Enabling Planetary Science by Preserving Artificially Implanted Genesis Collector Materials
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Genesis Sample Return Mission↗
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The Genesis Non-flight Implant Sample Archive
Introduction: For the past 20 years the Genesis science community has been analyzing solar wind captured in sample collectors now curated at Johnson Space Center (JSC). Non-flown flight like collector materials (non-flight) considered reference material was always allocated by the JSC Genesis team for testing experimental procedures. However, to expedite Genesis science, distribution of non-flown reference materials were also provided by, D. S. Burnett (Genesis PI, Caltech) and A. J. G. Jurewicz (ASU) who were funded to aid all Genesis PIs by providing engineering test materials archived at Caltech pre-flight as well as ion implants into these materials [1]. Implanted materials (non-flight reference, flight-like semiconductor materials, and NIST SRM glass) received from the Caltech collection during a pilot project are being used to develop an accession procedure for the purpose of making these materials available to researchers in the future. These implant samples are important because they can be utilized as measurement standards [2]. This is a work in progress and this work reports progress in documentation and imaging. The pilot program received 63 implanted reference materials with known implanted ions. Genesis Non-Flight Database: The existing non-flight material database was modified to allow for the description of implant sessions and to allow correlation of the implant information to individual specimens. An implant session has three main components: a known ion, a known dose (ion/cm2), and a known energy (keV). Procedure: Laboratory Procedure. Upon receiving non-flight analytical standards (independently calibrated implants), or implant samples (nominally calibrated implants), they will be imaged in their current containers to capture any information written before being brought into the Genesis Sample Laboratory. Documentation is provided by the donor and used for correlating the data between the implant sessions and implant samples. This information is not verified by Genesis Curation. The microscope used to image samples in the laboratory has an automated stage with a stainless-steel plate to hold samples and a camera that utilizes the software Surveyor to take photomosaic images of the implant samples. The camera attached to the microscope is a QICAM High Performance IEEE 1394 FireWire Digital CCD Camera. This setup, shown in Fig. 1, allows for photomosaics of small-scale samples with a 10x objective or 25x objective. Examples of images taken with this microscope setup are shown in Fig.2 and Fig. 3. After imaging, samples get stored in a clean fluoroware container or polypropylene vial depending on sample size for long term storage. Database Procedure. The Genesis Non-Flight Database currently allows for the addition of implant sessions. The required fields for adding an implant session are the implant session ion, the implant session dose, and the implant session energy. There are also fields for the date and vendor of the sessions as well as a field for if the session was calibrated or not. Once an implant session has been inserted into the database, additional documentation from the session can be attached. The database will automatically assign an Implant Session Number. After inserting an implant session, the implanted samples can be inserted. The fields required for an implant sample are the material of the sample and the size of the sample. The Generic name for the implant sample with be automatically generated by the database once it has been inserted. Implant sample numbers begin with 3X to distinguish from flown Genesis sample numbers. There are also fields for processors to add the location (room, cabinet, tray) and container type (fluoroware, polypropylene vial). Once an implant session and an associated sample(s) have been inserted into the database the sample can be then tied to all associated implant sessions. An implant sample can be tied to multiple implant sessions. Future work: For curation, future work consists of creating an online catalogue for implant samples as well as updating the database with more samples as we receive them. For the scientific community these implant samples have many potential uses. For Genesis research, they are directly applicable for testing and, in some cases, as analytical standards. For non-Genesis research, implants (especially calibrated implants) could be used for calibrating other, unique planetary materials [1].
C D Calva↗
A feasibility study of ion implantation techniques for mass spectrometer calibration
An experimental study was undertaken to examine the feasibility of using ion-implanted filaments doped with either an alkali metal or noble gas for in situ recalibration of onboard mass spectrometers during extended space missions. Implants of rubidium and krypton in rhenium ribbon filaments were subsequently tested in a bakeable 60 deg sector mass spectrometer operating in the static mode. Surface ionization and electron impact ion sources were both used, each yielding satisfactory results. The metallic implant with subsequent ionization provided a means of mass scale calibration and determination of system operating parameters, whereas the noble gas thermally desorbed into the system was more suited for partial pressure and sensitivity determinations.
Koslin, M. E.↗
Benchmarking of X‐Ray Fluorescence Microscopy with Ion Beam Implanted Samples Showing Detection Sensitivity of Hundreds of Atoms
Abstract Single impurities in insulators are now often used for quantum sensors and single photon sources, while nanoscale semiconductor doping features are being constructed for electrical contacts in quantum technology devices, implying that new methods for sensitive, non‐destructive imaging of single‐ or few‐atom structures are needed. X‐ray fluorescence (XRF) can provide nanoscale imaging with chemical specificity, and features comprising as few as 100 000 atoms have been detected without any need for specialized or destructive sample preparation. Presently, the ultimate limits of sensitivity of XRF are unknown – here, gallium dopants in silicon are investigated using a high brilliance, synchrotron source collimated to a small spot. It is demonstrated that with a single‐pixel integration time of 1 s, the sensitivity is sufficient to identify a single isolated feature of only 3000 Ga impurities (a mass of just 350 zg). With increased integration (25 s), 650 impurities can be detected. The results are quantified using a calibration sample consisting of precisely controlled numbers of implanted atoms in nanometer‐sized structures. The results show that such features can now be mapped quantitatively when calibration samples are used, and suggest that, in the near future, planned upgrades to XRF facilities might achieve single‐atom sensitivity.
36 MATERIALS SCIENCE↗
Hydrogen isotope analysis in W-tiles using fs-LIBS
Abstract Laser-Induced Breakdown Spectroscopy (LIBS) is a promising technology for in-situ analysis of Plasma-Facing Components in magnetic confinement fusion facilities. It is of major interest to monitor the hydrogen isotope retention i.e. tritium and deuterium over many operation hours to guarantee safety and availability of the future reactor. In our studies we use ultraviolet femtosecond laser pulses to analyze tungsten (W) tiles that were exposed to a deuterium plasma in the linear plasma device PSI-2, which mimics conditions at the first wall. A high-resolution spectrometer is used to detect the Balmer- $$\alpha$$ α transition of the surface from implanted hydrogen isotopes (H and D). We use Calibration Free CF-LIBS to quantify the amount of deuterium stored in W. This proof-of-principle study shows the applicability of femtosecond lasers for the detection of low deuterium concentration as present in first wall material of prevailing fusion experiments.
70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
Depth profiling and standardization from the back side of a sample for accurate analyses: Emphasis on quantifying low‐fluence, shallow implants in diamond‐like carbon
Rationale Back‐side thinning of wafers is used to eliminate issues with transient sputtering when analyzing near‐surface element distributions. Precise and accurate calibrated implants are created by including a standard reference material during the implantation. Combining these methods allows accurate analysis of low‐fluence, shallow features even if matrix effects are a concern. Methods Implanted Na (<2.0 × 10 11 ions/cm 2 , peaking <50 nm) in diamond‐like carbon (DLC) film on silicon (solar wind returned by NASA's Genesis mission) was prepared for measurement as follows. Implanted surfaces of samples were epoxied to wafers and back‐side‐thinned using physical or chemical methods. Thinned samples were then implanted with reference ions for accurate quantification of the solar wind implant. Analyses used a CAMECA IMS 7f‐GEO SIMS in depth‐profiling mode. Results Back‐side‐implanted reference ions reduced the need to change sample mounts or stage position and could be spatially separated from the solar wind implant even when measuring monoisotopic ions. Matrix effects in DLC were mitigated and the need to find an identical piece of DLC for a reference implant was eliminated. Accuracy was only limited by the back‐side technique itself. Conclusions Combining back‐side depth profiling with back‐side‐implanted internal standards aides quantification of shallow mono‐ and polyisotopic implants. This technique helps mitigate matrix effects and keeps measurement conditions consistent. Depth profile acquisition times are longer, but if sample matrices are homogeneous, procedural changes can decrease measurement times.
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
Micromachined Piezoresistive-sensed Diaphragms for Infrasonic Monitoring
Micromachined, piezoresistive-sensed diaphragms are designed and fabricated specifically for infrasound sensing applications. Relatively large diaphragms, up to 6 mm × 6 mm, are fabricated to meet the high sensitivity requirements of infrasonic monitoring. A double-stack SOI wafer process is used, resulting in a streamlined two-mask process without the need for doping or ion-implantation. Pressure-sensitivities of diaphragms are studied using a custom static calibration set-up. Here, the piezoresistance of longitudinal and transverse resistors are studied over a large pressure range of ±5,500 Pa so that the linear and nonlinear response regions of diaphragms are observed. Measurements are compared against a nonlinear finite element simulation—shown to accurately predict the sensor’s behavior over a large response range.
47 OTHER INSTRUMENTATION↗
Ultrasonic Doppler measurement of renal artery blood flow
An extensive evaluation of the practical and theoretical limitations encountered in the use of totally implantable CW Doppler flowmeters is provided. Theoretical analyses, computer models, in-vitro and in-vivo calibration studies describe the sources and magnitudes of potential errors in the measurement of blood flow through the renal artery, as well as larger vessels in the circulatory system. The evaluation of new flowmeter/transducer systems and their use in physiological investigations is reported.
Freund, W. R.↗
Post-growth modulation doping by ion implantation
Modulation doping is a commonly adopted technique to create two-dimensional (2D) electrons or holes in semiconductor heterostructures. One constraint, however, is that the intentional dopants required for modulation doping are controlled and incorporated during the growth of heterostructures. Here, using undoped strained germanium quantum wells as the model material system, we show that modulation doping can be achieved post-growth of heterostructures by ion implantation and dopant-activation anneals. The carrier density is controlled ex situ by varying the ion fluence and implant energy, and an empirical calibration curve is obtained. While the mobility of the resulting 2D holes is lower than that in undoped heterostructure field-effect transistors built using the same material, the achievable carrier density is significantly higher. Potential applications of this modulation-doping technique are discussed.
42 ENGINEERING↗
An implantable blood pressure and flow transmitter.
A miniature totally implantable FM/FM telemetry system has been developed to simultaneously measure blood pressure and blood flow, thus providing an appreciation of the hemodynamics of the circulation to the entire body or to a particular organ. Developed for work with animal subjects, the telemetry system's transmission time is controlled by an RF signal that permits an operating life of several months. Pressure is detected by a miniature intravascular transducer and flow is detected by an extravascular interferometric ultrasonic technique. Both pressure and flow are calibrated prior to implanting. The pressure calibration can be checked after the implanting by cannulation; flow calibration can be verified only at the end of the experiment by determining the voltage output from the implanted sensing system as a function of several measured flow rates. The utility of this device has been established by its use in investigating canine renal circulation during exercise, emotional encounters, administration of drugs, and application of accelerative forces.
Rader, R. D.↗
Performance characteristics of STIS detectors
We report quantum efficiency measurements of back-illuminated, ion-implanted, laser-annealed charge coupled devices (CCD's) in the wavelength range 13-10,000 A. The equivalent quantum efficiency (EQE = effective photons detected per incident photon) ranges from a minimum of 5 percent as 1216 A to a maximum of 87 percent at 135 A. Using a simple relationship for the charge collection efficiency of the CCD pixels as a function of depth, we present a semi-empirical model with few parameters which reproduces our measurements with a fair degree of accuracy. The advantage of this model is that is can be used to predict CCD QE performance for shallow backside implanted devices without detailed solution of a system of differential equations, as in conventional approaches, and yields a simple analytic form for the charge collection efficiency which is adequate for detector calibration purposes. Making detailed assumptions about the dopant profile, we also solve the carrier density and continuity equations in order to relate our semi-empirical model parameters to surface and bulk device properties. The latter procedure helps to better establish device processing parameters for a given level of CCD QE performance.
Stern, Robert A.↗
Fabrication of a Cryogenic Terahertz Emitter for Bolometer Focal Plane Calibrations
A fabrication process is reported for prototype emitters of THz radiation, which operate cryogenically, and should provide a fast, stable blackbody source suitable for characterization of THz devices. The fabrication has been demonstrated and, at the time of this reporting, testing was underway. The emitter is similar to a monolithic silicon bolometer in design, using both a low-noise thermometer and a heater element on a thermally isolated stage. An impedance-matched, high-emissivity coat ing is also integrated to tune the blackbody properties. This emitter is designed to emit a precise amount of power as a blackbody spectrum centered on terahertz frequencies. The emission is a function of the blackbody temperature. An integrated resistive heater and thermometer system can control the temperature of the blackbody with greater precision than previous incarnations of calibration sources that relied on blackbody emission. The emitter is fabricated using a silicon- on-insulator substrate wafer. The buried oxide is chosen to be less than 1 micron thick, and the silicon device thickness is 1-2 microns. Layers of phosphorus compensated with boron are implanted into and diffused throughout the full thickness of the silicon device layer to create the thermometer and heater components. Degenerately doped wiring is implanted to connect the devices to wire-bondable contact pads at the edge of the emitter chip. Then the device is micromachined to remove the thick-handle silicon behind the thermometer and heater components, and to thermally isolate it on a silicon membrane. An impedance- matched emissive coating (ion assisted evaporated Bi) is applied to the back of the membrane to enable high-efficiency emission of the blackbody spectrum.
Chervenak, James↗
Solar Flare Track Exposure Ages in Regolith Particles: A Calibration for Transmission Electron Microscope Measurements
Mineral grains in lunar and asteroidal regolith samples provide a unique record of their interaction with the space environment. Space weathering effects result from multiple processes including: exposure to the solar wind, which results in ion damage and implantation effects that are preserved in the rims of grains (typically the outermost 100 nm); cosmic ray and solar flare activity, which result in track formation; and impact processes that result in the accumulation of vapor-deposited elements, impact melts and adhering grains on particle surfaces. Determining the rate at which these effects accumulate in the grains during their space exposure is critical to studies of the surface evolution of airless bodies. Solar flare energetic particles (mainly Fe-group nuclei) have a penetration depth of a few millimeters and leave a trail of ionization damage in insulating materials that is readily observable by transmission electron microscope (TEM) imaging. The density of solar flare particle tracks is used to infer the length of time an object was at or near the regolith surface (i.e., its exposure age). Track measurements by TEM methods are routine, yet track production rate calibrations have only been determined using chemical etching techniques [e.g., 1, and references therein]. We used focused ion beam-scanning electron microscope (FIB-SEM) sample preparation techniques combined with TEM imaging to determine the track density/exposure age relations for lunar rock 64455. The 64455 sample was used earlier by [2] to determine a track production rate by chemical etching of tracks in anorthite. Here, we show that combined FIB/TEM techniques provide a more accurate determination of a track production rate and also allow us to extend the calibration to solar flare tracks in olivine.
Berger, Eve L.↗
A long-range and long-life telemetry data-acquisition system for heart rate and multiple body temperatures from free-ranging animals
The system includes an implantable transmitter, external receiver-retransmitter collar, and a microprocessor-controlled demodulator. The size of the implant is suitable for animals with body weights of a few kilograms or more; further size reduction of the implant is possible. The ECG is sensed by electrodes designed for internal telemetry and to reduce movement artifacts. The R-wave characteristics are then specifically selected to trigger a short radio frequency pulse. Temperatures are sensed at desired locations by thermistors and then, based on a heartbeat counter, transmitted intermittently via pulse interval modulation. This modulation scheme includes first and last calibration intervals for a reference by ratios with the temperature intervals to achieve good accuracy even over long periods. Pulse duration and pulse sequencing are used to discriminate between heart rate and temperature pulses as well as RF interference.
Lund, G. F.↗
Removal of Biologically Active Organic Contaminants using Atomic Oxygen
Biomedical devices that are to come into contact with living tissue, such as prosthetic and other implants for the human body and the containers used to store and transport them, are together cleaned of non-living, but biologically active organic materials, including endotoxins such as lipopolysaccharides, and assembled into a hermetically sealed package without recontamination. This is achieved by cleaning both the device and package components together in an apparatus, which includes a hermetically sealed chamber, in which they are contacted with atomic oxygen which biocleans them, by oxidizing the biologically active organic materials. The apparatus also includes means for manipulating the device and container and hermetically sealing the cleaned device into the cleaned container to form the package. A calibrated witness coupon visually indicates whether or not the device and container have received enough exposure to the atomic oxygen to have removed the organic materials from their surfaces. Gamma radiation is then used to sterilize the device in the sealed container.
Bruce A Banks↗
Evaluation of dual-tip micromanometers during 21-day implantation in goats
Investigative research efforts using a cardiovascular model required the determination of central circulatory haemodynamic and arterial system parameters for the evaluation of cardiovascular performance. These calculations required continuous beat-to-beat measurement of pressure within the four chambers of the heart and great vessels. Sensitivity and offset drift, longevity, and sources of error for eight 3F dual-tipped micromanometers were determined during 21 days of implantation in goats. Subjects were instrumented with pairs of chronically implanted fluid-filled access catheters in the left and right ventricles, through which dual-tipped (test) micromanometers were chronically inserted and single-tip (standard) micromanometers were acutely inserted. Acutely inserted sensors were calibrated daily and measured pressures were compared in vivo to the chronically inserted sensors. Comparison of the pre- and post-gain calibration of the chronically inserted sensors showed a mean sensitivity drift of 1.0 +/- 0.4% (99% confidence, n = 9 sensors) and mean offset drift of 5.0 +/- 1.5 mmHg (99% confidence, n = 9 sensors). Potential sources of error for these drifts were identified, and included measurement system inaccuracies, temperature drift, hydrostatic column gradients, and dynamic pressure changes. Based upon these findings, we determined that these micromanometers may be chronically inserted in high-pressure chambers for up to 17 days with an acceptable error, but should be limited to acute (hours) insertions in low-pressure applications.
Non-NASA Center↗
Improved quantitation of SIMS depth profile measurements of niobium via sample holder design improvements and characterization of grain orientation effects
The importance of SIMS analyses for “N-doped” impurity alloyed niobium and other surface-alloyed materials continues to increase. A major hurdle is the uncertainty of instrument calibration due to changes in sample height either from sample surface topography or from the sample holder itself. The CAMECA sample holder design allows for many types of samples to be analyzed. However, a drawback is that the holder faceplate can bend, contributing an uncertainty in the relative sensitivity factor (RSF) used to quantify the SIMS results. Here, we describe an improved sample holder having a reinforced faceplate, which prevents deflection and reduces uncertainty. Simulations show that the new design significantly reduces deflection from 10 μm to 5 nm. Sample measurements show a reduction of RSF uncertainty from this source from 4.1% to 0.95%. Grain orientation has long been suspected to affect RSF measurement as well. A bicrystal implant standard, consisting of randomly oriented and [001] grains, was successively rotated 15° between analyses. It was observed that 20% of the analyses performed on the randomly oriented grain exhibited anomalously high RSF values as well as slow sputter rates. These features were associated with the changing grain normal orientation with respect to the primary Cs + beam. The grain orientation associated with the rise in RSF was simulated and determined to be the [101] crystallographic plane, thus indicating that ion channeling was responsible for the significantly increased RSF. Focused ion beam analysis confirmed slower sputter rates for the cardinal crystallographic orientations, indicating that ion channeling occurred for each.
43 PARTICLE ACCELERATORS↗