along dislocation arrays connected to a chemical or structural sink results in continuous removal of selected elements (for example, Pb), even after deformation has ceased. However, in disconnected dislocations, trace elements remain locked. Our findings have important implications for the use of zircon as a geochronometer, and highlight the importance of deformation on trace element redistribution in minerals and engineering materials.

Dynamic reconstruction for atom probe tomography

Progress in the reconstruction for atom probe tomography has been limited since the first implementation of the protocol proposed by Bas et al. in 1995. This approach and those subsequently developed assume that the geometric parameters used to build the three-dimensional atom map are constant over the course of an analysis. Here, we test this assumption within the analyses of low-alloyed materials. By building upon methods recently proposed to measure the tomographic reconstruction parameters, we demonstrate that this assumption can introduce significant limitations in the accuracy of the analysis. Moreover, we propose a strategy to alleviate this problem through the implementation of a new reconstruction algorithm that dynamically accommodates variations in the tomographic reconstruction parameters.

Crystallographic structural analysis in atom probe microscopy via 3D Hough transformation

Whereas the atom probe is regarded almost exclusively as a technique for 3D chemical microanalysis of solids with the highest chemical and spatial resolution, we demonstrate that the technique can be used for detailed crystallographic determinations. We present a new method for the quantitative determination of crystal structure (plane spacings and angles) using a Hough transformation of the reconstructed atom probe data. The resolving power is shown to be high enough to identify poorly established, discontinuous planes that are typical in semiconducting materials. We demonstrate the determination of crystal geometry around a grain boundary and the use of the technique for the optimisation of tomographic reconstruction. We propose that this method will enable automatic spatial analysis and, ultimately, automated tomographic reconstruction in atom probe microscopy.

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.

Focused-ion-beam Milling: A Novel Approach to Probing the Interior of Particles Used for Inhalation Aerosols

PurposeThe current study aimed to examine the pharmaceutical applications of the focused-ion-beam (FIB) in the inhalation aerosol field, particularly to particle porosity determination (i.e. percentage of particles having a porous interior).Materials and MethodsThe interior of various spray dried particles (bovine serum albumin (BSA) with different degrees of surface corrugation, mannitol, disodium cromoglycate and sodium chloride) was investigated via FIB milling at customized conditions, followed by viewing under a high resolution field-emission scanning electron microscope. Two sets of ten particles for each sample were examined.ResultsFor the spray-dried BSA particles, a decrease in particle porosity (from 50 to 0%) was observed with increasing particle surface corrugation. Spray-dried mannitol, disodium cromoglycate and sodium chloride particles were determined to be 90–100%, 0–10% and 0% porous, respectively. The porosity in the BSA and mannitol particles thus should be considered for the aerodynamic behaviour of these particles.ConclusionsThe FIB technology represents a novel approach useful for probing the interior of particles linking to the aerosol properties of the powder. Suitable milling protocols have been developed which can be adapted to study other similar particles.

Transmission Electron Microscope Specimen Preparation of Metal Matrix Composites Using the Focused Ion Beam Miller

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.

Atom probe crystallography: Characterization of grain boundary orientation relationships in nanocrystalline aluminium

Spatial Distribution Maps (SDM) in their various forms have previously been used to identify and characterize crystallographic structure within APT reconstructions. Importantly, it has been shown that such SDM analyses can also provide the crystallographic orientation of the specimen with respect to the direction of the detector in the original experiment. In this study, we investigate the application of SDMs to the analysis of APT reconstruction of a nanocrystalline Al film. We demonstrate that significant intra-granular crystallographic information is retained in the reconstruction, even in the x-y plane perpendicular to the direction of the detector. Further, the crystallographic orientation of the grains can be characterized highly accurately not only with respect to the bulk specimen but also their misorientation with respect to neighbouring grains.