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DOE OSTI2022

Using Xe Plasma FIB for High-Quality TEM Sample Preparation

Here, a direct comparison between electron transparent transmission electron microscope (TEM) samples prepared with gallium (Ga) and xenon (Xe) focused ion beams (FIBs) is performed to determine if equivalent quality samples can be prepared with both ion species. We prepared samples using Ga FIB and Xe plasma focused ion beam (PFIB) while altering a variety of different deposition and milling parameters. The samples’ final thicknesses were evaluated using STEM-EELS $\textit{t/λ}$ data. Using the Ga FIB sample as a standard, we compared the Xe PFIB samples to the standard and to each other. We show that although the Xe PFIB sample preparation technique is quite different from the Ga FIB technique, it is possible to produce high-quality, large area TEM samples with Xe PFIB. We also describe best practices for a Xe PFIB TEM sample preparation workflow to enable consistent success for any thoughtful FIB operator. For Xe PFIB, we show that a decision must be made between the ultimate sample thickness and the size of the electron transparent region.

47 OTHER INSTRUMENTATION↗

NASA NTRS1994

Directional radiance measurements: Challenges in the sampling of landscapes

Most earth surfaces, particularly those supporting natural vegetation ecosystems, constitute structurally and spectrally complex surfaces that are distinctly non-Lambertian reflectors. Obtaining meaningful measurements of the directional radiances of landscapes and obtaining estimates of the complete bidirectional reflectance distribution functions of ground targets with complex and variable landscape and radiometric features are challenging tasks. Reasons for the increased interest in directional radiance measurements are presented, and the issues that must be addressed when trying to acquire directional radiances for vegetated land surfaces from different types of remote sensing platforms are discussed. Priority research emphases are suggested, concerning field measurements of directional surface radiances and reflectances for future research. Primarily, emphasis must be given to the acquisition of more complete and directly associated radiometric and biometric parameter data sets that will empower the exploitation of the 'angular dimension' in remote sensing of vegetation through enabling the further development and rigorous validation of state of the art plant canopy models.

Deering, D. W.↗

NASA NTRS1977

A high pressure modulated molecular beam mass spectrometric sampling system

The current state of understanding of free-jet high pressure sampling is critically reviewed and modifications of certain theoretical and empirical considerations are presented. A high pressure, free-jet expansion, modulated molecular beam, mass spectrometric sampling apparatus was constructed and this apparatus is described in detail. Experimental studies have demonstrated that the apparatus can be used to sample high temperature systems at pressures up to one atmosphere. Condensible high temperature gaseous species have been routinely sampled and the mass spectrometric detector has provided direct identification of sampled species. System sensitivity is better than one tenth of a part per million. Experimental results obtained with argon and nitrogen beams are presented and compared to theoretical predictions. These results and the respective comparison are taken to indicate acceptable performance of the sampling apparatus. Results are also given for two groups of experiments related to hot corrosion studies. The formation of gaseous sodium sulfate in doped methane-oxygen flames was characterized and the oxidative vaporization of metals was studied in an atmospheric pressure flowing gas system to which gaseous salt partial pressures were added.

Stearns, C. A.↗

NASA NTRS2009

Geolab 2010: Desert Rats Field Demonstration

In 2010, Desert Research and Technology Studies (Desert RATS), NASA's annual field exercise designed to test spacesuit and rover technologies, will include a first generation lunar habitat facility, the Habitat Demonstration Unit (HDU). The habitat will participate in joint operations in northern Arizona with the Lunar Electric Rover (LER) and will be used as a multi-use laboratory and working space. A Geology Laboratory or GeoLab is included in the HDU design. Historically, science participation in Desert RATS exercises has supported the technology demonstrations with geological traverse activities that are consistent with preliminary concepts for lunar surface science Extravehicular Activities (EVAs). Next year s HDU demonstration is a starting point to guide the development of requirements for the Lunar Surface Systems Program and test initial operational concepts for an early lunar excursion habitat that would follow geological traverses along with the LER. For the GeoLab, these objectives are specifically applied to support future geological surface science activities. The goal of our GeoLab is to enhance geological science returns with the infrastructure that supports preliminary examination, early analytical characterization of key samples, and high-grading lunar samples for return to Earth [1, 2] . Figure 1: Inside view schematic of the GeoLab a 1/8 section of the HDU, including a glovebox for handling and examining geological samples. Other outfitting facilities are not depicted in this figure. GeoLab Description: The centerpiece of the GeoLab is a glovebox, allowing for samples to be brought into the habitat in a protected environment for preliminary examination (see Fig. 1). The glovebox will be attached to the habitat bulkhead and contain three sample pass-through antechambers that would allow direct transfer of samples from outside the HDU to inside the glovebox. We will evaluate the need for redundant chambers, and other uses for the glovebox antechambers, such as a staging area for additional tools or samples. The sides of the glovebox are designed with instrument ports and additional smaller ports for cable pass-through, imagery feeds and environmental monitoring. This first glovebox version will be equipped with basic tools for manipulating, viewing, and early analysis of samples. The GeoLab was also designed for testing additional analytical instruments in a field setting.

Evans, Cindy A.↗

NASA NTRS2012

Coherent Detector for Near-Angle Scattering and Polarization Characterization of Telescope Mirror Coatings

A report discusses the difficulty of measuring scattering properties of coated mirrors extremely close to the specular reflection peak. A prototype Optical Hetero dyne Near-angle Scatterometer (OHNS) was developed. Light from a long-coherence-length (>150 m) 532-nm laser is split into two arms. Acousto-optic modulators frequency shift the sample and reference beams, establishing a fixed beat frequency between the beams. The sample beam is directed at very high f/# onto a mirror sample, and the point spread function (PSF) formed after the mirror sample is scanned with a pinhole. This light is recombined by a non-polarizing beam splitter and measured through heterodyne detection with a spectrum analyzer. Polarizers control the illuminated and analyzed polarization states, allowing the polarization dependent scatter to be measured. The bidirectional reflective or scattering distribution function is normally measured through use of a scattering goniometer instrument. The instrumental beam width (collection angle span) over which the scatterometer responds is typically many degrees. The OHNS enables measurement at angles as small as the first Airy disk diameter.

Macenka, Steven A.↗

NASA NTRS2014

Rapid Electrochemical Detection and Identification of Microbiological and Chemical Contaminants for Manned Spaceflight Project

Microbial control in the spacecraft environment is a daunting task, especially in the presence of human crew members. Currently, assessing the potential crew health risk associated with a microbial contamination event requires return of representative environmental samples that are analyzed in a ground-based laboratory. It is therefore not currently possible to quickly identify microbes during spaceflight. This project addresses the unmet need for spaceflight-compatible microbial identification technology. The electrochemical detection and identification platform is expected to provide a sensitive, specific, and rapid sample-to-answer capability for in-flight microbial monitoring that can distinguish between related microorganisms (pathogens and non-pathogens) as well as chemical contaminants. This will dramatically enhance our ability to monitor the spacecraft environment and the health risk to the crew. Further, the project is expected to eliminate the need for sample return while significantly reducing crew time required for detection of multiple targets. Initial work will focus on the optimization of bacterial detection and identification. The platform is designed to release nucleic acids (DNA and RNA) from microorganisms without the use of harmful chemicals. Bacterial DNA or RNA is captured by bacteria-specific probe molecules that are bound to a microelectrode, and that capture event can generate a small change in the electrical current (Lam, et al. 2012. Anal. Chem. 84(1): 21-5.). This current is measured, and a determination is made whether a given microbe is present in the sample analyzed. Chemical detection can be accomplished by directly applying a sample to the microelectrode and measuring the resulting current change. This rapid microbial and chemical detection device is designed to be a low-cost, low-power platform anticipated to be operated independently of an external power source, characteristics optimal for manned spaceflight and areas where power and computing resources are scarce.

Pierson, Duane↗

NASA NTRS2008

BRDF of Salt Pan Regolith Samples

Laboratory Bi-directional Reflectance Distribution Function (BRDF) measurements of salt pan regolith samples are presented in this study in an effort to understand the role of spatial and spectral variability of the natural biome. The samples were obtained from Etosha Pan, Namibia (19.20 deg S, 15.93 deg E, alt. 1100 m). It is shown how the BRDF depends on the measurement geometry - incident and scatter angles and on the sample particle sizes. As a demonstration of the application of the results, airborne BRDF measurements acquires with NASA's Cloud Absorption Radiometer (CAR) over the same general site where the regolith samples were collected are compared with the laboratory results. Good agreement between laboratory measured and field measured BRDF is reported.

Georgiev, Georgi T.↗

NASA NTRS2009

Systems and methods for correcting optical reflectance measurements

We disclose measurement systems and methods for measuring analytes in target regions of samples that also include features overlying the target regions. The systems include: (a) a light source; (b) a detection system; (c) a set of at least first, second, and third light ports which transmit light from the light source to a sample and receive and direct light reflected from the sample to the detection system, generating a first set of data including information corresponding to both an internal target within the sample and features overlying the internal target, and a second set of data including information corresponding to features overlying the internal target; and (d) a processor configured to remove information characteristic of the overlying features from the first set of data using the first and second sets of data to produce corrected information representing the internal target.

Yang, Ye↗

NASA NTRS2014

Systems and Methods for Correcting Optical Reflectance Measurements

Yang, Ye↗

DOE OSTI2020

In-Field Alpha Spectrometry to Assess Uranium Enrichment In Uranium Hexafluoride

A new In-Field Alpha Spectrometry (IFAS) system is being developed to allow quick turnaround measurements of uranium enrichment in uranium hexafluoride (UF6) samples. Samples are collected using specially-designed Single-Use Destructive Assay (SUDA) wafers which have an absorptive film of zeolite deposited onto a quartz or metal substrate. The SUDA samples, along with a special holder, are designed to be attached directly to a sampling tap at a gas centrifuge enrichment plant or a uranium conversion facility, allowing gaseous UF6 to come into direct contact with the zeolite. The zeolite absorbs this material and converts it into stable, safe UO2F2 within a few minutes. Once the sample has been collected it is transferred to the IFAS system where a solid-state, silicon alpha spectrometer is used to quantitatively measure the alpha emissions from 234U, 235U, and 238U in the sample. The IFAS system is a small, light-weight device that can be quickly turned on and put into use. The SUDA samples and IFAS hardware are designed so that thin-film spectra are produced, allowing a complete measurement with a final 235U:Utotal determination having a precision <±2% to be made in less than eight hours. This short time frame will allow an inspector to get results on-site within one working shift; further innovations may reduce this to even shorter times.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2020

In-Field Alpha Spectrometry to Assess Uranium Enrichment In Uranium Hexafluoride

A new In-Field Alpha Spectrometry (IFAS) system is being developed to allow quick turnaround measurements of uranium enrichment in uranium hexafluoride samples. Samples are collected using specially-designed Single-Use Destructive Assay (SUDA) wafers which have an absorptive thin film of zeolite deposited onto a quartz substrate. The SUDA samples, along with a special holder, are designed to be attached directly to a sampling tap at a gas centrifuge enrichment plant or a uranium conversion facility, allowing gaseous UF6 to come into direct contact with the zeolite. The zeolite absorbs this material and converts it into stable, safe UO2F2 within a few minutes. Once the sample has been collected it is transferred to the IFAS system where a solid-state, silicon alpha spectrometer is used to quantitatively measure the alpha emissions from 234U, 235U, and 238U form the sample. The SUDA samples are designed so that thin-film spectra are produced, and the SUDA samples and IFAS system are designed so that a complete measurement, with a final 235U:Utotal determination of <±2%, can be made in less than eight hours. This short time frame will allow an inspector to get results on-site within one working shift.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

NASA NTRS1992

Gamma-ray burst locations from the Burst and Transient Source Experiment

The Burst and Transient Source Experiment (BATSE) consists of eight anisotropic gamma-ray spectrometers at the corners of the Compton Gamma Ray Observatory. BATSE monitors the full sky from a fixed orientation and determines the direction of gamma-ray bursts with an accuracy appropriate for studying the bursts' celestial distribution. We describe the calculation of gamma-ray burst directions from measurements made by BATSE. We present a sample of calculated directions from BATSE's measurement of solar flaxes and compare the calculated directions with the solar direction. We describe the systematic errors apparent in these data and discuss ongoing efforts to correct them.

Brock, M. N.↗

DOE OSTI2022

Time-resolved chemical studies via time-of-flight secondary ion mass spectrometry

A method of performing time-of-flight secondary ion mass spectrometry on a sample includes the step of directing a beam of primary ions to the sample, and stimulating the migration of ions within the sample while the beam of primary ions is directed at the sample. The stimulation of the ions is cycled between a stimulation state and a lower stimulation state. Secondary ions emitted from the sample by the beam of primary ions are collected in a time-of-flight mass spectrometer. Time-of-flight secondary ion mass spectrometry is then performed on the secondary ions. A system for performing time-of-flight secondary ion mass spectrometry on a sample is also disclosed.

Ievlev, Anton V.↗

DOE OSTI2020

Nanoscale optical tomography with cathodoluminescence spectroscopy

In one aspect, a cathodoluminescence (CL) spectroscopic tomography device includes a sample stage to support a sample. An electron beam source scans an electron beam over the sample to yield light emission by the sample. A reflective element directs the light emission by the sample to a light detector. A controller controls operation of the sample stage, the electron beam source, and the light detector. In one aspect, a CL spectroscopic tomography device includes an electron beam source which directs an electron beam at an object to yield an emission by the object. A detector detects the emission. A controller receives information from the detector related to the detected emission. The controller derives a two-dimensional (2D) CL map from the information related to the detected emission, and derives a three-dimensional (3D) CL tomogram from the 2D CL map.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

NASA NTRS2010

Compact Sensitive Piezoelectric Mass Balance for Measurement of Unconsolidated Materials in Space

In many in-situ instruments information about the mass of the sample could aid in the interpretation of the data and portioning instruments might require an accurate sizing of the sample mass before dispensing the sample. In addition, on potential sample return missions a method to directly assess the captured sample size would be required to determine if the sampler could return or needs to continue attempting to acquire sample. In an effort to meet these requirements piezoelectric balances were developed using flextensional actuators which are capable of monitoring the mass using two methods. A piezoelectric balance could be used to measure mass directly by monitoring the voltage developed across the piezoelectric which is linear with force, or it could be used in resonance to produce a frequency change proportional to the mass change. In this case of the latter, the piezoelectric actuator/balance would be swept in frequency through its fundamental resonance. If a mass is added to the balance the resonance frequency would shift down proportionally to the mass. By monitoring the frequency shift the mass could be determined. This design would allow for two independent measurements of the mass. In microgravity environments spacecraft thrusters could be used to provide acceleration in order to produce the required force for the first technique or to bring the mass into contact with the balance in the second approach. In addition, the measuring actuators, if driven at higher voltages, could be used to fluidize the powder to aid sample movement. In this paper, we outline some of our design considerations and present the results of a few prototype balances that we have developed.

resonance↗

NASA NTRS1979

Sampling for area estimation: A comparison of full-frame sampling with the sample segment approach

The author has identified the following significant results. Full-frame classifications of wheat and non-wheat for eighty counties in Kansas were repetitively sampled to simulate alternative sampling plans. Evaluation of four sampling schemes involving different numbers of samples and different size sampling units shows that the precision of the wheat estimates increased as the segment size decreased and the number of segments was increased. Although the average bias associated with the various sampling schemes was not significantly different, the maximum absolute bias was directly related to sampling size unit.

Hixson, M.↗

NASA NTRS1979

Sampling for area estimation - A comparison of full-frame sampling with the sample segment approach

The objective of this investigation was to evaluate the effect of sampling on the accuracy (precision and bias) of crop area estimates made from classifications of Landsat MSS data. Full-frame classifications of wheat and non-wheat for eighty counties in Kansas were repetitively sampled to simulate alternative sampling plans. Four sampling schemes involving different numbers of samples and different size sampling units were evaluated. The precision of the wheat area estimates increased as the segment size decreased and the number of segments was increased. Although the average bias associated with the various sampling schemes was not significantly different, the maximum absolute bias was directly related to sampling unit size.

Hixson, M. M.↗

NASA NTRS1979

Sampling for area estimation: A comparison of full-frame sampling with the sample segment approach

The effect of sampling on the accuracy (precision and bias) of crop area estimates made from classifications of LANDSAT MSS data was investigated. Full-frame classifications of wheat and non-wheat for eighty counties in Kansas were repetitively sampled to simulate alternative sampling plants. Four sampling schemes involving different numbers of samples and different size sampling units were evaluated. The precision of the wheat area estimates increased as the segment size decreased and the number of segments was increased. Although the average bias associated with the various sampling schemes was not significantly different, the maximum absolute bias was directly related to sampling unit size.

Hixson, M. M.↗