Determination of solute site occupancies within γ' precipitates in nickel-base superalloys via orientation-specific atom probe tomography.

The analytical limitations in atom probe tomography such as resolving a desired set of atomic planes, for solving complex materials science problems, have been overcome by employing a well-developed unique and reproducible crystallographic technique, involving synergetic coupling of orientation microscopy with atom probe tomography. The crystallographic information in atom probe reconstructions has been utilized to determine the solute site occupancies in Ni-Al-Cr based superalloys accurately. The structural information in atom probe reveals that both Al and Cr occupy the same sub-lattice within the L12-ordered γ' precipitates to form Ni3(Al,Cr) precipitates in a Ni-14Al-7Cr (at%) alloy. Interestingly, the addition of Co, which is a solid solution strengthener, to a Ni-14Al-7Cr alloy results in the partial reversal of Al site occupancy within γ' precipitates to form (Ni,Al)3(Al,Cr,Co) precipitates. This unique evidence of reversal of Al site occupancy, resulting from the introduction of other solutes within the ordered structures, gives insights into the relative energetics of different sub-lattice sites when occupied by different solutes.

Probing the crystallography of ordered Phases by coupling of orientation microscopy with atom probe tomography.

The determination of atomic scale structural and compositional information using atom probe tomography is currently limited to elemental solids and dilute alloys. In the present article, a unique coupling of orientation microscopy and atom probe tomography successfully facilitates the crystallographic study of non-dilute alloy systems, with high evaporation fields. This reproducible methodology affords a new perspective to the conventional atom probe tomography of ordered precipitate strengthened superalloys. The high accuracy in crystallographic site-specific sample preparation results in high spatial resolution in APT, which has been demonstrated in Co-base superalloys. The practical applications of this technique can be extended to accurately characterize the nature of buried order/disorder interfaces at the atomic scale, as well as the site occupancies associated with different solute atoms in multi-component superalloys.

3D reconstruction of prior ß grains in friction stir-processed Ti-6Al-4V.

The prior ß grain structure and orientations in the central stir zone of friction stir-processed Ti-6Al-4V were reconstructed from measured α phase orientations obtained by three-dimensional serial sectioning in a dual-beam focused ion beam scanning electron microscope. The data were processed to obtain the α colony and ß grain size distributions in the volume. Several ß grains were individually analysed to determine the total number of unique α variants and the respective volume fractions of each. The analysis revealed that some grains experienced overwhelming variant selection (i.e. one variant dominated) whereas other ß grains contained a more evenly distributed mixture of all 12 variants.

Using cross-correlation for automated stitching of two-dimensional multi-tile electron backscatter diffraction data.

A method for automatically aligning consecutive data sets of large, two-dimensional multi-tile electron backscatter diffraction (EBSD) scans with high accuracy was developed. The method involved first locating grain and phase boundaries within search regions containing overlapping data in adjacent scan tiles, and subsequently using cross-correlation algorithms to determine the relative position of the individual scan tiles which maximizes the fraction of overlapping boundaries. Savitzky-Golay filtering in two dimensions was used to estimate the background, which was then subtracted from the cross-correlation to enhance the peak signal in samples with a high density of interfaces. The technique was demonstrated on data sets with a range of interface densities. The equations were implemented as enhancements to a recently published open source code for stitching of multi-tile EBSD data sets.

A novel method for acquiring large-scale automated scanning electron microscope data.

Recent software and hardware advances in the field of electron backscatter diffraction have led to an increase in the rate of data acquisition. Combining automated stage movements with conventional beam control have allowed researchers to collect data from significantly larger areas of samples than was previously possible. This paper describes a LabVIEW™ and AutoIT(©) code which allows for increased flexibility compared to commercially available software. The source code for this software has been made available in the online version of this paper.

Novel mixed-mode phase transition involving a composition-dependent displacive component.

Solid-solid displacive, structural phase transformations typically undergo a discrete structural change from a parent to a product phase. Coupling electron microscopy, three-dimensional atom probe, and first-principles computations, we present the first direct evidence of a novel mechanism for a coupled diffusional-displacive transformation in titanium-molybdenum alloys wherein the displacive component in the product phase changes continuously with changing composition. These results have implications for other transformations and cannot be explained by conventional theories.

AnyStitch: a tool for combining electron backscatter diffraction data sets.

Recent advances in electron backscatter diffraction equipment and software have permitted increased data acquisition rates on the order of hundreds of points per second with additional increases in the foreseeable future likely. This increase in speed allows users to collect data from statistically significant areas of samples by combining beam-control scans and automated stage movements. To facilitate data analysis, however, the individual tiles must be combined, or stitched, into a single data set. In this paper, we describe a matlab(®) (The Mathworks, Inc., Natick, MA, USA) program to facilitate stitching of electron backscatter diffraction data. The method offers users a wide range of controls for tile placement including independent overlaps for horizontal and vertical tiles and also includes a parameter to account for systematic stage positioning errors or improperly calibrated scan rotation. The code can stitch data collected on either square or hexagonal grids and contains a function to reduce the resolution of square grid data if the resulting file is too large (or has too many grains) to be opened by the analysis software. The software was primarily written to work with TSL(®) OIM™ data sets and includes a function to quickly read compressed *.osc files into a variable in the matlab(®) workspace as opposed to using slower, text-reading functions. The output file is in *.ang format and can be opened directly by TSL(®) OIM™ Analysis software. A set of functions to facilitate stitching of text-based *.ctf files produced by Oxford Instruments HKL systems are also included. Finally, the code can also be used to combine *.tif images to produce a montage. The source code, a graphical user interface and a compiled version of the software was made available in the online version of this paper.

Measurement of gamma' precipitates in a nickel-based superalloy using energy-filtered transmission electron microscopy coupled with automated segmenting techniques.

Precipitates of the ordered L1(2) gamma' phase (dispersed in the face-centered cubic or FCC gamma matrix) were imaged in Rene 88 DT, a commercial multicomponent Ni-based superalloy, using energy-filtered transmission electron microscopy (EFTEM). Imaging was performed using the Cr, Co, Ni, Ti and Al elemental L-absorption edges in the energy loss spectrum. Manual and automated segmentation procedures were utilized for identification of precipitate boundaries and measurement of precipitate sizes. The automated region growing technique for precipitate identification in images was determined to measure accurately precipitate diameters. In addition, the region growing technique provided a repeatable method for optimizing segmentation techniques for varying EFTEM conditions.

Novel automatic electrochemical-mechanical polishing (ECMP) of metals for scanning electron microscopy.

A low-stress automated polishing device was developed for preparing titanium and nickel alloys for scanning electron microscopy imaging. The system used pulsed electrochemical reactions within an alkaline electrolyte to generate a thin passivation layer on the surface of the sample, which was removed by the mechanical vibration of the system. The passivation layer development and removal were documented for Ti-6Al-4V and IN718 samples subjected to varying electrical potential cycles and polishing times. Results indicated that the applied cyclic potentials removed material faster than typical removal techniques. In addition, electron back scatter diffraction data showed a decrease in subsurface damage using the developed electrochemical-mechanical process compared to standard mechanical polishing techniques.

Atomic scale structure and chemical composition across order-disorder interfaces.

Through a combination of aberration-corrected high-resolution scanning transmission electron microscopy and three-dimensional atom probe tomography, the true atomic-scale structure and change in chemical composition across the complex order-disorder interface in a metallic alloy has been determined. The study reveals the presence of two interfacial widths, one corresponding to an order-disorder transition, and the other to the compositional transition across the interface, raising fundamental questions regarding the definition of the interfacial width in such systems.