Electron microbeam testing of integrated circuits
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Crawford, C. K.↗
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Microbeam analysis of four chondritic interplanetary dust particles for major elements, carbon and oxygen
Chemical compositions determined using electron excited X-rays are reported for four interplanetary dust particles collected in the stratosphere. These analyses include measurements of carbon and oxygen abundances which are important elements in these primitive materials. Spot analyses show very heterogeneous compositions on a micrometer scale although average composition approaches that of C1 carbonaceous chondrites. While the spot analyses show intermediate compositions between cometary dust and carbonaceous chondrites, the heterogeneity more closely resembles that of comet Halley dust particles.
Blanford, G. E.↗
Microbeam Investigations of Presolar and Early Solar System Materials
This grant provided three years of funding to initiate an independent research program in Cosmochemistry at Arizona State University. Because the new equipment that was installed at ASU took longer than expected to get running, the project was extended for a fourth year with no additional funding. By the time the funds were expended, we had set up an entirely new ion microprobe laboratory at ASU, and we have been fully operational for over two years. This laboratory was funded in almost equal parts by NASA, NSF, and ASU. Papers describing the first results from this new laboratory are being published now, and the results have been making an impact on the Cosmochemistry community. While this laboratory was being built, I continued my research program in collaboration with G. J. Wasserburg at Caltech. As equipment became available, I gradually shifted my research to ASU. Over the lifetime of this grant, my research program resulted in 12 papers and 13 abstracts on topics ranging from presolar grains (2 papers, 3 abstracts), short-lived radionuclides (6 papers, 6 abstracts), chemical compositions of chondritic materials (3 papers, 3 abstracts), silicon isotopic fractionation (1 abstract), and the oxygen composition of the Sun (1 paper). The most important results of this period were the discovery of presolar hibonite in a meteorite residue, the measurement of 26A1 in CAIs from enstatite chondrites, and the measurements of 10Be in type A CAIs from CV chondrites. All of these results have had a significant impact on research in Cosmochemstry.
Huss, Gary R.↗
The Mars Microbeam Raman Spectrometer: An Improved Advanced Brassboard
An advanced brassboard (ADBB) of the Mars Miscrobeam Raman Spectrometer is being developed. The probe and spectrograph have been redesigned with improved optics and the electronics have been miniaturized. The modified optical design in the probe and spectrograph provides better spectral resolution than the previous model and enables the probe design to be more compatible with robotic arm deployment. The CCD detector is now cooled thermoelectrically in anticipation of eventual terrestrial field testing of the instrument.
Haskin, L. A.↗
Oxygen Isotopes in Early Solar System Materials: A Perspective Based on Microbeam Analyses of Chondrules from CV Carbonaceous Chondrites
Some of the biggest challenges to understanding the early history of the solar system include determining the distribution of oxygen isotopes amongst materials that existed in the solar nebula, and interpreting the processes that might have resulted in the observed isotopic distributions. Oxygen isotope ratios in any individual mineral grain from a chondritic meteorite may be the cumulative product of a variety of processes, including stellar nucleosynthetic events, gas/solid interactions in the molecular cloud, mixing of independent isotopic reservoirs in the nebula, mass-independent processing in the nebula, and mass-dependent fractionation effects in various environments. It is not possible to unravel this complex isotopic record unless the distribution of oxygen isotope ratios in chondritic materials is fully understood.
Jones, R. H.↗
Microbeam studies of the sensitivity of structures within living cells
Determining the biological effects of low doses of radiation with high linear energy transfer (LET) is complicated by the stochastic nature of charged-particle interactions. Populations of cells exposed to very low radiation doses contain a few cells which have been hit by a charged particle, while the majority of the cells receive no radiation damage. At somewhat higher doses, a few cells receive two or more events. Because the effects of damage produced by separate events can interact in the cell, we have had to make assumptions about the nature of these interactions in order to interpret the results of the experiments. Many of those assumptions can be tested if we can be sure of the number of charged-particle events which occur in individual cells, and correlate this number with the biological effect. We have developed a special irradiation facility at Pacific Northwest Laboratory (PNL) to control the actual number of charged particle tracks that pass through cell nuclei. The beam from a 2 MeV tandem accelerator is collimated to approximately 5 microns. Cells, grown in special dishes with 1.5 microns thick plastic bottoms, are positioned so that the desired portion of the cell aligns with the collimator. A shutter in the beam line is opened and closed after the desired number of particle tracks has been counted. This approach can be used to investigate the effects of the interaction between irradiated and unirradiated cells in an organized system, as well as to study the effects of spatial and temporal distribution of radiation damage within single cells.(ABSTRACT TRUNCATED AT 250 WORDS).
Non-NASA Center↗
Microbeam Investigations of Presolar and Early Solar System Materials
This grant provided three years of funding for my Cosmochemistry research program at Arizona State University. This research resulted in 11 peer-reviewed papers in six Journals and 35 abstracts to 11 Conferences and Workshops (see list below). My original proposal listed three main areas of research: 1) Studies of presolar grains; 2) Studies of short-lived radionuclides and; 3) Investigations of nebular processes and the origin of chondritic components.
Huss, Gary R.↗
Characterization of Apollo Regolith by X-Ray and Electron Microbeam Techniques: An Analog for Future Sample Return Missions
The Apollo missions collected 382 kg of rock and regolith from the Moon; approximately 1/3 of the sample mass collected was regolith. Lunar regolith consists of well mixed rocks, minerals, and glasses less than 1-centimeter n size. The majority of most surface regolith samples were sieved into less than 1, 1-2, 2-4, and 4-10- millimiter size fractions; a portion of most samples was re-served unsieved. The initial characterization and classification of most Apollo regolith particles was done primarily by binocular microscopy. Optical classification of regolith is difficult because (1) the finest fraction of the regolith coats and obscures the textures of the larger particles, and (b) not all lithologies or minerals are uniquely identifiable optically. In recent years, we have begun to use more modern x-ray beam techniques [1-3], coupled with high resolution 3D optical imaging techniques [4] to characterize Apollo and meteorite samples as part of the curation process. These techniques, particularly in concert with SEM imaging of less than 1-millimeter regolith grain mounts, allow for the rapid characterization of the components within a regolith.
Zeigler, Ryan A.↗
Multimodal, microspectroscopic speciation of legacy phosphorus in two US mid-Atlantic agricultural soils
To understand phosphorus (P) mobility in agricultural soils and its potential environmental risk, it is essential to directly measure solid phase P speciation. Often, bulk P K-edge X-ray absorption near edge structure (XANES) spectroscopy followed by linear combination fitting (LCF) is utilized to determine the solid P phases in soil. However, this method may limit results to only a few major phases. Additionally, XANES spectra for different P species may have very similar features, leading to an over- or underestimate of their contribution to LCF. Here, an improved P speciation by pairing multimodal microbeam-X-ray fluorescence (µ-XRF) mapping coupled with µ-XANES (microbeam-X-ray absorption near edge structure) analysis to directly speciate major and minor P phases on the micron scale is provided. We combined maps of both tender (P, sulfur, aluminum, and silicon) and hard energy (calcium, iron [Fe], and manganese) elements to evaluate the elemental co-locations with P. To better account for uncertainty assigning XANES peaks to individual compounds, a more quantitative fingerprinting by “spectral feature analysis” was completed. With this analysis, an R-factor is reported for the fit. These results were compared to traditional LCF. Pre-edge fitting results revealed the presence of a two-component pre-edge feature for phosphate adsorbed to ferrihydrite. Additionally, phytate co-precipitated with ferrihydrite (Phytate-Fe-Cop) had a pre-edge feature, indicating direct association with Fe. Lastly, a unique P species associated with manganese oxide was identified in the soil via multimodal mapping and µ-XANES. These results allow for better prediction of P dissolution and mobility.
36 MATERIALS SCIENCE↗
A dual dynamic shutter system for accelerating ion irradiation sample throughput via lateral gas implantation gradients
Ion irradiation for material performance testing is limited due to its serial nature, which allows for only one value of the implantation (appm) versus dose (dpa) parameter space to be explored for each ion and experiment at a time. While ion irradiation can accelerate the process by up to three orders of magnitude compared to neutron irradiation experiments, the sample throughput for ion irradiation remains relatively low. To address these limitations, a novel capability has been developed at the Michigan Ion Beam Laboratory (MIBL), enabling for the creation of single- and two-dimensional lateral ion implantation gradients using recently installed motorized-controlled ion-beam shutters. This advancement can generate a wide scope of the two-dimensional (H+, He2+) implantation parameter space within a single sample. Integration of this new capability now allows for dual- and triple-ion beam experiments to be performed with full user control over not only the ion implantation depth, but also laterally across the sample by imposing ion implantation concentration gradients, thus providing researchers with a high-throughput means for material testing under various irradiation conditions. Furthermore, recent improvements in MIBL's microbeam ion-beam analysis (IBA) target station now allow for probing these concentration gradients in irradiated alloys with exceptional spatial resolution, down to 10 µm. These two approaches promise to significantly improve ion irradiation capabilities and increase the sample throughput by several orders of magnitude. The application of the shutter technique plus the subsequent microbeam characterization of the imposed implantation gradients are showcased by two proof-of-principle ion-irradiated experiments, one performed on single-crystal Si and the other on the fusion-candidate alloy F82H-IEA. These advancements mark a substantial leap in ion-beam technology, offering researchers a robust, high-throughput method to efficiently investigate candidate alloys with high technological readiness for both advanced fission and fusion reactor applications, in a time- and cost-effective manner.
36 - MATERIALS SCIENCE↗
Refinements for Bragg coherent X-ray diffraction imaging: electron backscatter diffraction alignment and strain field computation
Bragg coherent X-ray diffraction imaging (BCDI) allows the 3D measurement of lattice strain along the scattering vector for specific microcrystals. If at least three linearly independent reflections are measured, the 3D variation of the full lattice strain tensor within the microcrystal can be recovered. However, this requires knowledge of the crystal orientation, which is typically attained via estimates based on crystal geometry or synchrotron microbeam Laue diffraction measurements. Presented here is an alternative method to determine the crystal orientation for BCDI measurements using electron backscatter diffraction (EBSD) to align Fe–Ni and Co–Fe alloy microcrystals on three different substrates. The orientation matrix is calculated from EBSD Euler angles and compared with the orientation determined using microbeam Laue diffraction. The average angular mismatch between the orientation matrices is less than ∼6°, which is reasonable for the search for Bragg reflections. The use of an orientation matrix derived from EBSD is demonstrated to align and measure five reflections for a single Fe–Ni microcrystal via multi-reflection BCDI. Using this data set, a refined strain field computation based on the gradient of the complex exponential of the phase is developed. This approach is shown to increase accuracy, especially in the presence of dislocations. The results demonstrate the feasibility of using EBSD to pre-align BCDI samples and the application of more efficient approaches to determine the full lattice strain tensor with greater accuracy.
42 ENGINEERING↗
In Situ Synchrotron X-ray Micro-Diffraction Investigation of Elastic Strains in Laminated Ti-Al Composites
Spatially resolved elastic strains in the bulk interior of a laminated Ti-Al metal composite were studied during in situ tensile loading at strains up to 1.66% by a synchrotron-based micro-diffraction technique, namely differential aperture X-ray microscopy (DAXM). For both Al and Ti grains, deviatoric elastic strains were estimated based on polychromatic X-ray microbeam diffraction, while lattice strains along the normal direction of the tensile sample were directly measured using monochromatic X-ray microbeam diffraction. The estimated deviatoric strains show large spatial variations, and the mean values are consistent with the external loading conditions, i.e., increasing tensile strain along the tensile direction and increasing compressive strain along the sample normal with increasing loading. The directly measured lattice strains also show large spatial variations, although the magnitude of this variation is smaller than that for the estimated deviatoric strain. The directly measured lattice strains in Ti grains are largely consistent with the external loading, whereas those in Al grains are in contradiction with the external loading. The causes of the experimental results are discussed and related to both the laminated microstructure of the composite material and the limitations of the techniques.
36 MATERIALS SCIENCE↗
Single Event Transient Analysis of an SOI Operational Amplifier for Use in Low-Temperature Martian Exploration
The next generation of Martian rover#s to be launched by JPL are to examine polar regions where temperatures are extremely low and the absence of an earth-like atmosphere results in high levels of cosmic radiation at ground level. Cosmic rays lead to a plethora of radiation effects including Single Event Transients (SET) which can severely degrade microelectronic functionality. As such, a radiation-hardened, temperature compensated CMOS Single-On-Insulator (SOI) Operational Amplifier has been designed for JPL by the University of Tennessee and fabricated by Honeywell using the SOI V process. SOI technology has been shownto be far less sensitive to transient effects than both bulk and epilayer Si. Broad beam heavy-ion tests at the University of Texas A&M using Kr and Xebeams of energy 25MeV/amu were performed to ascertain the duration and severity of the SET for the op-amp configured for a low and high gain application. However, some ambiguity regarding the location of transient formation required the use of a focused MeV ion microbeam. A 36MeV O6(+) microbeam. the Sandia National Laboratory (SNL) was used to image and verify regions of particular concern. This is a viewgraph presentation
operational amplifier↗
High-Speed Single-Event Current Transient Measurements in SiGe HBTs
Time-resolved ion beam induced charge reveals heavy ion response of IBM 5AM SiGe HBT: 1) Position correlation. 2) Unique response for different bias schemes. 3) Similarities to TPA pulsed-laser data. Heavy ion broad-beam transients provide more realistic device response: 1) Feedback using microbeam data 2) Overcome existing issues of LET and ion range with microbeam Both micro- and broad-beam data sets yield valuable input for TCAD simulations. Uncover detailed mechanisms for SiGe HBTs and other devices fabricated on lightly-doped substrates.
Pellish, Jonathan A.↗
Heavy Ion Current Transients in SiGe HBTs
Time-resolved ion beam induced charge reveals heavy ion response of IBM 5AM SiGe HBT: a) Position correlation[ b) Unique response for different bias schemes; c) Similarities to TPA pulsed-laser data. Heavy ion broad-beam transients provide more realistic device response: a) Feedback using microbeam data; b) Overcome issues of LET and ion range with microbeam. Both micro- and broad-beam data sets yield valuable input for TCAD simulations. Uncover detailed mechanisms for SiGe HBTs and other devices fabricated on lightly-doped substrates.
Pellish, Jonathan A.↗
In-situ X-ray scattering study of isotactic polypropylene/graphene nanocomposites under shear during fused deposition modeling 3D printing
Complementary techniques were applied to characterize the structure property relationships of FDM printed isotactic polypropylene/graphene nanocomposites. Raman spectroscopy indicated that graphene was mostly exfoliated during the nozzle extrusion process. Rheological measurements of the viscosity indicated that the presence of graphene induced shear thinning during extrusion. Azimuthal scans of wide angle x-ray scattering indicate correlated thermal fluctuations of the graphene platelets which stops abruptly at the onset of transcrystallization, or templating of the iPP chains on the graphene. X-ray microbeam SAXS analysis show the formation of ‘shish-kebab’ structures at the core of the unfilled filaments, where the ‘kebab’ component vanishes at the fiber-fiber interface enabling interdiffusion. Weak lamellar structure, and a corresponding decrease in the storage modulus are observed with the addition of 5% graphene. The lamellar structure disappears entirely with the addition of 10% graphene, while the storage modulus is decreased by nearly 50%. Thermal imaging of heat flux dissipation across molded and printed samples shows no orientational effects in pure iPP despite differences in crystal structure. Thermal conductivity increases dramatically in the samples with 10% graphene, and strong orientational effects are observed where the thermal coefficients differ by 180% between samples printed parallel or perpendicular to the heat flux.
36 MATERIALS SCIENCE↗
Fracture resistance of hierarchical Cu–Mo nanocomposite thin films
We report the fracture behavior of high-temperature co-sputtered Cu/Mo nanocomposite thin films was investigated through in situ 3-point bend testing of pre-notched microbeams in SEM. The as-synthesized nanocomposites present hierarchical nano/microstructures composed of a matrix of phase-separated Cu–Mo with nanoscale ligaments dispersed with sub-micron scale Cu-rich islands containing Mo nano-precipitates. Results show a significant crack growth resistance in the hierarchical nanocomposite, several times higher than that measured in Cu/Mo nanoscale multilayers. Based on electron microscopy characterization, three mechanisms of crack growth resistance in the hierarchical structures are proposed: crack bridging by the Cu-rich layer, crack deflection via shear along the Cu/Mo interface, and multiple cracking. This work demonstrates an approach to increase toughness in high strength nanocomposites through interface micro-structure design.
36 MATERIALS SCIENCE↗
Carbonated apatite lattice parameter variation across incremental growth lines in teeth
Here, results of microbeam mapping (x-ray excited x-ray fluorescence and transmission x-ray diffraction) of Beluga whale cementum and of beaver dentin reveal growth bands are defined by variation in mineral content (carbonated hydroxyapatite, cAp), by variation in Zn content and by variation in cAp lattice parameter a. For both tissues, diffraction and fluorescence data show that Zn signal and a are anti-correlated, that is high Zn signal is co-located with low a, and vice versa. In cementum and bone, treatment with acid removes Ca, Zn and cAp. The data are strong evidence that Zn is incorporated into the cAp lattice in these tissues and that the amount of Zn incorporated varies across two very different types of growth bands, annual bands in Beluga cementum and daily incremental bands in beaver dentin. To the best of the authors’ knowledge, this is the first observation of spatial variation of lattice parameter within growth bands.
36 MATERIALS SCIENCE↗