Nanogeology of metamorphic magnetite using three-dimensional atom probe and focused ion beam secondary mass spectroscopy
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nonorthogonal MEMS three-dimensional atom probe x-↗
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Novel Applications of Focused Ion Beam Technique for Planetary Sample Analyses
We are using innovative FIB techniques to prepare samples of planetary materials for different types of coordinated analyses using ion microprobes, synchrotron beamlines, and specialized transmission electron microscopy (TEM) techniques. In these cases, the FIB sample preparation is the critical step in enabling these specialized analyses. We discuss several examples below utilizing the FEI Quanta3D instrument at the NASA Johnson Space Center. Trace element analyses utilizing synchrotron x-ray fluorescence. The trace element content of mineral grains in comet dust provides important clues on their formation and processing in the early solar system. We preformed coordinated analyses of a comet dust particle that had been prepared using ultramicrotomy for TEM analysis. Following the TEM analyses, we extracted a 70 nm thick section from a region of the carbon (C) film of the TEM grid, for additional analyses. A carbon ring ~2-3 μm thick was deposited on top of the C film using the FIB. The C film on the outer rim of the ring was milled away using various patterns to uniformly release the stresses on the film, preventing rupture and collapse, and was attached to the micromanipulator needle. We then isolated the ring completely and transferred the section to a silicon sample holder for analysis using the HXN (hard X-ray nanoprobe) beamline at NSLSII at Brookhaven National Lab. Coordinated Analyses of Presolar Grains. Rare sub-m presolar grains that originate in evolved stars and supernovae, occur in primitive astromaterials and are identified by their exotic isotopic compositions. Coordinated analyses of these grains using NanoSIMS, TEM, and other techniques on the same grain is enabled by innovative FIB sample preparation. In order to obtain subsequent isotopic analyses of Mg and Fe, contributions from surrounding grains were minimized. We precisely deposited a protective cap of Pt on top of the grain to preserve the grain of interest and then milled away about 5 μm diameter of the surrounding material. Following the isotopic analyses, the spindle was extracted and thinned to electron transparency for TEM microstructural analyses. In situ heating TEM experiments on lunar samples. We extracted a FIB thin section from Apollo 17 lunar rock 76015. To avoid ion-beam damage, e-beam deposition was used to deposit the first 500 nm of the C strap, followed by ion beam-assisted deposition of ~3 μm carbon. We performed an ex situ lift-out of the section and placed the section on one of the elements of a microelectromechanical systems (MEMS) - specialized heating substrate and attached the section to the substrate by depositing small C straps with the FIB. The heating chips utilize silicon nitride windows to support the samples and provide uniform heating while enabling TEM imaging. The heating chip was loaded into a Hitachi “Blaze” heating holder and analyzed using a Hitachi HF5000 at the University of Arizona.
Rahman, Z.↗
Comparison of Single-Event Transients in an Epitaxial Silicon Diode Resulting from Heavy Ion-, Focused X-Ray-, and Pulsed Laser-Induced Charge Generation
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Kaitlyn L Ryder↗
Ion heating in a plasma focus
Ion acceleration and heating in a plasma focus were investigated by the numerical integration of the three-dimensional equations of motion. The electric and magnetic fields given were derived from experimental data. The results obtained show that during the collapse phase of focus formation, ions are efficiently heated to temperatures of several keV. During the phase of rapid current reduction, ions are accelerated to large velocities in the axial direction. The results obtained with the model are in general agreement with experimental results.
Hohl, F.↗
Ion extraction from a plasma
An experimental investigation of the physical processes governing ion extraction from a plasma is presented. The screen hole plasma sheath of a multiaperture ion accelerator system is defined by equipotential plots for a variety of accelerator system geometries and operating conditions. A sheath thickness of at least fifteen Debye lengths is shown to be typical. The electron density variation within the sheath satisfies a Maxwell Boltzmann density distribution at an effective electron temperature dependent on the discharge plasma primary to Maxwellian electron density ratio. Plasma ion flow up to and through the sheath is predominately one dimensional and the ions enter the sheath with a modified Bohm velocity. Low values of the screen grid thickness to screen hole diameter ratio give good ion focusing and high extracted ion currents because of the effect of screen webbing on ion focusing.
Aston, G.↗
Ion extraction from a plasma
The physical processes governing ion extraction from a plasma have been examined experimentally. The screen hole plasma sheath (the transition region wherein significant ion acceleration and complete electron retardation occurs) has been defined by equipotential plots for a variety of ion accelerator system geometries and operating conditions. It was found that the screen hole plasma sheath extends over a large distance, and influences ion and electron trajectories at least 15 Debye lengths within the discharge chamber. The electron density variation within the screen hole plasma sheath satisfied a Maxwell-Boltzmann density distribution at an effective electron temperature dependent on the discharge plasma primary-to-Maxwellian electron density ratio. Plasma ion flow up to and through the sheath was predominantly one-dimensional, and the ions entered the sheath region with a modified Bohm velocity. Low values of the screen grid thickness to screen hole diameter ratio were found to give good ion focusing and high extracted ion currents because of the effect of screen webbing on ion focusing.
Aston, G.↗
Genesis Solar Wind Science Canister Components Curated as Potential Solar Wind Collectors and Reference Contamination Sources
The Genesis mission collected solar wind for 27 months at Earth-Sun L1 on both passive and active collectors carried inside of a Science Canister, which was cleaned and assembled in an ISO Class 4 cleanroom prior to launch. The primary passive collectors, 271 individual hexagons and 30 half-hexagons of semiconductor materials, are described in. Since the hard landing reduced the 301 passive collectors to many thousand smaller fragments, characterization and posting in the online catalog remains a work in progress, with about 19% of the total area characterized to date. Other passive collectors, surfaces of opportunity, have been added to the online catalog. For species needing to be concentrated for precise measurement (e.g. oxygen and nitrogen isotopes) an energy-independent parabolic ion mirror focused ions onto a 6.2 cm diameter target. The target materials, as recovered after landing, are described in. The online catalog of these solar wind collectors, a work in progress, can be found at: http://curator.jsc.nasa.gov/gencatalog/index.cfm This paper describes the next step, the cataloging of pieces of the Science Canister, which were surfaces exposed to the solar wind or component materials adjacent to solar wind collectors which may have contributed contamination.
Allton, J. H.↗
Ion-beam focusing in a double-plasma device
The authors studied the propagation of a low-energy charge-neutralized ion beam injected into the target region of a long double-plasma device. A magnetic field of up to about 180 G may be applied along the axis of the device. As a result of charge exchange collisions, the ion beam is attenuated as it propagates into the target region. However, under certain conditions of magnetic field strength and neutral gas pressure, the authors have observed a `reemergence' of the beam on axis far downstream in the target. This reemergence of the ion beam is attributed to a focusing of the ions by a self-consistently produced radial ambipolar electric field. The effect may be expected to occur in other types of plasma devices as well, whenever a sufficiently large radially inward electric field is present.
Johnson, James C.↗
New Methods of Sample Preparation for Atom Probe Specimens
Magnetite is a common conductive mineral found on Earth and Mars. Disk-shaped precipitates approximately 40 nm in diameter have been shown to have manganese and aluminum concentrations. Atom-probe field-ion microscopy (APFIM) is the only technique that can potentially quantify the composition of these precipitates. APFIM will be used to characterize geological and planetary materials, analyze samples of interest for geomicrobiology; and, for the metrology of nanoscale instrumentation. Prior to APFIM sample preparation was conducted by electropolishing, the method of sharp shards (MSS), or Bosch process (deep reactive ion etching) with focused ion beam (FIB) milling as a final step. However, new methods are required for difficult samples. Many materials are not easily fabricated using electropolishing, MSS, or the Bosch process, FIB milling is slow and expensive, and wet chemistry and the reactive ion etching are typically limited to Si and other semiconductors. APFIM sample preparation using the dicing saw is commonly used to section semiconductor wafers into individual devices following manufacture. The dicing saw is a time-effective method for preparing high aspect ratio posts of poorly conducting materials. Femtosecond laser micromachining is also suitable for preparation of posts. FIB time required is reduced by about a factor of 10 and multi-tip specimens can easily be fabricated using the dicing saw.
rock varnish↗
Electronic drive and acquisition system for mass spectrometry
The present invention discloses a mixed signal RF drive electronics board that offers small, low power, reliable, and customizable method for driving and generating mass spectra from a mass spectrometer, and for control of other functions such as electron ionizer, ion focusing, single-ion detection, multi-channel data accumulation and, if desired, front-end interfaces such as pumps, valves, heaters, and columns.
Schaefer, Rembrandt Thomas↗
Ion collection from a plasma by a pinhole
Ion focusing by a biased pinhole is studied numerically. Laplace's equation is solved in 3-D for cylindrical symmetry on a constant grid to determine the potential field produced by a biased pinhole in a dielectric material. Focusing factors are studied for ions of uniform incident velocity with a 3-D Maxwellian distribution superimposed. Ion currents to the pinhole are found by particle tracking. The focusing factor of positive ions as a function of initial velocity, temperature, injection radius, and hole size is reported. For a typical Space Station Freedom environment (oxygen ions having a 4.5 eV ram energy, 0.1 eV temperature, and a -140 V biased pinhole), a focusing factor of 13.35 is found for a 1.5 mm radius pinhole.
Snyder, David B.↗
Micrometer to Atomic Scale Characterisation of Primitive Astromaterials Using A Novel Method, Metis-Fa: A Coordinated Atom Probe Tomography, Transmission Electron Microscopy and NanoSIMS Approach
Introduction: Presolar grains preserve isotopic, chemical and microstructural records of physical and chemical processing, and formation mechanisms within a vast range of evolved stellar systems, the interstellar medium, solar nebula and their parent bodies. These evolutionary records are preserved at the micrometric to atomic scale, requiring coordinated studies to expand our understanding of evolutionary processes occurringthroughout ours and external stellar systems [1]. NanoSIMS enabled rapid in situ identification and isotopic characterisation of presolar grains and their stellar origins using 17O/16O and 18O/16O, and 13C/12C isotopic ratios [1]. Coordination with transmission electron microscopy (TEM) revealed crystallographic and localised contextual relationships and quantitively constrained their major and minor compositions [1]. However, trace elements cannot be quantified, the most sensitive geochemical tracers of environmental conditions, essential to unravelling the chemical record of their evolutionary pathway and parent stellar systems [2-3] . Furthermore, owing to the combination of technical limitations (only 5 – 7 isotopes can be measured per NanoSIMS run) and their small grain sizes of 100 nm < 3 μm (with rare exceptions in nanodiamonds (2 nm ≤) and SiC (< 40 μm)), the number of measurable isotopes per grain volume is limited [1,3] . Through more comprehensive isotopic studies of presolar grains, NanoSIMS studies have shown the importance of the latter, identifying Fe and Mg as important indicators of nuclear synthetic processing and their stellar origins, respectively [4- 5]. Coordination of NanoSIMS and Atom Probe Tomography (APT) revealed morphological signatures, and isotopic and chemical signatures at major to trace levels without requirements for preselection of elements [6]. However, crystallographic signatures in localized contextual relationships cannot be measured. Consequently, coordination of NanoSIMS, TEM and APT is essential to gain access to almost all contextual, structural and geochemical signatures within each presolar grain.Transmission electron microscopy requires a 100 nm thin lamella which is unstable in APT and would not produce any viable data. Atom probe tomography requires a needle-shaped specimen which when measured in TEM removes the local context, impacts the quality of the TEM diffraction images due to the shank angle of the needle, and can alter the chemistry of beam sensitive materials from the higher degree of surface exposure at the tip. To address these issues, we developed METIS-Fa (Multi-technical measurements of Electron Transparent materials using an Indium Sandwich - a FIB approach). A novel method which enables coordination of NanoSIMS, TEM and APT for generalized and targeted studies of individual grains, including beam sensitive materials, without compromising sample preparation requirements for TEM and APT. This method requires only indium and a Focus Ion Beam (FIB), minimizing the movement of fragile materials while still enabling preparation of TEM lamella into APT needles. Samples: Initial experimental development and testing of the method occurred at Astromaterials Research and Exploration Science (ARES), Johnson Space Centre (JSC), NASA and APT measurements and needle preparation occurred at JdLC, Curtin University. Synthetic silicate samples were used as analogs for presolar silicates when performing a trial run of the method. Samples were extracted from a polished thin section created at JSC, NASA, comprised of 38 wt.% Si, 17 wt.% FeO, 13 wt.% MgO, 12 wt.% Al, 11 wt.% Ca based on electron microprobe analysis (EMPA) [8] . Experimental details, pressure and temperature conditions were presented in [8] and references therein. Testing of the capability to target individual grains in mineral matrices using this method for acquisition in APT, measured matrix regions in meteoritic thin sections of primitive meteorites. These meteorites and their identified presolar grains for future targeted studies are detailed in [9]. Techniques: The TEM-FIB lamella were prepared using a FIB. An e-beam assisted pt deposition was used as a protective coating for the synthetic and meteoritic samples. When targeting individual grains, a secondary e-beam assisted pt deposition button is placed over the desired grain before the protective coating to denote its location. A JEOL 2500SE field-emission TEM was used for high-resolution imaging, energy-dispersive X-ray (EDX) and electron diffraction data.TheMETIS-Fa method was experimentally designed, tested and executed using a FIB at ARES, JSCNASA. Needles for APT were prepared using the Tescan Lyra3 GM Dual Beam Focus Ion Beam (FIB) Field Emission SEM (FE-SEM) at the JdLC, Curtin University. Atom probe tomography measurements were conducted using a CAMECA Local Electrode Atom Probe, LEAP 4000X HR. Two pure indium needles were analyzed initially to constraining acquisition parameters and stability under the beam. Manual acquisition was required to maintain evaporation of specimen’s at the apex and monitor interactions with measurement parameters. Experimental Design: Indium foil is pressed onto an Al stub with a pneumatic press and mounted into the FIB adjacent to the TEM-FIB lamella of interest. Using a FIB, two indium slices (5 μm x ~300 nm x 3 μm) are extracted from indium foil and aligned with the TEM-FIB lamella before touching the TEM-FIB lamella. Each slice is then attached through cold welding to the FIB-TEM lamella. This approach eliminates the need for chemical treatments and proved effective for aligning the Indium within the region of interest for APT, holding it in place for up to 4 days during testing.Once both indium slices are attached within their pre-determined region per grain targeting requirements, they are gradually melted onto the FIB-TEM lamella.When targeting a specific grain, measurements should be taken of the pt button and its distance from edge to edge of the lamella before and after sandwiching. A secondary button should be placed over the same region after the Indium slices have been attached to improve precision when preparing APT needles. Results: Figure 1 shows two indium slices melted onto a FIB-TEM lamella, adding additional bulk for preparation into APT needles as shown in Figure 2 [7] . The latter was essential so samples could be measured in TEM and APT without compromising sample preparation requirements and consequently data quality and acquisition stability. METIS-Fa proved effective forimproving geometry. Figure 3 shows a successful APTrun of the synthetic silicate. EMPA, TEM and APTshowed no chemical alterations. During targetingtesting, a solar silicate grain was successfully identifiedand measured in TEM, and prepared into an APTneedle. However, the indium was melted too long during sample preparation, causing expansion andformation of internal porosity leading to sample loss.Conclusion: METIS-Fa greatly expands the number of isotopic and chemical signatures measured per grain volume, and enables measurements of contextual, structural, crystallographic, isotopic and geochemical signatures within individual grains. Gaining access to such a vast range of evolutionary signatures required for expanding our understanding of external stellar and planetary systems and the evolution of our solar system. This method was designed for application to a vast range of phases including being sensitive materials and thus provides a way for coordination of NanoSIMS, TEM and APT not just for the study of presolar grains and by extension primitive astromaterials, but studies in a vast range of other fields including the geosciences and material sciences.Acknowledgments: Thankyou to ARES, JSC, NASA; JdLC Curtin University and Space Science Technology Centre for the use of laboratory facilities and funding [confirm].
Nicole D Nevill↗
Investigating the Role of Incident Ion Flux in Solar Wind Space Weathering of Carbon-Rich Asteroidal Regolith Via H+ and He+ Irradiation of the Murchison Meteorite
We present results from a set of low and high flux 1 keV/amu H + and He + irradiation experiments performed on slabs of the Murchison CM2 carbonaceous chondrite. The low flux conditions for H + and He + irradiation were ~1-1.5 orders of magnitude lower than the high flux conditions, and each experiment was irradiated to a total fluence between ~3 × 10 16 to ~6 × 10 16 ions/cm 2 . Irradiation-induced changes in the surface chemistry and optical properties of the Murchison samples were evaluated using in situ X-ray photoelectron spectroscopy (XPS) and visible and near-infrared spectroscopy (VNIR). We characterized the microstructure and composition of ion damaged rims in focused ion beam (FIB) cross-sections extracted from olivine and matrix material in each irradiated Murchison slab using transmission electron microscopy (TEM). XPS results suggest that both low flux and high flux H + and He + irradiation cause minor sputtering of surface carbon as well as a reduction in the valence state of iron, from Fe 3+ to Fe 2+ . Slope bluing is observed in VNIR spectra of the irradiated samples which may reflect carbonization and dehydrogenation of organic species and contrasts with reddening trends associated with npFe 0 formation. Although we do not observe a strong flux-dependence on the crystallinity of ion-damaged olivine, TEM analyses reveal a variety of microstructures in all olivine FIB-sections, suggesting that crystallographic orientation affects amorphization efficiency. Analyses of matrix FIB-sections indicate that phyllosilicate alteration is mainly driven by He+ irradiation, where the higher incident flux leads to greater amorphization and the formation of more distinct ion-damaged layers, similar to smooth layers in returned Ryugu particles. TEM results also provide some evidence that higher ion flux leads to greater vesiculation, with He + irradiation being more efficient at vesiculation than H + irradiation, and that higher ion flux may promote the segregation of Mg and Si into laterally extensive lenses and layers in olivine samples. We discuss the implications of these findings for constraining the role that ion flux plays in the development of space weathering characteristics in silicate phases present in carbonaceous asteroidal regoliths. These results will be important for understanding the complexity of this process and how it operates on carbon-rich airless bodies like asteroids Bennu and Ryugu.
meteorites↗
Thermal Ion Transport on the Moon and the Formation of the Lunar Swirls
The bright "swirl" features observed on the lunar surface are generally associated with crustal magnetic anomalies. Prominent explanations that invoke these fields include: magnetic shielding in the form of a mini-magnetosphere, which impedes space weathering by the solar wind; magnetically controlled dust transport; and cometary or asteroidal impacts, that could result in shock magnetization with concomitant formation of the swirls. Here we consider another possibility in which the ambient magnetic and electric fields can transport and channel secondary ions produced by micrometeorite or solar wind ion impacts. We use a simplified model of the fields, which incorporates a two-dipole magnetic field model for Reiner Gamma, and typical solar wind conditions. We will present preliminarily results suggesting that ions created over significant regions of the lunar surface can be transported under the influence of local and interplanetary electromagnetic fields to narrow areas ncar arcas of high crustal magnetic field strength. The flux of these focused ions may be of sufficient intensity to chemically process (or otherwise bleach) the surface leading to the formation of the high albedo component of the lunar swirls. The theory is appealing since through a lensing effect, it is possible that this flux is sufficient to overcome other space weathering processes which would otherwise tend to erase the features. Also, with relatively low energy ions, and consistent with the observed focusing, the ion gyro radii in the local magnetic fields is small enough to resolve the swirls.
Keller, John W.↗
High performance auxiliary-propulsion ion thruster with ion-machined accelerator grid
An improvement in thruster performance was achieved by reducing the diameter of the accelerator grid holes. The smaller accelerator grid holes resulted in a reduction in neutral mercury atoms escaping the discharge chamber, which in turn enhanced the discharge propellant utilization from approximately 68 percent to 92 percent. The accelerator grids were fabricated by ion machining with an 8-centimeter-diameter thruster, and the screen grid holes individually focused ion beamlets onto the blank accelerator grid. The resulting accelerator grid holes are less than 1.12 millimeters in diameter, while previously used accelerator grids had hole diameters of 1.69 millimeters. The thruster could be operated with the small-hole accelerator grid at neutralizer potential.
Hudson, W. R.↗
The screen hole plasma sheath of an ion accelerator system
Results of the first probing of the screen hole sheath of an ion accelerator system are presented. The screen hole sheath, represented as a set of equipotential contours, extends over a large distance within the discharge plasma. Under no conditions examined does the sheath enter the screen hole. Edge hole defocusing of multiaperture accelerator systems is due primarily to local plasma density variations rather than adjacent screen hole sheath interactions. The sheath boundary is independent of screen-to-accelerator grid spacing when the grid set is operated at the minimum ion beam divergence condition. Significant ion focusing effects occur in the sheath adjacent to the screen grid webbing leading to increased ion source beam current efficiency with decreasing screen-to-accelerator grid separation and/or screen grid thickness.
Aston, G.↗