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Residual gas analyzer and leak detector by time of flight measurements on neutral metastable atoms and molecules between pulsed electron gun and auger surface detector
Fatigue behavior of aluminum in reduced partial pressures of oxygen, water and hydrogen, noting residual gas atmosphere role
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.
With a revived focus to create a permanent presence on the moon and in preparation for future Mars exploration, it is imperative that all resources are utilized to their fullest potential.[1] 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(LO2) for not only breathable air, but also for rocket propellant. On the moon and potentially Mars, one of the most O2 rich resources is in the presence of regolith.[2],[3] 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.
Residual gases in oil-diffusion-pump ultrahigh vacuum determined as function of various trapping conditions
The amounts and composition of residual gases formed in sealed silica glass ampoules were investigated. The effect of the silica brand, outgassing and annealing conditions, system geometry, and a presence of graphite were determined and discussed.
The amounts and composition of residual gases formed in sealed silica glass ampoules were investigated. The effect of the silica brand, outgassing and annealing conditions, system geometry, and presence of graphite are determined and discussed.
The amounts and composition of residual gases formed in sealed ampoules loaded with different sources (elements and II-VI and IV-VI compounds) after consecutive annealings were investigated. A given source was subjected to a series of heat treatments, with intermediate measurements and removal of the gas accumulated in the system. The results of these experiments are discussed in terms of the underlying thermochemical and kinetic phenomena and practical limitations of reducing the amount of residual gases in sealed ampoules.
The amount and composition of residual gases formed in sealed ampoules loaded with different elements or binary II-VI or IV-VI compounds were investigated. The source materials underwent different thermal processings, annealing and/or resublimation conducted under different conditions. The results of these experiments are discussed in terms of the procedural, thermochemical, and kinetic limitations to the process.
The amount and composition of residual gases formed in sealed ampoules loaded with different elements or binary II-VI or IV-VI compounds and subjected to various thermal processings, annealing and/or resublimation conducted under different conditions were investigated. The results of these experiments are discussed in terms of the procedural, thermochemical, and kinetic limitations to the process.
Our long term goal has been to make detached solidification reproducible, which requires a full understanding of the mechanisms underlying it. Our Moving Meniscus Model of steady-state detachment predicts that it depends strongly on the surface tension of the melt and the advancing contact angle with the ampoule wall. Thus, the objective of the current project was to determine the influence of residual gases on the surface tension and contact angle of molten semiconductors on typical ampoule materials. Our focus was on the influence of oxygen on indium antimonide on clean silica ("quartz"). The research was performed by three chemical engineering graduate students, the third of whom will complete his research in the summer of 2005. Originally, we had planned to use a sealed silica cell containing a zirconia electrochemical element to control the oxygen partial pressure. However, zirconia requires an operating temperature above the 530 C melting point of InSb and is difficult to form a gas-tight seal with silica. Thus, we decided instead to flow an oxygen-containing gas through the cell. A special apparatus was designed, built and perfected. A piece of InSb was placed on a horizontal silica plate in a quartz cell. High purity argon, helium or hydrogen-containing gas is passed continuously through the cell while the oxygen concentration in the effluent gas is measured. The shape of the resulting drop was used to determine contact angle and surface tension of Ga-doped and high purity InSb. Oxygen appeared to decrease the contact angle, and definitely did not increase it. The following section gives the background for the research. Section 2 summarizes the results obtained on Ga-doped InSb with relatively high oxygen concentrations. Section 3 describes recent improvements made to the apparatus and methods of analysis. Section 4 gives recent results for high-purity InSb at low oxygen concentrations. Final results will be obtained only this summer (2005). Each section has its own references.
Many microgravity directional solidification experiments yielded ingots with portions that grew without contacting the ampoule wall, leading to greatly improved crystallographic perfection. Our long-term goal is to make such detached solidification reproducible, which requires a full understanding of the mechanisms underlying it. Our Moving Meniscus Model of steady-state detachment predicts that it depends strongly on the surface tension of the melt and the advancing contact angle with the ampoule wall. Detached solidification is more likely when the contact angle for the melt on the ampoule wall is high, i.e. non-wetting. It has been claimed that impurities increase the contact angle. The objective of the current project is to determine the influence of residual gases on the surface tension and contact angle of molten semiconductors on typical ampoule materials. We are focusing on determining the influence of oxygen on the contact angle of molten InSb on clean silica ('quartz'), including the advancing and retreating contact angles in addition to the usual equilibrium contact angle. We have created a gas flow system that allows us to control the oxygen partial pressure over a sessile drop of InSb on a horizontal quartz surface. The cell is slowly tilted while videotaping to reveal the contact angles on the two sides of the drop just prior to it rolling down the surface. Thus far, we have learned the following: (1) Molten InSb readily forms an oxide layer in the presence of the trace amounts of oxygen found in high purity argon; (2) This oxide contains a substantial amount of Ga, which presumably is a trace contaminant that is not detectable in the starting material; (3) The addition of 10% hydrogen to the argon gas is sufficient to reduce the oxide and produce a clean drop; (4) An infrared filter must precede the video camera in order to produce a sharp image of the drop for later image analysis; (5) Tilting the surface on which the drop rests causes the two sides of the drop to display different contact angles, reflecting contact line sticking; (6) Vibration strongly accelerates the approach of the drop to its final shape on a horizontal surface by helping to overcome sticking of the contact line; (7) Oscillation of the drop surface due to vibration appears to increase as the surface is inclined from horizontal. Presumably, the angle at which the drop rolls down the surface is also reduced by vibration. This observation is particularly significant, as the meniscus must move along the ampoule wall during detached solidification.
A computer program for automatic determination of gases found in an environmental chamber during spacecraft testing is discussed. Program testing is reviewed. The program is being used for the solution of experimental spectra, where the mass spectrometer is used as a contamination monitor by an untrained spectroscopist.
Types of instruments studied were magnetic sector, omegatron, quadrupole, and monopole. Experimental results obtained included absolute sensitivity to argon, relative sensitivity to ten gases (hydrogen, helium, neon, nitrogen, carbon monoxide, oxygen, argon, carbon dioxide, krypton, and xenon), and cracking patterns for these gases.
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With a revived focus to create a permanent presence on the moon and in preparation for future Mars exploration ,it is imperative that all resources are utilized to their fullest potential.[1] 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 (LO2)for not only breathable air, but also for rocket propellant.On the moon and potentially Mars, one of the most O2rich resources is in the presence of regolith.[2],[3]Although there are numerous minerals within regolith and various processes to extract O2, this is not the scope of this poster
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The Carbothermal Reduction Demonstration (CaRD) project is currently developing a subscale system to demonstrate the operation and performance of the carbothermal reduction process and quantify the production of molar equivalent oxygen via carbon monoxide (CO) and carbon dioxide (CO2). Traditionally, gas chromatography (GC) systems are utilized to quantify gases due to their ability to separate volatile compounds within the gas mixture, followed by detection of the isolated component of interest. Despite their capabilities, GCs require carrier gas consumables for their operational mobile phase and consequently are not often considered a flight-forward option. An alternative analytical technique known as mass spectrometry measures the presence of gas phase molecules without the need of carrier gas. Residual gas analyzers (RGAs), which are smaller and rugged mass spectrometers, are not traditionally used to quantify analytes as they serve more as a monitoring tool. However, proper application and calibration can result in a flight-forward analytical instrument capable of direct quantification of volatile compounds of interest. Kennedy Space Center's role for the JSC led CaRD project is to design a gas analyzer system to detect and quantify the CO and CO2 gases produced during the carbothermal reaction utilizing a commercial version of the Mass Spectrometer observing lunar operations (MSolo) instrument. MSolo is a modified commercial off-the-shelf RGA, which consists of quadrupole mass filter and space rated electronics. MSolo is currently a TRL 6 technology and manifested on the PRIME-1 and VIPER missions. This paper describes leveraging MSolo based instrumentation to develop a gas analysis system for the work outlined in the 2023 International Conference on Environmental Systems (ICES) paper number 313.