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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 55 records · Page 3
All sourcesNASA NTRSDOE OSTI
DOE OSTI2026

Automation of Laser Plasma Focused Ion Beam Microscopy for Next-Gen Energy Materials

Automation can revolutionize the use of ultrafast laser ablation and plasma-focused ion beam (PFIB) techniques for high-throughput, reproducible cross-sectioning and various sample preparation in materials characterization. As these methods become essential for analyzing complex energy materials and next-generation devices, efficient, standardized workflows are needed to minimize variability and enhance precision. This work highlights our advancements in developing automated processes for sample preparation that integrates machine learning, workflow optimization, and large-scale data acquisition to improve efficiency and scalability in applications such as electrolyzers, photovoltaic cells, and microelectronics. To streamline cross-sectioning and lamella fabrication, we have implemented fully automated workflows that standardize laser ablation and PFIB milling sequences. These workflows incorporate pre-programmed protocols for material removal, alignment, and thinning, reducing user intervention and ensuring consistency across different sample types. Machine learning algorithms further enhance automation by predicting optimal milling strategies and adapting parameters based on material properties and sectioning requirements. This approach significantly improves throughput while maintaining the structural integrity of prepared samples for high-resolution imaging and analysis, including transmission electron microscopy. Beyond sample preparation, our automation platform enables the acquisition of large, high-resolution datasets through serial sectioning, image alignment, and 3D reconstruction. These automated routines facilitate multi-scale characterization, capturing structural and compositional details from the nanoscale to the device level. By reducing variability and increasing efficiency, our automated approach enhances defect analysis, failure diagnostics, and process optimization, accelerating advancements in materials research and device engineering.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Ionic Liquid Gating of SrTiO 3 Lamellas Fabricated with a Focused Ion Beam

Here, in this work, we combine two previously incompatible techniques for defining electronic devices: shaping three-dimensional crystals by focused ion beam (FIB), and two-dimensional electrostatic accumulation of charge carriers. The principal challenge for this integration is nanometer-scale surface damage inherent to any FIB-based fabrication. We address this by using a sacrificial protective layer to preserve a selected pristine surface. The test case presented here is accumulation of 2D carriers by ionic liquid gating at the surface of a micron-scale SrTiO 3 lamella. Preservation of surface quality is reflected in superconductivity of the accumulated carriers. This technique opens new avenues for realizing electrostatic charge tuning in materials that are not available as large or exfoliatable single crystals, and for patterning the geometry of the accumulated carriers.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2020

Fracture toughness of zirconia with a nanometer size notch fabricated using focused ion beam milling

Zirconia with 3 mol% yttria (3Y-TZP) has been used for dental crowns and bridges due to its excellent mechanical behavior. Performing fracture toughness testing on this nanograin material, however, can be a challenge. For reliable results, fracture toughness testing requires an extremely sharp notch in the test specimen that closely approximates a very sharp crack. This study was to investigate an alternative method to produce nanometer-sized notches, which are less than the average grain size of 3Y-TZP, during the preparation of single-edge V-notched beam specimens and report the resulting fracture toughness value. We present a method using focused ion beam (FIB) milling to fabricate nanometer-sized notches in 3Y-TZP. The notch tip is <100 nm wide, which is smaller than the grain size, and is consistent throughout the thickness of the specimen. The FIB-notched specimens show a much reduced average fracture toughness of 5.64 ± 1.14 MPa√m compared to 8.90 ± 0.23 MPa√m for the specimens without FIB-notches. The FIB-milling did not appear to create any monoclinic phase prior to fracture toughness testing. Fractures originated at the FIB-notches, and the notch size can be readily identified post-mortem using a microscope. A considerable amount of tetragonal-to-monoclinic phase transformation was observed throughout the fracture surfaces. FIB milling provides an alternative method to fabricate nanometer-sized notches that are smaller than the grain size of tetragonal zirconia polycrystal. The fracture toughness determined using FIB-notches was ~5.64 MPa√m, smaller than the specimens with V-notches fabricated using saw blades.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Novel Focused Ion Beam Liftouts for Spatial Characterization of Spherical Biominerals With Transmission Electron Microscopy

Abstract Focused ion beam (FIB) is frequently used to prepare electron- and X-ray-beam-transparent thin sections of samples, called lamellae. Typically, lamellae are prepared from only a subregion of a sample. In this paper, we present a novel approach for FIB lamella preparation of microscopic samples, wherein the entire cross-section of the whole sample can be investigated. The approach was demonstrated using spherical, porous, and often hollow microprecipitates of biologically precipitated calcium carbonate. The microprecipitate morphology made these biogenic samples more fragile and challenging than materials commonly investigated using FIB lamellae. Our method enables the appropriate orientation of the lamellae required for further electron/X-ray analyses after attachment to the transmission electron microscopy (TEM) grid post and facilitates more secure adhesion onto the grid post. We present evidence of autofluorescence in bacterially precipitated vaterite using this lamella preparation method coupled with TEM selected area diffraction. This innovative approach allows studying biomineralization at the micro to nano scales, which can provide novel insights into bacterial responses to microenvironmental conditions.

47 OTHER INSTRUMENTATION↗
DOE OSTI2020

Focused ion beam deposited carbon-platinum nanowires for cryogenic resistive thermometry

The study of thermal effects, both classical and quantum, at cryogenic temperatures requires the use of on-chip, local, high-sensitivity thermometry. Carbon-platinum composites fabricated using focused ion beam (FIB) assisted deposition form a granular structure which is shown in this study to be uniquely suited for this application. Carbon-platinum thermometers deposited using a 24 pA ion beam current have high sensitivities below 1 K, comparable to the best cryogenic thermometers. In addition, these thermometers can be accurately placed to within 10s of nanometers on the chip using a mask-free process. Furthermore, they also have a weak magnetic field dependence, 3% change in resistance with applied magnetic fields from 0 to 8 T. Finally, these thermometers are integrable into a variety of nanoscale devices due to the existing wide spread use of FIB.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
DOE OSTI2021

Annealing of focused ion beam damage in gold microcrystals: an in situ Bragg coherent X-ray diffraction imaging study

Focused ion beam (FIB) techniques are commonly used to machine, analyse and image materials at the micro- and nanoscale. However, FIB modifies the integrity of the sample by creating defects that cause lattice distortions. Methods have been developed to reduce FIB-induced strain; however, these protocols need to be evaluated for their effectiveness. Here, non-destructive Bragg coherent X-ray diffraction imaging is used to study the in situ annealing of FIB-milled gold microcrystals. Two non-collinear reflections are simultaneously measured for two different crystals during a single annealing cycle, demonstrating the ability to reliably track the location of multiple Bragg peaks during thermal annealing. The thermal lattice expansion of each crystal is used to calculate the local temperature. This is compared with thermocouple readings, which are shown to be substantially affected by thermal resistance. To evaluate the annealing process, each reflection is analysed by considering facet area evolution, cross-correlation maps of the displacement field and binarized morphology, and average strain plots. The crystal's strain and morphology evolve with increasing temperature, which is likely to be caused by the diffusion of gallium in gold below ~280°C and the self-diffusion of gold above ~280°C. The majority of FIB-induced strains are removed by 380–410°C, depending on which reflection is being considered. These observations highlight the importance of measuring multiple reflections to unambiguously interpret material behaviour.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗
NASA NTRS2000

Fracture Tests of Etched Components Using a Focused Ion Beam Machine

Many optical MEMS device designs involve large arrays of thin (0.5 to 1 micron components subjected to high stresses due to cyclic loading. These devices are fabricated from a variety of materials, and the properties strongly depend on size and processing. Our objective is to develop standard and convenient test methods that can be used to measure the properties of large numbers of witness samples, for every device we build. In this work we explore a variety of fracture test configurations for 0.5 micron thick silicon nitride membranes machined using the Reactive Ion Etching (RIE) process. Testing was completed using an FEI 620 dual focused ion beam milling machine. Static loads were applied using a probe. and dynamic loads were applied through a piezo-electric stack mounted at the base of the probe. Results from the tests are presented and compared, and application for predicting fracture probability of large arrays of devices are considered.

Kuhn, Jonathan, L.↗
DOE OSTI2024

Structural Changes in YBa 2 Cu 3 O 7 Thin Films Modified with He + -Focused Ion Beam for High-Temperature Superconductive Nanoelectronics

Irradiation of high-temperature superconductor YBa 2 Cu 3 O 7 (YBCO) with high-energy He + ions is known to cause structural changes in the YBCO film, decreasing the critical temperature T C and finally leading to a superconductor-to-insulator transition. Here, this allows one to pattern narrow insulating regions with a focused ion beam (FIB) and thus fabricate nanoscale Josephson junctions on YBCO films. Moreover, such ion irradiation is known to cause structural changes in the YBCO film. However, details of how these structural changes occur in nanoscale devices produced by FIB remain unknown. Using nanofocus X-ray diffraction, we study the changes in the YBCO crystal lattice and investigate how the nature of these changes depends on the size of the irradiated regions. These data provide an important understanding of how oxide superconductors can be tailored at the nanometer scale for various applications.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2023

Plasma Focused Ion Beam Nanothermometry

In this report we detail demonstration of temperature dependent effects on grayscale intensity imaged in Focused Ion Beam (FIB) microscope, as well as secondary electron (SE) dependence on temperature in the Auger Electron Spectroscopy (AES) and a Scanning Electron Microscope (SEM). In each instrument an intrinsic silicon sample is imaged at multiple temperatures over the course of each experiment. The grayscale intensity is shown to scale with sample temperature. Sample preparation procedures are discussed, along with hypothesized explanations for unsuccessful trials. Anticipated outcomes and future directions for these measurements are also detailed.

77 NANOSCIENCE AND NANOTECHNOLOGY↗
NASA NTRS2022

Mechanisms of Heavy Ion-, Focused X-Ray-, and Pulsed Laser-Induced Single Event Transients in an Epitaxial Silicon Diode

Heavy ion-, focused X ray-, and pulsed laser induced single event effects in an epitaxial silicon diode were simulated using Sentaurus Technology Computer Aided Design (TCAD). The variation of the potential with time in simulation agrees with previous experimental data, which suggests that the different radiation sources result in different amounts of potential modulation. The charge generation spatial profile strongly affects the potential modulation. The longitudinal range and starting location of generated charge most strongly impacts the amount of potential modulation, while the radial width has a slight effect, and the temporal duration of charge injection has negligible impact on potential modulation

Kaitlyn L. Ryder↗
NASA NTRS1988

GaAs/GaAlAs distributed Bragg reflector laser with a focused ion beam, low dose dopant implanted grating

The performance of a GaAs/GaAlAs distributed Bragg reflector (DBR) laser using a focused ion beam implanted grating (FIB-DBR) is reported for the first time. Stripes of Si(2+) with a period of 2300 A and a dose about 10 to the 14th/sq cm are directly implanted into the passive large optical cavity layer to provide the distributed feedback. Surface-emitting light from the second-order grating is observed. Threshold current of 110 mA and single DBR mode operation from 20 to 40 C are obtained. The wavelength tuning rate with temperature is 0.8 A/C. The coupling coefficient is estimated to be 15/cm. The results show that FIB technology is practical for distributed feedback and DBR lasers and optoelectronic integrated circuits.

Wu, M. C.↗
DOE OSTI2025

Impacts of Focused Ion Beam Processing on the Fabrication of Nanoscale Functionalized Probes

Herein, we examine the impact of Ga + ion kinetic energy and the target material type on the extent of ion implantation and structural damage in atomic force microscopy probes made of Al 2 O 3 and ZnO manufactured by focused ion beam (FIB) using scanning transmission electron microscopy and energy-dispersive X-ray mapping. Penetration of Ga into the Al 2 O 3 lattice induced structural distortions and amorphization. For ZnO probes, Ga is uniformly dispersed across the surface, resulting in the formation of distinct clusters. Atom probe tomography further validates the Ga distributions in Al 2 O 3 and ZnO nanoprobes. Complementary Monte Carlo simulations with the transport of ions in the matter program indicated that the introduction of Ga + prompts the generation of cation and anion vacancies, an occurrence more pronounced in Al 2 O 3 compared to ZnO. In conclusion, this study not only enriches the knowledge of ion-matter interactions, but also serves as a practical guide for the fabrication of nanoscale functionalized AFM probes.

Al2O3↗
DOE OSTI2024

Optimal Geometry for Focused Ion Beam-Milled Samples for Direct-Pull Micro-Tensile Testing Performed In Situ in a Scanning Electron Microscope

A thorough procedure was developed to efficiently manufacture dogbone samples using focused ion beam (FIB) milling for micro-tensile testing. A Bruker PI 89 PicoIndenter, Billerica, MA, USA, was used as a case study, although the analysis and results are applicable to other micro-mechanical testing systems capable of mounting a standard, Ø12.7 mm × Ø3.2 mm pin, scanning electron microscopy (SEM) pin stub (Ted Pella, Redding, CA, USA). Nine dogbones were made from an Fe-45Cu alloy additively manufactured using powder-fed laser-directed energy deposition (DED-LB). Testing showed that fracture was confined to the gauge section for all dogbones and that the fracture mode, ductile vs. brittle, was entirely dependent on the grain orientation relative to the loading direction. The analysis showed that the measured plastic strain to failure can vary from >11% (optimal geometry) to <1% (non-optimal geometry) in micro-tensile testing of high-tensile-strength (>1 GPa) metallic materials. Subsequently, a finite element analysis (FEA) was conducted to identify the improved dogbone geometries. A total of ten thousand dogbone geometries were tested, and their dimensions were defined by a set of four adjustable parameters (corner radius, load surface angle, load surface length, and dogbone head length). The gauge width and gauge length were fixed to 4 µm and 10 µm, respectively. Three-dimensional surface plots of the stress concentration as a function of two parameters were used to identify the optimal ranges of parameter values. The addition of maximum width and length constraints, measuring 25 µm and 30 µm, respectively, allowed us to identify an optimal geometry at load surface angles of 30° and 45°. Their respective dimensions (corner radius, load surface length, and dogbone head length) are, in µm, 12, 6, and 7 and 10, 7, and 7. Testing these two optimal geometries with a range of gauge lengths from 4 to 20 µm showed that smaller gauge lengths only slightly reduced the detrimental stress concentration outside the gauge section. However, smaller gauge lengths will notably improve the FIB surface polishing step as tapering is reduced with smaller dogbone lengths.

Chemistry↗
NASA NTRS2006

Focused Ion Beam Recovery of Hypervelocity Impact Residue in Experimental Craters on Metallic Foils

The Stardust sample return capsule will return to Earth in January 2006 with primitive debris collected from Comet 81P/Wild-2 during the fly-by encounter in 2004. In addition to the cometary particles embedded in low-density silica aerogel, there will be microcraters preserved in the Al foils (1100 series; 100 micrometers thick) that are wrapped around the sample tray assembly. Soda lime spheres (approximately 49 m in diameter) have been accelerated with a light-gas-gun into flight-grade Al foils at 6.35 km s(sup -1) to simulate the potential capture of cometary debris. The preserved crater penetrations have been analyzed using scanning electron microscopy (SEM) and x-ray energy dispersive spectroscopy (EDX) to locate and characterize remnants of the projectile material remaining within the craters. In addition, ion beam induced secondary electron imaging has proven particularly useful in identifying areas within the craters that contain residue material. Finally, high-precision focused ion beam (FIB) milling has been used to isolate and then extract an individual melt residue droplet from the interior wall of an impact penetration. This enabled further detailed elemental characterization, free from the background contamination of the Al foil substrate. The ability to recover pure melt residues using FIB will significantly extend the interpretations of the residue chemistry preserved in the Al foils returned by Stardust.

Graham, G. A.↗
DOE OSTI2026

Integrated fluorescence light microscopy-guided cryo-focused ion beam-milling for in situ montage cryo-ET

Cryogenic-electron tomography (cryo-ET) permits the in situ visualization of biological macromolecules at the molecular level. Owing to the variable thickness of cells, tissues and organisms, frozen specimens may need to be thinned by cryo-focused ion beam (FIB) milling to produce thin (<500 nm) cryo-lamellae suitable for cryo-ET. Locating regions of interest remains a challenge because untargeted milling can lead to inadvertent ablation and removal of regions of interest. Correlative light and electron microscopy, combined with cryo-FIB milling, can guide the identification of labeled targets in the cellular milieu. Multiple transfers between cryo-imaging instruments, cumbersome correlation algorithms, limited accuracy and low throughput have hindered the routine adoption of cryo-FIB milling within a multimodal correlative workflow for in situ structural biology. Here, in this study, we present a workflow for 3D correlative cryo-fluorescence light microscopy-FIB-ET that streamlines fluorescence light microscopy-guided FIB milling, improving throughput while preserving both structural and contextual information. The complete integration of hardware and software described here minimizes sample contamination from cross-platform exchanges and greatly enhances the efficiency of 3D targeting in cryo-milling. We then describe procedures for implementing montage parallel array cryo-ET (MPACT), which can be easily adapted to any modern life-science transmission electron microscope. MPACT supports high-throughput cryo-ET acquisitions (10 tilt series in 1.5 h) for structure determination and comprehensive contextual understanding of macromolecules within their native surroundings. A complete session from sample preparation to MPACT data processing takes 5−7 d for an individual experienced in both cryo-EM and cryo-FIB milling.

Yang, Jie E. [Univ. of Wisconsin, Madison, WI (Uni↗
NASA NTRS2005

Focused Ion Beam Microscopy of ALH84001 Carbonate Disks

Our aim is to understand the mechanism(s) of formation of carbonate assemblages in ALH84001. A prerequisite is that a detailed characterization of the chemical and physical properties of the carbonate be established. We present here analyses by transmission electron microscopy (TEM) of carbonate thin sections produced by both focused ion beam (FIB) sectioning and ultramicrotomy. Our results suggest that the formation of ALH84001 carbonate assemblages were produced by considerably more complex process(es) than simple aqueous precipitation followed by partial thermal decomposition as proposed by other investigators [e.g., 1-3].

Thomas-Keprta, Kathie L.↗
DOE OSTI2022

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. Here, 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.

36 MATERIALS SCIENCE↗
NASA NTRS2004

Focused Ion Beam Recovery and Analysis of Interplanetary Dust Particles (IDPs) and Stardust Analogues

Meteoritics research is a major beneficiary of recent developments in analytical instrumentation [1,2]. Integrated studies in which multiple analytical techniques are applied to the same specimen are providing new insight about the nature of IDPs [1]. Such studies are dependent on the ability to prepare specimens that can be analyzed in multiple instruments. Focused ion beam (FIB) microscopy has revolutionized specimen preparation in materials science [3]. Although FIB has successfully been used for a few IDP and meteorite studies [1,4-6], it has yet to be widely utilized in meteoritics. We are using FIB for integrated TEM/NanoSIMS/synchrotron infrared (IR) studies [1].

Graham, G. A.↗