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At least 37 records · Page 2

Analysis of Off-Gas Streams from Small- and Large-Scale Sparging Salt Vessels using Laser-Induced Breakdown Spectroscopy

Laser-induced breakdown spectroscopy (LIBS) is being developed as an analytical monitoring tool for molten salt reactor (MSR) systems. A mobile LIBS platform was configured on a small-scale salt vessel (~100 g of salt) and then transported 0.6 km to successfully monitor an engineering-scale pumped salt loop (~100 kg of salt). Several studies on monitoring salt aerosols, hydrogen isotopes, and noble gases were performed on the small-scale system. All these studies were then implemented for monitoring various tests on the engineering-scale loop. Aerosolized salts from both the storage tank and pump bowl were monitored using LIBS to assess bulk salt analyte ratios (Mg, Na, K) and evaluate impurities (H, O, Ca). In addition to monitoring salt aerosols, LIBS was used in tandem with a residual gas analyzer (RGA) and a Raman spectroscopy system to detect hydrogen isotopes as they were sparged through and subsequently depleted from the loop storage tank. Lastly, a similar test with noble gases (100 ppm Kr, 1000 ppm Xe) was performed, in which LIBS demonstrated a faster response than the RGA used in-line. The tests and results are summarized in this report with detailed publications to follow. Key takeaways are listed in the conclusion of the report.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Reduced gravity multibody dynamics testing

The Final Report on reduced gravity multibody dynamics testing is presented. Tests were conducted on board the NASA KC-135 RGA in Houston, Texas. The objective was to analyze the effects of large angle rotations on flexible, multi-segmented structures. The flight experiment was conducted to provide data which will be compared to the data gathered from ground tests of the same configurations. The flight and ground tested data will be used to validate the TREETOPS software, software which models dynamic multibody systems, and other multibody codes. The flight experiment consisted of seven complete flights on board the KC-135 RGA during two one-week periods. The first period of testing was 4-9 Apr. 1993. The second period of testing was 13-18 Jun. 1993.

Sillanpaa, Meija↗

Apparatus Measures Permeation Of Gases Through Coupons

Apparatus measures permeation of any variety of commercially available pure or mixed gases through polymeric or other material coupons of various thicknesses. Permeability measured at wide range of temperatures and pressures. Includes residual-gas-analyzer (RGA) sensor head and associated circuitry, and vacuum system. Also includes manifold with valves, through which gas of interest allowed to permeate through test coupon before traveling downstream to evacuated RGA sensor head. Temperature of test coupon monitored by thermocouple and maintained at specified value above ambient by use of electrical heating mantle or below ambient by use of bath of ethylene glycol, water, and dry ice.

Adam, Steven J.↗

The Development of a CO2 Test Capability in the NASA JSC ARCJet for Mars Reentry Simulation

The Atmospheric Reentry Materials and Structures Evaluation Facility (ARMSEF) located at NASA Johnson Space Center is used for simulating the extreme environment experienced upon reentry for the development and certification of thermal protection systems (TPS). The facility supports a large variety of programs and was heavily leveraged for the certification and operational support of the TPS for the Orbiter and, more recently, the development of the heat shield for CEV. This paper will provide more detail into the heritage of the facility. Unique attributes of the facility include a modular aerodynamically stabilized arc heater and independently controlled O2 and N2 for the test gases. When combining the O2 and N2 in a 23:77 mass ratio respectively the Earth s atmosphere is accurately simulated and via modification of this ratio the investigation of the effects of atomic oxygen on a material s response is possible. In the summer of 2010 a development effort was started to add CO2 as a third independently controlled test gas such that, when combined with N2, opens up the possibility of accurately simulating a Martian reentry environment. This paper will discuss the test facility, especially the arc heater, in more detail. Initial testing involved relatively low concentrations of CO2 combined with N2 for the primary purpose of gathering data to answer two pressing safety concerns. The first being the rate of production of carbon monoxide (CO) within the ejector vacuum system. The main concern was that CO can be flammable and possibly explosive at high enough concentrations and pressures. The hazard control during the development phase involved the use of injecting N2 inside the test chamber diffuser to dilute and reduce the concentration of any and all CO present. A residual gas analyzer (RGA) was used to determine the relative amount of CO in the exhaust gas and provide a conversion rate of CO2 to CO. This paper will discuss in more detail the results of the RGA data and the calculated conversion rate. The second safety concern addressed is the possible formation of hydrogen cyanide (HCN) and cyanide (CN). HCN would primarily be present in the cooling water while the CN would most probably condense onto the interior surfaces of the test chamber. Water samples and wipes of the test chamber surfaces were analyzed by an industrial hygienist for the presence of HCN and CN. His paper will discuss these results in more detail. Throughout this development effort measurements of the CO2:N2 flowfield were made with heat flux and pressure probes and with laser induced fluorescence (LIF) of the atomic oxygen. This paper will discuss these results

DelPapa, Steven V.↗

Analytical and Experimental Studies of Leak Location and Environment Characterization for the International Space Station

The International Space Station program is developing a robotically-operated leak locator tool to be used externally. The tool would consist of a Residual Gas Analyzer for partial pressure measurements and a full range pressure gauge for total pressure measurements. The primary application is to detect NH3 coolant leaks in the ISS thermal control system.An analytical model of leak plume physics is presented that can account for effusive flow as well as plumes produced by sonic orifices and thruster operations. This model is used along with knowledge of typical RGA and full range gauge performance to analyze the expected instrument sensitivity to ISS leaks of various sizes and relative locations (directionality).The paper also presents experimental results of leak simulation testing in a large thermal vacuum chamber at NASA Goddard Space Flight Center. This test characterized instrument sensitivity as a function of leak rates ranging from 1 lbmyr. to about 1 lbmday. This data may represent the first measurements collected by an RGA or ion gauge system monitoring off-axis point sources as a function of location and orientation. Test results are compared to the analytical model and used to propose strategies for on-orbit leak location and environment characterization using the proposed instrument while taking into account local ISS conditions and the effects of ramwake flows and structural shadowing within low Earth orbit.

Leak Locator↗

Analytical and Experimental Studies of Leak Location and Environment Characterization for the International Space Station

The International Space Station program is developing a robotically-operated leak locator tool to be used externally. The tool would consist of a Residual Gas Analyzer for partial pressure measurements and a full range pressure gauge for total pressure measurements. The primary application is to detect NH3 coolant leaks in the ISS thermal control system. An analytical model of leak plume physics is presented that can account for effusive flow as well as plumes produced by sonic orifices and thruster operations. This model is used along with knowledge of typical RGA and full range gauge performance to analyze the expected instrument sensitivity to ISS leaks of various sizes and relative locations ("directionality"). The paper also presents experimental results of leak simulation testing in a large thermal vacuum chamber at NASA Goddard Space Flight Center. This test characterized instrument sensitivity as a function of leak rates ranging from 1 lb-mass/yr. to about 1 lb-mass/day. This data may represent the first measurements collected by an RGA or ion gauge system monitoring off-axis point sources as a function of location and orientation. Test results are compared to the analytical model and used to propose strategies for on-orbit leak location and environment characterization using the proposed instrument while taking into account local ISS conditions and the effects of ram/wake flows and structural shadowing within low Earth orbit.

000000↗

In-Situ Reaction Monitoring for Lunar Applications Utilizing a Single Quadrupole Residual Gas Analyzer

With a revived focus to create a permeant presence on the moon and in preparation for future Mars exploration, it is imperative that all re-sources are utilized to their fullest potential. In-Situ Resource Utilization (ISRU) will be critical for future mission success as it would enable independent operation of missions while minimally relying on the complex supply chain created between the Earth, moon and Mars. One of the most critical resources that have been identified for ISRU is the creation of liquid oxygen (O2) for not only breathable air, but also for rocket fuel. On the moon and potentially Mars, one of the most O2 rich resources is in the presence of regolith. Although there are numerous minerals within regolith and various processes to extract O2, this is not the scope of this paper. Since the O2 extraction method can vary, a critical standardized analytical method is needed to verify O2 (or oxygenated precursor compounds) for extraction efficiency and purity. Our group utilizes a modified consumer off-the-shelf (COTS), Residual Gas Analyzer (RGA) Single Quadrupole Mass Spectrometer (QMS). Due to the current field mission requirements, the gas analysis module will need to rely only on mass-to-charge ratios (m/z) and peak intensities to differentiate and quantitate targeted gas-phase reactants or products, i.e. carbon monoxide (CO), carbon dioxide (CO2), methane (CH4) and hydrogen (H2). However, due to solar wind implanted volatiles and various other compounds present in lunar regolith, such as nitrogen (N2), helium (He), and deuterium (D2), deconvolution and quantification of isobaric compounds becomes quite difficult. Specifically, the presence of N2 makes quantification of CO, an oxygenated precursor, difficult due to both compounds having a peak at m/z 28. Approaches to differentiate isobaric components: Initially, the solution to overcome isobaric overlap was to use isotopic ratios, particularly be-tween carbon-13 and nitrogen-15. Although limited literature discuss isotopic composition and attempt to quantify the ratios, variation is particularly high and limited to a few lunar regolith samples. The following were identified as potential approaches to quantify isobaric species, N2 and CO, using our RGA. Threshold Ionization. CO and N2 both have peaks at m/z 28, but only N2 is capable of producing a peak at m/z 7. While a N2 peak at m/z 7 is generally rare, instrument parameters can be optimized in order to maximize the peak intensity. Typically a standard ionization energy of 70 eV is used to monitor a batch process and would produce reliable results for a majority of the reactants or products that we are interested in quantifying. However, to analyze the rare molecular fragment of N2 (N2+ at m/z 7), a different ionization energy may be beneficial. Threshold Ionization Mass Spectrometry (TIMS) will be explored to optimize the N2+ peak at m/z 7 by varying parameters such as ionization energy and pressure. Therefore, a quantitative value at m/z 7 will be used to determine the product gas concentration of N2, which will be subtracted from the total concentration determined at m/z 28 enabling us to approximate the amount of CO. Secondary Detector (infrared gas detector, IR). Another approach to quantitate and differentiate be-tween isobaric components is to leverage alternative modes of detection. Unlike mass spectrometry, which generally uses a separation step prior to analysis (i.e. gas chromatography), IR produces energy that is specifically absorbed depending on the bond and configuration of the molecule. This technique could be leveraged since it is generally only active on non-symmetric molecules, i.e. CO. Utilizing concentrations of CO determined from another detector could help correct concentrations of CO obtained from the QMS. However, the inclusion of another detector adds additional mission requirements, such as power, software changes and avionics updates that add additional cost and schedule requirements.

mass spectrometry↗

In-situ Nanoscale Ablation

An understanding of the ablation of carbon-based materials is crucial to modeling the behavior of atmospheric entry spacecrafts equipped with thermal protection systems (TPS).Carbon is the backbone of TPS systems such as PICA (phenolic-impregnated carbon ablator).Therefore in the present work we study ablation of highly oriented pyrolytic graphite (HOPG)in oxygen at temperatures up to 1000°C done within a gas reaction cell housed in a scanning transmission electron microscope (STEM). Observation of the HOPG oxidation on specimens sectioned parallel and normal to the carbon basal planes in the presence of oxygen are reported.Pitting caused by residual oxygen and/or platinum particles from the sectioning process was observed before oxygen gas flow was established at 750°C in the specimen sectioned with the carbon basal planes parallel to the beam direction. Introduction of oxygen flow caused rapid oxidation moving in a uniform front that completely consumed the HOPG in approximately 1.5minutes. The specimen sectioned with the carbon basal planes normal to the beam direction did not show the same pitting phenomenon but exhibited rapid oxidation at 1000°C that proceeded in a uniform front and completed in approximately 1 minute. All specimens tested had a husk resembling the original specimen shape left over after oxidation. It is concluded that this husk is most likely ash impurity from the HOPG or impurities from the sectioning process or E-chip. A residual gas analyszer (RGA) was successfully used to monitor gas flows during the experiments but was yet unsuccessful in monitoring oxidation gas products produced during the experiment.Future studies will optimize the RGA setup in order to maximize the potential for detecting these species. These in-situ studies successfully show how this highly ordered carbon ablates on a nano- and micro-scopic length scale and can be used to provide fundamental understanding of carbon ablation that can be used to design the next-generation of TPS systems.

Nanoscale Ablation↗

Bakeout Workshop

Spacecraft hardware thermal vacuum exposures and bakeouts have been used for years to reduce molecular outgassing to limit contamination to critical optics and sensors on-ground and in orbit. This presentation will discuss lessons learned and vacuum procedural techniques to make the most of your vacuum time. Quartz Crystal Microbalances (QCMs) and Residue Gas Analyzers (RGA) are 2 devices that help track molecular outgassing and examples will be shown on how to use them for your analytical benefit.

Outgassing thermal vacuum QCM RGA↗

Ionic Liquid Sheath Stabilizes Atomically Dispersed Reduced Graphene Aerogel‐Supported Iridium Complexes during Ethylene Hydrogenation Catalysis

Abstract An atomically dispersed reduced graphene aerogel (rGA)‐supported iridium catalyst having reactive ethylene ligands was synthesized at an iridium loading of 9.9 wt % and coated with an ionic liquid, 1‐ethyl‐3‐methylimidazolium acetate ([EMIM][OAc]). Continuous‐scan X‐ray absorption spectra demonstrated that the iridium remained site‐isolated in flowing equimolar C 2 H 4 and H 2 during a temperature ramp to 100 °C. The data further showed the lack of detectable iridium aggregation when the feed was H 2 ‐rich or even pure H 2 at 100 °C. An Arrhenius plot determined for ethylene hydrogenation catalysis with the sample in flowing equimolar ethylene and hydrogen showed no variation in the apparent activation energy at temperatures up to 100 °C, confirming that the active sites remained intact at the higher temperatures. The results point to opportunities for overcoming the stability limitations of atomically dispersed supported noble metal catalysts by choice of electron‐donor supports and ionic liquid sheaths.

Kurtoğlu‐Öztulum, Samira F.↗

Development of an accelerator-based neutron source to prototype Mo-99 production, Part II: A liquid LBE loop under a high vacuum

To provide US domestic supply of Mo-99 without using high-enriched uranium (HEU), a subcritical uranium target assembly (UTA) is irradiated by an accelerator-based neutron source to create Mo-99 through fission. Part I of this work discusses the design of a liquid lead–bismuth eutectic (LBE) windowless target for an accelerator-based neutron source development. Part II discusses how to couple this windowless target to an accelerator operating at an ultra-high vacuum and the subcritical UTA cooled by water at room temperature. Due to the windowless design of the target, the liquid LBE flow shares an ultra-high vacuum (<1.3 × 10 -7 Pa or 10 -9 Torr) space with the accelerator. As a result of this shared vacuum space, the LBE system must operate at a high vacuum (10 -3 ~10 -6 Pa or 10 -5 ~10 -8 Torr). A magnetic rotary motion feedthrough unit utilizes magnetic fluid to allow rotation of the pump while maintaining a high vacuum environment. Prior to testing the LBE system under vacuum, a pump curve measurement is performed to estimate flowrate in the system. This measurement also generates data on orifice loss coefficients, which are compared to correlations in literature. The second experiment investigates vacuum level in the LBE system during operation. High vacuum is maintained (10 -3 ~10 -5 Pa or 10 -5 ~10 -7 Torr) during system operation, and a residual gas analyzer (RGA) scan shows that partial pressures of residual gases in the LBE system lower over the duration of LBE system operations. The third experiment investigates the gravity driven liquid LBE flowing out of the target chamber in the return line, which is partially full. If the liquid LBE is not drained quickly enough, flooding in the target chamber could occur. The coefficient n in the Manning equation is found to be around 0.008 s/m 1/3 . The last experiment performed is a demonstration that a vacuum jacket could provide sufficient thermal insulation to allow coupling between 300 °C LBE loop and a water tank at room temperature. In conclusion, the results from these experiments have influenced the development of the neutron source for the future commercial scale Mo-99 production system.

43 PARTICLE ACCELERATORS↗

Operando XPS for Plasma Process Monitoring: A Case Study on the Hydrogenation of Copper Oxide Confined under h-BN

Here, we demonstrate that ambient pressure x-ray photoelectron spectroscopy (APXPS) can be used for in situ studies of dynamic changes in surface chemistry in a plasma environment. This opens a new and vast application space for XPS and greatly complements modern spectroscopy techniques to probe plasma-solid/liquid interactions relevant to process monitoring in the semiconductor industry, bio-medical plasma applications and plasma remediation technologies. Hexagonal boron nitride (h-BN) grown on Cu was used in this study as a well-defined model system for plasma process monitoring and because of its unique chemical, optical and electrical properties that make it a prospective material for advanced electronics. To better understand the stability and surface chemistry of h-BN during plasma assisted processing, we track in real time the plasma-induced chemical state changes of B, N and the underlying Cu substrate using APXPS equipped with an AC discharge plasma source operating at 13 Pa. Residual gas analysis (RGA) mass-spectra were concurrently collected during plasma-XPS to track reaction products formed during plasma exposure. A clear reduction of Cu x O is seen, while an h-BN layer remains intact, suggesting hydrogen radical (H • ) species can attack the exposed and h-BN covered Cu oxide patches and partially reduce the underlying substrate without significantly damaging the overlaying h-BN, which is of practical importance for development of h-BN encapsulated devices and interfaces. In addition to demonstration of plasma-XPS capabilities we discuss the observed challenges (e.g., parasitic plasma-chamber walls reactions and charging effects) and propose potential solutions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Uniform Whole Wafer Anisotropic Etching of Structural Ta Thin Films

Tantalum (Ta) has promise as a structural material for micromechanical sensors and actuators. Anisotropic etching of alpha (α) phase Ta is required for micromachining applications. Uniform thickness and etch across a full wafer are desirable features. An experimental investigation is conducted to study plasma etching rate and anisotropy in etching α -Ta in relation to pressure and gas flow ratio. A comparatively low toxicity gas, carbon tetrafluoride (CF4), and argon (Ar) are used. Spectrometry by optical emission spectrometry (OES) and residual gas analysis (RGA) are employed to characterize the plasma to gain insight into the etch mechanisms. At low flow, the etch rate is slow due to an inadequate supply of the etching gas, CF4. The etch rate is also slowed at high flow due to a reduced CF4 residence time. Flow and pressure conditions to achieve a good etch rate and vertical sidewalls are identified and explained by means of a full factorial experiment coupled with emission spectra. Finally, with these conditions, uniform etching of 2.5 μm thick α-Ta across a 4-inch wafer is demonstrated.

36 MATERIALS SCIENCE↗

Ultra-High Vacuum Outgassing Characterization of Thermally Processed Low-Carbon Steel for Advanced Particle Accelerator and Gravitational Wave Detector Applications

This dissertation investigated AISI 1020 low-carbon steel as an alternative vacuum chamber material to conventional stainless steel for ultra-high vacuum (UHV) and extreme-high vacuum (XHV) applications. After a 400 °C/48 h bake, AISI 1020 tube chambers achieved a hydrogen outgassing rate of 2.4 × 10¿¹6 Torr·L·s¿¹·cm¿², approximately 2,300 times lower than the prebaked 316L stainless-steel comparator, among the lowest hydrogen outgassing rates ever reported for an uncoated metallic vacuum chamber. Bare and magnetite-coated AISI 1020 chambers were then compared using throughput and rate-of-rise methods. The magnetite coating yielded 5× lower water outgassing at room temperature, but this advantage disappeared after 80 °C baking. After full thermal conditioning (400 °C/48 h prebake followed by 150 °C/96 h and 200 °C/110 h), bare steel achieved 25× lower hydrogen outgassing than the magnetite-coated chamber (9.6 × 10¿¹6 Torr·L·s¿¹·cm¿²) and >99% H2 purity with carbon species below RGA detection. Monte Carlo molecular flow simulations of a CEBAF photogun beamline (96 scenarios) showed that replacing 304L stainless steel with AISI 1020 reduces equilibrium H2 pressure by a factor of 833; a single 304L electrode contributes 98.8% of the gas load despite occupying only 9.1% of the internal surface area. A 500-m Einstein Telescope beampipe screening showed that corrugated bellows contribute 18% of the gas load from only 0.7% of the surface area. A five-model adsorption isotherm framework applied to 22 pumpdown datasets (164 fits with AR(1)-GLS correction) established that the experimental protocol, not the material, controls isotherm identifiability: Dubinin–Radushkevich wins isothermal pipe pumpdowns; Langmuir wins thermally dominated chamber bakes. Cross-dataset joint fitting of the AISI 1020 pipe pumpdowns yielded an H2 diffusion activation energy Ed = 7.24 ± 1.28 kcal·mol¿¹, consistent with trap dominated diffusion in commercial low-carbon steels. Two companion innovations were developed: a Variable Conductance Device (VCD, patent pending IDF-00723) for XHV outgassing measurement, and VacuumDesignerPro (VDP), a MATLAB-based design tool validated against LIGO benchmarks.

Al-Allaq, Aiman H [Old Dominion University]↗

A remote operation quadrupole mass spectrometer using a custom radio-frequency link approach

A commercial quadrupole mass spectrometer (residual gas analyzer, RGA) system has been modified to operate at large separations of its electronics console and sensing head. The methods implemented have made practical applications, as well as operation, of such a system possible for the first time. This advance was stimulated by a need for placing sensors at remote (45 or 60 m) chamber locations for space simulation testing of orbital flight spacecraft. Emphasis is placed on instrument functional requirements and describing the hardware changes and adjustment techniques necessary to assure operation at the extended cable lengths.

Tashbar, P. W.↗

High Energy Astronomy Observatory program

The series of three orbiting high energy astronomy observatories that comprise the HEAO program are described. Several unique designs as well as the attitude control and determination system, used for observatory scan rotation of the first and third missions and for precision pointing on the second mission, are analyzed. Attention is given to observatory requirements, design characteristics, and the RGA performance summary.

Wojtalik, F. S.↗

Space simulation testing of the Earth Radiation Budget Satellite (ERBS)

The Earth radiation budget components and dynamics and the interactions of this energy cycle, which influences our climate were investigated. The satellite package was subjected to space simulation testing. The size of the spacecraft dictated that the testing be conducted in the new BRUTUS Thermal Vacuum Facility. Computer aided control (CAC), quartz crystal microbalance (QCM), and residual gas analysis (RGA) monitoring are combined with rigid contamination control procedures to protect the flight hardware from anomalous and potentially destructive out of scope test environments.

Magette, E.↗

A long-baseline method for HST gyro drift rate bias calibration

The routine on-orbit calibration of the Hubble Space Telescope (HST) rate gyro assemblies (RGA's) has depended on several related algorithms for drift rate bias calibration. The gyros have exhibited time-varying biases, which must be regularly corrected to maintain pointing stability. Currently, gyro drift parameters are uplinked to the spacecraft every 1-2 days for low rate mode and every 7 days for high rate mode. In order to minimize the impact of frequent calibrations on the HST science schedule, we have refined the gyro calibration algorithms and data collection schemes to reduce the amounts of telemetry data and processing time required for accurate bias calibration. We present a review of the evolution of the gyro calibration algorithms, with particular attention to what we have called the long-baseline bias (LBBIAS) technique, and describe the relative success of these methods in maintaining spacecraft stability.

Boia, John J.↗