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DOE OSTI2022

Surface analysis insight note: Synthetic line shapes, integration regions and relative sensitivity factors

Here, methods for estimating photoemission intensity from X-ray photoelectron spectroscopy data are examined. The role played by “synthetic” bell-shaped curves, integration intervals, background curves, and the use of relative sensitivity factors (RSFs) in reporting percentage atomic concentration for a sample is presented. In particular, photoemission lines with differing energy distributions obtained from the NaCl sample surface are used to demonstrate how a comparison of photoemission intensities is dependent on the line shapes, background curves, and appropriate use of RSFs.

42 ENGINEERING↗

DOE OSTI2022

Quantitative XPS of plutonium: Evaluation of the Pu4f peak shape, relative sensitivity factors and estimated detection limits

We report that high-resolution X-ray photoelectron spectra have been acquired from sputter cleaned and in situ oxidized samples of α-plutonium and a face-centred cubic δ-plutonium–gallium alloy. The differences in the Pu4f peak shape in these two materials have been investigated, and the poorly screened satellite peaks have been quantified. Curve fitting parameters for the Pu4p 3/2 , Pu4d 5/2 , Pu4f and Pu6p 3/2 photoelectron peaks are reported, and relative sensitivity factors have been determined. The Pu4f curve fit model has been applied to data acquired using different spectrometers and alloys. Examples of quantification of the plutonium spectra are provided and minimum detection limits are calculated for common impurities in plutonium metal.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Accuracy limitations for composition analysis by XPS using relative peak intensities: LiF as an example

Although precision in XPS can be excellent, allowing small changes to be easily observed, obtaining accurate absolute elemental composition of a solid material from relative peak intensities is generally much more problematical, involving many factors: background removal; differing analysis depths at different photoelectron kinetic energies; possible angular distribution effects; calibration of the instrument transmission function, and variations of the distribution of the photoelectron intensity between “main” peaks (those usually used for analysis) and associated substructure following the main peak, as a function of the chemical bonding of the elements concerned. The last item, coupled with the use of photoionization cross-sections and/or relative sensitivity factors, is the major subject of this paper, though it is necessary to consider the other items also, using LiF as a test case. The results show that the above issues, which are relevant to differing degrees in most XPS analyses, present significant challenges to highly accurate XPS quantification.

Brundle, Christopher R.↗

DOE OSTI2024

Composition Quantification of SiGeSn Alloys Through Time-of-Flight Secondary Ion Mass Spectrometry: Calibration Methodologies and Validation With Atom Probe Tomography

Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS) is a powerful technique for elemental compositional analysis and depth profiling of materials. However, it encounters the problem of matrix effects that hinder its application. In this work, we introduce a pioneering ToF-SIMS calibration method tailored for SixGeySnz ternary alloys. SixGe1-x and Ge1-zSnz binary alloys with known compositions are used as calibration reference samples. Through a systematic SIMS quantification study of SiGe and GeSn binary alloys, we unveil a linear correlation between secondary ion intensity ratio and composition ratio for both SiGe and GeSn binary alloys, effectively mitigating the matrix effects. Extracted relative sensitivity factor (RSF) value from SixGe1-x (0.07 < x < 0.83) and Ge1-zSnz (0.066 < z < 0.183) binary alloys are subsequently applied to those of SixGeySnz (0.011 < x < 0.113, 0.863 < y < 0.935 and 0.023 < z < 0.103) ternary alloys for elemental compositions quantification. These values are cross-checked by Atom Probe Tomography (APT) analysis, an indication of the great accuracy and reliability of as-developed ToF-SIMS calibration process. Furthermore, the proposed method and its reference sample selection strategy in this work provide a low-cost as well as simple-to-follow calibration route for SiGeSn composition analysis, thus driving the development of next-generation multifunctional SiGeSn-related semiconductor devices.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Preliminary Insights Into the Feasibility of Determining the Purification Date of Enriched Uranium by Direct Measurement of the 230 Th/ 234 U Ratio Using an All-Faraday Detector Configuration on the Neoma MC-ICP-MS

Rationale: Mass spectrometric measurement of the 230 Th/ 234 U ratio to calculate the purification age of enriched uranium is typically conducted via a combination of ion counters and faraday detectors, thus requiring an inter-detector calibration scheme. Here, our aim is to understand whether the pursuit of a simplified measurement scheme involving only faraday detectors is feasible. Methods: We investigate the possibility of determining U-Th model ages for two enriched uranium standards (NBL U630 and U850) by direct measurement of the 230 Th/ 234 U ratio (without chromatographic separation or isotope dilution) on a ThermoFisher Scientific Neoma MC-ICP-MS utilizing both solution and laser ablation (LA)-based sampling techniques and an all-faraday detector configuration. Results: For the solution mode analyses conducted on aliquots containing sub μg/mL total U, we produce composite average 230 Th/ 234 U model dates of May 19, 1988 (± 351 days), and March 26, 1961 (± 2.5 years) using the directly measured 230 Th/ 234 U ratios for the NBL U630 and U850 uranium standards, which have certified purification dates of June 6, 1988 (± 190 days), and December 31, 1957 (± 36.5 days), respectively. The ages produced by LA-based sampling of dried residues of the same standards deposited onto cotton TexWipes are less accurate and of poorer precision (June 23, 2004 ± 8.7 years for U630 and December 21, 1965 ± 7.9 years for U850) but still yield meaningful information in regards to the purification date. Conclusions: We believe that further refinement of the all faraday detector measurement approach to include development of a more robust Th/U relative sensitivity factor determination, signal cutoff selection, and data processing protocols will allow for this approach to be confidently applied to enriched uranium materials with unknown purification histories. Potential advantages of the method include the reduced sample handling and infrastructure requirements as well as the ability to simultaneously generate a broad picture of the uranium isotopic composition in tandem with the U-Th age determination.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Advances in secondary ion mass spectrometry for N-doped niobium

Accurate secondary ion mass spectroscopy measurement of nitrogen in niobium relies on the use of closely equivalent standards, made by ion implantation, to convert nitrogen signal intensity to nitrogen content by determination of relative sensitivity factors (RSFs). Accurate RSF values for ppm-range nitrogen contents are increasingly critical, as more precision is sought in processes for next-generation superconducting radiofrequency (SRF) accelerator cavities. Furthermore, factors influencing RSF value measurements were investigated with the aim of reliably attaining better than 10% accuracy in nitrogen concentrations at various depths into the bulk. This has been accomplished for materials typical of SRF cavities at the cost of increased attention to all aspects.

47 OTHER INSTRUMENTATION↗

DOE OSTI2022

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↗

DOE OSTI2025

Understanding the Quadrupole Mass Filter and Testing a High-Resolution QMS RGA for ITER

A common type of residual gas analyzer is the quadrupole mass spectrometer. One of the main components within this instrument is a mass filter known as the quadrupole. It is responsible for the selective throughput of the ionized gas particles - by ascending mass number - prior to ion impacts on the analyzer (or detector) surface from which the ion current signal is generated for processing. However, the quadrupole is not fully described in relation to the electric field characteristics and the function as an ion mass separator. This paper describes the basic origins of the electrical design, the intricate assembly criteria, and performance of the quadrupole within the spectrometer. A specialized quadrupole mass spectrometer is part of a configuration for a diagnostic gas analyzer system planned for ITER, a fusion research machine. It has a verified capability, essential as a diagnostic criterion for this reactor project, to successfully deconvolute the mass signals of Helium-4 and deuterium (reactor fuel exhaust gases, separated by only 0.026 atomic mass units), down to a relative three-percent concentration of the former gas. The associated preliminary testing, performed at the Oak Ridge National Laboratory, is also addressed. Finally, one of the key parameters used to express gas concentration, the relative sensitivity factor, will be explained, including an evaluation of dependency on other variables.

Marcus, Chris [ORNL] (ORCID:0000000190139636)↗

NASA NTRS1974

Neutral winds and electric fields from model studies using reduced ionograms

A relationship between the vertical component of the ion velocity and electron density profiles derived from reduced ionograms is developed. Methods for determining the horizontal components of the neutral winds and electric fields by using this relationship and making use of the variations of the inclinations and declinations of the earth's magnetic field are presented. The effects that electric fields have on the neutral wind calculations are estimated to be small but not second order. Seasonal and latitudinal variations of the calculated neutral winds are presented. From the calculated neutral winds a new set of neutral pressure gradients is determined. The new pressure gradients are compared with those generated from several static neutral atmospheric models. Sensitivity factors relating the pressure gradients and neutral winds are calculated and these indicate that mode coupling and harmonic generation are important to studies which assume linearized theories.

Baran, D. E.↗

NASA NTRS1995

Sputtering erosion in ion and plasma thrusters

An experimental set-up to measure low-energy (below 1 keV) sputtering of materials is described. The materials to be bombarded represent ion thruster components as well as insulators used in the stationary plasma thruster. The sputtering takes place in a 9 inch diameter spherical vacuum chamber. Ions of argon, krypton and xenon are used to bombard the target materials. The sputtered neutral atoms are detected by a secondary neutral mass spectrometer (SNMS). Samples of copper, nickel, aluminum, silver and molybdenum are being sputtered initially to calibrate the spectrometer. The base pressure of the chamber is approximately 2 x 10(exp -9) Torr. the primary ion beam is generated by an ion gun which is capable of delivering ion currents in the range of 20 to 500 nA. The ion beam can be focused to a size approximately 1 mm in diameter. The mass spectrometer is positioned 10 mm from the target and at 90 deg angle to the primary ion beam direction. The ion beam impinges on the target at 45 deg. For sputtering of insulators, charge neutralization is performed by flooding the sample with electrons generated from an electron gun. Preliminary sputtering results, methods of calculating the instrument response function of the spectrometer and the relative sensitivity factors of the sputtered elements will be discussed.

Ray, Pradosh K.↗

NASA NTRS2009

Rare Earth Element Measurements of Melilite and Fassaite in Allende Cai by Nanosims

The rare earth elements (REEs) are concentrated in CAIs by approx. 20 times the chondritic average [e.g., 1]. The REEs in CAIs are important to understand processes of CAI formation including the role of volatilization, condensation, and fractional crystallization [1,2]. REE measurements are a well established application of ion microprobes [e.g., 3]. However the spatial resolution of REE measurements by ion microprobe (approx.20 m) is not adequate to resolve heterogeneous distributions of REEs among/within minerals. We have developed methods for measuring REE with the NanoSIMS 50L at smaller spatial scales. Here we present our initial measurements of REEs in melilite and fassaite in an Allende Type-A CAI with the JSC NanoSIMS 50L. We found that the key parameters for accurate REE abundance measurements differ between the NanoSIMS and conventional SIMS, in particular the oxide-to-element ratios, the relative sensitivity factors, the energy distributions, and requisite energy offset. Our REE abundance measurements of the 100 ppm REE diopside glass standards yielded good reproducibility and accuracy, 0.5-2.5 % and 5-25 %, respectively. We determined abundances and spatial distributions of REEs in core and rim within single crystals of fassaite, and adjacent melilite with 5-10 m spatial resolution. The REE abundances in fassaite core and rim are 20-100 times CI abundance but show a large negative Eu anomaly, exhibiting a well-defined Group III pattern. This is consistent with previous work [4]. On the other hand, adjacent melilite shows modified Group II pattern with no strong depletions of Eu and Yb, and no Tm positive anomaly. REE abundances (2-10 x CI) were lower than that of fassaite. These patterns suggest that fassaite crystallized first followed by a crystallization of melilite from the residual melt. In future work, we will carry out a correlated study of O and Mg isotopes and REEs of the CAI in order to better understand the nature and timescales of its formation process and subsequent metamorphic history.

Ito, M.↗

NASA NTRS1975

An experimental investigation of compressor stall using an on-line distortion indicator and signal conditioner

The relation of the steady-state and dynamic distortions and the stall margin of a J85-13 turbojet engine was investigated. A distortion indicator capable of computing two distortion indices was used. A special purpose signal conditioner was also used as an interface between transducer signals and distortion indicator. A good correlation of steady-state distortion and stall margin was established. The prediction of stall by using the indices as instantaneous distortion indicators was not successful. A sensitivity factor that related the loss of stall margin to the turbulence level was found.

Costakis, W. G.↗

NASA NTRS1990

Probabilistic analysis of a materially nonlinear structure

A probabilistic finite element program is used to perform probabilistic analysis of a materially nonlinear structure. The program used in this study is NESSUS (Numerical Evaluation of Stochastic Structure Under Stress), under development at Southwest Research Institute. The cumulative distribution function (CDF) of the radial stress of a thick-walled cylinder under internal pressure is computed and compared with the analytical solution. In addition, sensitivity factors showing the relative importance of the input random variables are calculated. Significant plasticity is present in this problem and has a pronounced effect on the probabilistic results. The random input variables are the material yield stress and internal pressure with Weibull and normal distributions, respectively. The results verify the ability of NESSUS to compute the CDF and sensitivity factors of a materially nonlinear structure. In addition, the ability of the Advanced Mean Value (AMV) procedure to assess the probabilistic behavior of structures which exhibit a highly nonlinear response is shown. Thus, the AMV procedure can be applied with confidence to other structures which exhibit nonlinear behavior.

Millwater, H. R.↗

NASA NTRS2010

Utilizing In Situ Directional Hyperspectral Measurements to Validate Bio-Indicator Simulations for a Corn Crop Canopy

Two radiative transfer canopy models, SAIL and the two-layer Markov-Chain Canopy Reflectance Model (MCRM), were coupled with in situ leaf optical properties to simulate canopy-level spectral band ratio vegetation indices with the focus on the photochemical reflectance index in a cornfield. In situ hyperspectral measurements were made at both leaf and canopy levels. Leaf optical properties were obtained from both sunlit and shaded leaves. Canopy reflectance was acquired for eight different relative azimuth angles (psi) at three different view zenith angles (Theta (sub v)), and later used to validate model outputs. Field observations of photochemical reflectance index (PRI) for sunlit leaves exhibited lower values than shaded leaves, indicating higher light stress. Canopy PRI expressed obvious sensitivity to viewing geometry, as a function of both Theta (sub v) and psi . Overall, simulations from MCRM exhibited better agreements with in situ values than SAIL. When using only sunlit leaves as input, the MCRM-simulated PRI values showed satisfactory correlation and RMSE, as compared to in situ values. However, the performance of the MCRM model was significantly improved after defining a lower canopy layer comprised of shaded leaves beneath the upper sunlit leaf layer. Four other widely used band ratio vegetation indices were also studied and compared with the PRI results. MCRM simulations were able to generate satisfactory simulations for these other four indices when using only sunlit leaves as input; but unlike PRI, adding shaded leaves did not improve the performance of MCRM. These results support the hypothesis that the PRI is sensitive to physiological dynamics while the others detect static factors related to canopy structure. Sensitivity analysis was performed on MCRM in order to better understand the effects of structure related parameters on the PRI simulations. Leaf area index (LAI) showed the most significant impact on MCRM-simulated PRI among the parameters studied. This research shows the importance of hyperspectral and narrow band sensor studies, and especially the necessity of including the green wavelengths (e.g., 531 nm) on satellites proposing to monitor carbon dynamics of terrestrial ecosystems.

Cheng, Yen-Ben↗

NASA NTRS1994

Optimization of Adaptive Intraply Hybrid Fiber Composites with Reliability Considerations

The reliability with bounded distribution parameters (mean, standard deviation) was maximized and the reliability-based cost was minimized for adaptive intra-ply hybrid fiber composites by using a probabilistic method. The probabilistic method accounts for all naturally occurring uncertainties including those in constituent material properties, fabrication variables, structure geometry, and control-related parameters. Probabilistic sensitivity factors were computed and used in the optimization procedures. For actuated change in the angle of attack of an airfoil-like composite shell structure with an adaptive torque plate, the reliability was maximized to 0.9999 probability, with constraints on the mean and standard deviation of the actuation material volume ratio (percentage of actuation composite material in a ply) and the actuation strain coefficient. The reliability-based cost was minimized for an airfoil-like composite shell structure with an adaptive skin and a mean actuation material volume ratio as the design parameter. At a O.9-mean actuation material volume ratio, the minimum cost was obtained.

Shiao, Michael C.↗

NASA NTRS1995

A Probabilistic Design Method Applied to Smart Composite Structures

A probabilistic design method is described and demonstrated using a smart composite wing. Probabilistic structural design incorporates naturally occurring uncertainties including those in constituent (fiber/matrix) material properties, fabrication variables, structure geometry and control-related parameters. Probabilistic sensitivity factors are computed to identify those parameters that have a great influence on a specific structural reliability. Two performance criteria are used to demonstrate this design methodology. The first criterion requires that the actuated angle at the wing tip be bounded by upper and lower limits at a specified reliability. The second criterion requires that the probability of ply damage due to random impact load be smaller than an assigned value. When the relationship between reliability improvement and the sensitivity factors is assessed, the results show that a reduction in the scatter of the random variable with the largest sensitivity factor (absolute value) provides the lowest failure probability. An increase in the mean of the random variable with a negative sensitivity factor will reduce the failure probability. Therefore, the design can be improved by controlling or selecting distribution parameters associated with random variables. This can be implemented during the manufacturing process to obtain maximum benefit with minimum alterations.

Shiao, Michael C.↗

NASA NTRS2006

Assisting Public Organizations in Their Outsourcing Endeavors: A Decision Support Mode

There has been a tremendous growth in outsourcing practices in recent years. The public organizations in the United States have outsourced some functions and are now being compelled to outsource additional ones. While there are numerous studies that document and analyze outsourcing practices, there is limited research to guide public or governmental organizations in determining what functions to outsource. This study fills this gap by developing a decision support model for a typical public organization in determining what to outsource and how. A set of outsourcing decision factors is identified that can be used as parameters in the three integer programming formulations developed. These formulations are used as solution engines in the model. The first formulation identifies which functions are the best candidates for outsourcing given the organization's priorities. The other formulations place the functions into recommended contracts and re-assign displaced employees. Data from NASA Glenn Research Center in Ohio is used to test and analyze the model. Analysis indicates that cost and skills-related factors are the most sensitive parameters for the data tested. The model and the formulations are a relatively comprehensive package and may help guide outsourcing decisionmakers and policymakers in public organizations.

Kremic, TIbor↗

NASA NTRS1989

Ozone trends in Atlanta, Georgia - Have emission controls been effective?

Nine years of summertime ozone data from the Atlanta metropolitan area are analyzed and compared to local emissions of volatile organic carbon and nitrogen oxides. Trends from 1979 to 1987 were studied for the number of days per year ozone exceeded the NAAQS standard, the second-highest ozone level observed per year, and the first quartile summertime average ozone observed, as well as the mean difference between the ozone level observed downwind and upwind of the city. Because this last parameter is sensitive to chemical factors but relatively insensitive to the number of days each year with meteorological conditions conducive to ozone formation, its trend may be best suited for determining how effective emission controls have been in reducing O3 in the Atlanta area. In spite of the fact that sizeable reductions have been claimed for volatile organic carbon emissions over the past several years, the data give no indication that ozone levels have decreased and in fact, imply that summertime ozone production may have increased. The results imply that either emissions have not decreased as much as has been claimed or that ozone is not sensitive to anthropogenic volatile organic carbon emissions.

Lindsay, Ronald W.↗