Characterization of Anomalous Grains in FeCo Magnetic Alloys.

Heat-treated FeCo-based magnetic alloys were characterized using a suite of electron microscopy techniques to gain insight into their structural properties. Electron channeling contrast imaging (ECCI) in the scanning electron microscope (SEM) found unique grains towards the outer edge of a FeCo sample with nonuniform background contrast. High-magnification ECCI imaging of these nonuniform grains revealed a weblike network of defects that were not observed in standard uniform background contrast grains. High-resolution electron backscattered diffraction (HR-EBSD) confirmed these defect structures to be dislocation networks and additionally found subgrain boundaries within the nonuniform contrast grains. The defect content within these grains suggests that they are unrecrystallized grains, and ECCI can be used as a rapid method to quantify unrecrystallized grains. To demonstrate the insight that can be garnered via ECCI on these unique grains, the sample was imaged before and after micro indentation. This experiment showed that slip bands propagate throughout the material until interacting with the dislocation networks, suggesting that these specific defects provide a barrier to plastic deformation. Taken together, these results show how ECCI can be used to better understand failure mechanisms in alloys and provides further evidence that dislocation networks play a critical role in the brittle failure of FeCo alloys.

Mechanism of FIB-Induced Phase Transformation in Austenitic Steel.

The transformation of unstable austenite to ferrite or α' martensite as a result of exposure to Xe+ or Ga+ ions at room temperature was studied in a 304 stainless steel casting alloy. Controlled Xe+ and Ga+ ion beam exposures of the 304 were carried out at a variety of beam/sample geometries. It was found that both Ga+ and Xe+ ion irradiation resulted in the transformation of the austenite to either ferrite or α' martensite. In this paper, we will refer to the transformation product as a BCC phase. The crystallographic orientation of the transformed area was controlled by the orientation of the austenite grain and was consistent with either the Nishiyama­Wasserman or the Kurdjumov­Sachs orientation relationships. On the basis of the Xe+ and Ga+ ion beam exposures, the transformation is not controlled by the chemical stabilization of the BCC phase by the ion species, but is a result of the disorder caused by the ion-induced recoil motion and subsequent return of the disordered region to a more energetically favorable phase.

Focused Ion Beam Preparation of Low Melting Point Metals: Lessons Learned From Indium.

Indium (In) and other low melting point metals are used as interconnects in a variety of hybridized circuits and a full understanding of the metallurgy of these interconnects is important to the reliability and performance of the devices. This paper shows that room temperature focused ion beam (FIB) preparation of cross-sections, using Ga+ or Xe+ can result in artifacts that obscure the true In microbump structure. The use of modified milling strategies to minimize the increased local sample temperature are shown to produce cross-sections that are representative of the In bump microstructure in some sample configurations. Furthermore, cooling of the sample to cryogenic temperatures is shown to reliably eliminate artifacts in FIB prepared cross-sections of In bumps allowing the true bump microstructure to be observed.

Identification of Star Defects in Gallium Nitride with HREBSD and ECCI.

This paper characterizes novel "star" defects in GaN films grown with metal­organic vapor phase deposition (MOVPE) on GaN substrates with electron channeling contrast imaging (ECCI) and high-resolution electron backscatter diffraction (HREBSD). These defects are hundreds of microns in size and tend to aggregate threading dislocations at their centers. They are the intersection of six nearly ideal low-angle tilt boundaries composed of $\langle a\rangle$-type pyramidal edge dislocations, each on a unique slip system.

Comparison of Orientation Mapping in SEM and TEM.

Multiple experimental configurations for performing nanoscale orientation mapping are compared to determine their fidelity to the true microstructure of a sample. Transmission Kikuchi diffraction (TKD) experiments in a scanning electron microscope (SEM) and nanobeam diffraction (NBD) experiments in a transmission electron microscope (TEM) were performed on thin electrodeposited hard Au films with two different microstructures. The Au samples either had a grain size that is >50 or <20 nm. The same regions of the samples were measured with TKD apparatuses at 30 kV in an SEM with detectors in the horizontal and vertical configurations and in the TEM at 300 kV. Under the proper conditions, we demonstrate that all three configurations can produce data of equivalent quality. Each method has strengths and challenges associated with its application and representation of the true microstructure. The conditions needed to obtain high-quality data for each acquisition method and the challenges associated with each are discussed.

Room-temperature voltage tunable phonon thermal conductivity via reconfigurable interfaces in ferroelectric thin films.

Dynamic control of thermal transport in solid-state systems is a transformative capability with the promise to propel technologies including phononic logic, thermal management, and energy harvesting. A solid-state solution to rapidly manipulate phonons has escaped the scientific community. We demonstrate active and reversible tuning of thermal conductivity by manipulating the nanoscale ferroelastic domain structure of a Pb(Zr0.3Ti0.7)O3 film with applied electric fields. With subsecond response times, the room-temperature thermal conductivity was modulated by 11%.

Application of electron backscatter diffraction for crystallographic characterization of tin whiskers.

Understanding the growth of whiskers or high aspect ratio features on substrates can be aided when the crystallography of the feature is known. This study has evaluated three methods that utilize electron backscatter diffraction (EBSD) for the determination of the crystallographic growth direction of an individual whisker. EBSD has traditionally been a technique applied to planar, polished samples, and thus the use of EBSD for out-of-surface features is somewhat more difficult and requires additional steps. One of the methods requires the whiskers to be removed from the substrate resulting in the loss of valuable physical growth relationships between the whisker and the substrate. The other two techniques do not suffer this disadvantage and provide the physical growth information as well as the crystallographic growth directions. The final choice of method depends on the information required. The accuracy and the advantages and disadvantages of each method are discussed.

Focused ion beam induced microstructural alterations: texture development, grain growth, and intermetallic formation.

Copper, gold, and tungsten thin films have been exposed to 30 kV Ga+ ion irradiation, and the resulting microstructural modifications are studied as a function of ion dose. The observed microstructural changes include texture development with respect to the easy channeling direction in the target, and in the case of Cu, an additional intermetallic phase is produced. Texture development in these target materials is a function of the starting materials grain size, and these changes are not observed in large grained materials. The accepted models of differential damage driven grain growth are not supported by the results of this study. The implications of this study to the use of focused ion beam tools for sample preparation are discussed.

Multivariate statistical approach to electron backscattered diffraction.

This paper assesses the potential of multivariate statistical analysis (MSA) applied to electron backscattered diffraction (EBSD) data. Instead of directly indexing EBSD patterns on an individual basis, this multivariate approach reduces a large (thousands) set of individual EBSD patterns into a core set of statistically derived component EBSD patterns which can be subsequently indexed. The following hypotheses are considered in this paper: (1) experimental EBSD patterns from a microstructure can be analytically treated as linear combinations of spatially simple components, (2) MSA has an angular resolution on par with standard EBSD, (3) MSA can discriminate between similar and dissimilar phases, and (4) the MSA approach can improve the effective spatial resolution of automated EBSD.

Lithographically defined three-dimensional graphene structures.

A simple and facile method to fabricate 3D graphene architectures is presented. Pyrolyzed photoresist films (PPF) can easily be patterned into a variety of 2D and 3D structures. We demonstrate how prestructured PPF can be chemically converted into hollow, interconnected 3D multilayered graphene structures having pore sizes around 500 nm. Electrodes formed from these structures exhibit excellent electrochemical properties including high surface area and steady-state mass transport profiles due to a unique combination of 3D pore structure and the intrinsic advantages of electron transport in graphene, which makes this material a promising candidate for microbattery and sensing applications.

High resolution at low beam energy in the SEM: resolution measurement of a monochromated SEM.

The resolution of secondary electron low beam energy imaging of a scanning electron microscope equipped with a monochromator is quantitatively measured using the contrast transfer function (CTF) method. High-resolution images, with sub-nm resolutions, were produced using low beam energies. The use of a monochromator is shown to quantitatively improve the resolution of the SEM at low beam energies by limiting the chromatic aberration contribution to the electron probe size as demonstrated with calculations and images of suitable samples. Secondary electron image resolution at low beam energies is ultimately limited by noise in the images as shown by the CTFs.

Forensic analysis of bioagents by X-ray and TOF-SIMS hyperspectral imaging.

Hyperspectral imaging combined with multivariate statistics is an approach to microanalysis that makes the maximum use of the large amount of data potentially collected in forensics analysis. This study examines the efficacy of using hyperspectral imaging-enabled microscopies to identify chemical signatures in simulated bioagent materials. This approach allowed for the ready discrimination between all samples in the test. In particular, the hyperspectral imaging approach allowed for the identification of particles with trace elements that would have been missed with a more traditional approach to forensic microanalysis. The importance of combining signals from multiple length scales and analytical sensitivities is discussed.

Tomographic Spectral Imaging with Multivariate Statistical Analysis: Comprehensive 3D Microanalysis.

A comprehensive three-dimensional (3D) microanalysis procedure using a combined scanning electron microscope (SEM)/focused ion beam (FIB) system equipped with an energy-dispersive X-ray spectrometer (EDS) has been developed. The FIB system was used first to prepare a site-specific region for X-ray microanalysis followed by the acquisition of an electron-beam generated X-ray spectral image. A small section of material was then removed by the FIB, followed by the acquisition of another X-ray spectral image. This serial sectioning procedure was repeated 10-12 times to sample a volume of material. The series of two-spatial-dimension spectral images were then concatenated into a single data set consisting of a series of volume elements or voxels each with an entire X-ray spectrum. This four-dimensional (three real space and one spectral dimension) spectral image was then comprehensively analyzed with Sandia's automated X-ray spectral image analysis software. This technique was applied to a simple Cu-Ag eutectic and a more complicated localized corrosion study where the powerful site-specific comprehensive analysis capability of tomographic spectral imaging (TSI) combined with multivariate statistical analysis is demonstrated.

Automated analysis of SEM X-ray spectral images: a powerful new microanalysis tool.

Spectral imaging in the scanning electron microscope (SEM) equipped with an energy-dispersive X-ray (EDX) analyzer has the potential to be a powerful tool for chemical phase identification, but the large data sets have, in the past, proved too large to efficiently analyze. In the present work, we describe the application of a new automated, unbiased, multivariate statistical analysis technique to very large X-ray spectral image data sets. The method, based in part on principal components analysis, returns physically accurate (all positive) component spectra and images in a few minutes on a standard personal computer. The efficacy of the technique for microanalysis is illustrated by the analysis of complex multi-phase materials, particulates, a diffusion couple, and a single-pixel-detection problem.