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ASTM E 1559 method for measuring material outgassing/deposition kinetics has applications to aerospace, electronics, and semiconductor industries

The American Society for Testing and Materials has published a new standard test method for characterizing time and temperature-dependence of material outgassing kinetics and the deposition kinetics of outgassed species on surfaces at various temperatures. This new ASTM standard, E 1559(1), uses the quartz crystal microbalance (QCM) collection measurement approach. The test method was originally developed under a program sponsored by the United States Air Force Materials Laboratory (AFML) to create a standard test method for obtaining outgassing and deposition kinetics data for spacecraft materials. Standardization by ASTM recognizes that the method has applications beyond aerospace. In particular, the method will provide data of use to the electronics, semiconductor, and high vacuum industries. In ASTM E 1559 the material sample is held in vacuum in a temperature-controlled effusion cell, while its outgassing flux impinges on several QCM's which view the orifice of the effusion cell. Sample isothermal total mass loss (TML) is measured as a function of time from the mass collected on one of the QCM's which is cooled by liquid nitrogen, and the view factor from this QCM to the cell. The amount of outgassed volatile condensable material (VCM) on surfaces at higher temperatures is measured as a function of time during the isothermal outgassing test by controlling the temperatures of the remaining QCM's to selected values. The VCM on surfaces at temperatures in between those of the collector QCM's is determined at the end of the isothermal test by heating the QCM's at a controlled rate and measuring the mass loss from the end of the QCM's as a function of time and temperature. This reevaporation of the deposit collected on the QCM's is referred to as QCM thermogravimetric analysis. Isothermal outgassing and deposition rates can be determined by differentiating the isothermal TML and VCM data, respectively, while the evaporation rates of the species can be obtained as a function of temperature by differentiating the QCM thermogravimetric analysis data.

Garrett, J. W.↗

Temporary Atmospheres Produced By Human Activities on the Moon

Outgassing from materials, whether through the ascent/descent stages of lunar vehicles, airlock depressurizing, rover or astronaut suit outgassing, may cause an effect of unwanted accumulation of volatiles at the surface and exosphere. This is especially important at (or proximal) to permanently shadowed regions (PSRs) at the lunar poles. Herein, we provide estimates of expected outgassing from various human-landed objects on the Moon, including backpacks, airlocks, rovers, landers, trash and mining operations. Astronaut suits produce some level of oxygen outgassing (Helou et al., 2022), which may transport and condense in these PSRs, even in micro- cold traps (Glavin et al., 2010).We estimate the outgassing from drill mining and trash-to-gas conversion assuming a specific technology is operating. These outgassing systems can create local, temporary atmospheres in the vicinity (∼100 km radius) of the sources. The atmosphere may be particularly high within meters of the source. To obtain column densities for these temporary atmospheres, we first bracket ranges for the gas number loss as a function of time. We then derive the maximum distance traveled and the time the released molecules remain in the exosphere for a single ballistic hop, assuming the molecules are ejected from the surface of the object at its surface temperature. In some cases, such as the astronaut backpack and the rover, the temperature is that of the source. Given this information, an average and peak local exospheric density and column density can be estimated. We find that backpacks, airlock releases, and the Starship lander can create relatively high-density local atmospheres, with local near-lander outgassing water densities exceeding 107/cm3. This local water exosphere is over 106 times greater than the LADEE-derived lower limit of the natural water exosphere at ∼3/cm3. Thus, the anthropogenic temporary water exosphere will likely dominate the environment near the lander, making an assessment of the natural exospheric water environment difficult.

Rosemary M Killen↗

Application of Molecular Adsorber Coatings in Chamber A for the James Webb Space Telescope

As a coating made of highly porous zeolite materials, the Molecular Adsorber Coating (MAC) was developed to capture outgassed molecular contaminants, such as hydrocarbons and silicones. For spaceflight applications, the adsorptive capabilities of the coating can alleviate on-orbit outgassing concerns on or near sensitive surfaces and instruments within the spacecraft. Similarly, this sprayable paint technology has proven to be significantly beneficial for ground-based space applications, in particular, for vacuum chamber environments. This presentation describes the application of the MAC technology for the James Webb Space Telescope (JWST) at NASA Johnson Space Center (JSC). The coating was used as a mitigation tool to entrap outgassed contaminants, specifically silicone-based diffusion pump oil, from within JSCs cryogenic optical vacuum chamber test facility called Chamber A. This presentation summarizes the background, fabrication, installation, chemical analysis test results, and future plans for the MAC technology, which was effectively used to protect the JWST test equipment from vacuum chamber contamination. As a coating made of highly porous zeolite materials, the Molecular Adsorber Coating (MAC) was developed to capture outgassed molecular contaminants, such as hydrocarbons and silicones. For spaceflight applications, the adsorptive capabilities of the coating can alleviate on-orbit outgassing concerns on or near sensitive surfaces and instruments within the spacecraft. Similarly, this sprayable paint technology has proven to be significantly beneficial for ground-based space applications, in particular, for vacuum chamber environments. This presentation describes the application of the MAC technology for the James Webb Space Telescope (JWST) at NASA Johnson Space Center (JSC). The coating was used as a mitigation tool to entrap outgassed contaminants, specifically silicone-based diffusion pump oil, from within JSCs cryogenic optical vacuum chamber test facility called Chamber A. This presentation summarizes the background, fabrication, installation, chemical analysis test results, and future plans for the MAC technology, which was effectively used to protect the JWST test equipment from vacuum chamber contamination.

molecular contamination↗

Improved materials characterization for spacecraft applications

A material outgassing test consists of an effusion cell, mass spectrometer, and thermally controlled quartz crystal microbalance (TQCM). The material sample is placed in the effusion cell at a predetermined temperature, and the sample is outgassed in a vacuum of 0.000001 torr range. The total outgassing mass as a function of time is determined with the TQCM which is cooled to LN2 temperatures. Based on the view factor of the TQCM, the total outgassed mass can be determined. The technique can be verified by comparing the results to the actual mass loss of the sample which is determined by hanging the diffusion cell from the Cohn microbalance. The mass spectrometer can be used to determine if there are any low molecular weight components outgassing, such a nitrogen which does not condense on the TQCM. After the material outgasses to a point of saturation, the effusion cell is closed off, and the TQCM is slowly heated to allow the condensed film to be broken down into its components. As the temperature is increased, the components evaporate from the surface at a different rate and can be detected with the mass spectrometer. The relative amount of each component is found by the change in frequency of the TQCM as the component evaporates. Hence, from this test, not only is isothermal kinetic data obtained, but the primary components can also be identified in terms of their molecular weight.

Cull, R.↗

Some Sources of Contaminants in the Shuttle Bay Measured with Temperature-Controlled Quartz Crystal Microbalances (TQCM)

The sources of molecular deposits on a Temperature-Controlled Quartz Crystal Microbalance (TQCM) attached to the shuttle bay wall at some distance from the payload and pointing out of the bay have been investigated. Explored as possible sources are: (1) the outgassing of the shuttle tiles treated with the water proofing di-methyl-ethoxy-silane (DMES) compound, scattered back by the ambient molecules into the bay; (2) The ambient scattered return flux of the outgassing, from the RTV 560 silicone which is used as the adhesive for the tiles; (3) the ambient scattered return flux of the payload outgassing; (4) the return C, flux from outgassing source originating near, below, or adjacent to the package containing the TQCM; and (5) the self-scattering of venting plumes and outgassing above the monitor package depositing on the TQCM. In all of these sources, the magnitudes of the outgassing, of the leakage rates, and venting had to be estimated in the absence of data. The resulting analyses which can be useful for similar investigations, indicates that the outgassin- from the tiles, the RTV, the payloads, or the shuttle may not have been the sources of the deposit (about 1 micro g/cm(sup 2) during a the period from bay door opening and payload release from the bay). It appears more probable that the origin is the self- and/or ambient-scattered return fluxes originating near, below, or internal to the monitor package.

Scialdone, John J.↗

Self-contamination and environment of an orbiting spacecraft

The flux of molecules emitted by a spacecraft and subsequently reflected to its surface was investigated. The reflection occurs upon collision of the outgassed molecules with ambient molecules. Evaluation of the flux was based on a knowledge of the spacecraft outgassing rate, the spacecraft dimensions, and the orbit parameters. Condensation rates and adsorption layers on critical surfaces were calculated from the knowledge of this flux and the nature and temperature of the gas and the surface. Based on estimated and measured emission rates, calculation of these parameters was performed for a number of spacecraft. The relationships and graphs developed allow an estimate of several important parameters for an orbiting spacecraft to be made. The pressures and densities at various distances from the spacecraft, as produced by the surrounding ambient molecules and by the spacecraft's own outgassing, are presented. The pressure and density produced by the outgassing can be obtained as a function of time if the behavior of the outgassing with time is known. The number of desorbed molecules ionized by impact with ambient charged particles and the effect of the spacecraft's electric field on polarized desorbed molecules were considered.

Scialdone, J. J.↗

Potential for EMU Fabric Damage by Electron Beam and Molten Metal During Space Welding for the International Space Welding Experiment

As a consequence of preparations concerning the International Space Welding Experiment (ISWE), studies were performed to better understand the effect of molten metal contact and electron beam impingement with various fabrics for space suit applications. The question arose as to what would occur if the electron beam from the Ukrainian Universal Hand Tool (UHT) designed for welding in space were to impinge upon a piece of Nextel AF-62 ceramic cloth designed to withstand temperatures up to 1427 C. The expectation was that the electron beam would lay down a static charge pattern with no damage to the ceramic fabric. The electron beam is capable of spraying the fabric with enough negative charge to repel further electrons from the fabric before significant heating occurs. The static charge pattern would deflect any further charge accumulation except for a small initial amount of leakage to the grounded surface of the welder. However, when studies were made of the effect of the electron beam on the insulating ceramic fabric it was surprisingly found that the electron beam did indeed burn through the ceramic fabric. It was also found that the shorter electron beam standoff distances had longer burnthrough times than did some greater electron beam standoff distances. A possible explanation for the longer burnthrough times for the small electron beam standoff distance would be outgassing of the fabric which caused the electron beam hand-tool to cycle on and off to provide some protection for the cathodes. The electron beam hand tool was observed to cycle off at the short standoff distance of two inches likely due to vapors being outgassed. During the electron beam welding process there is an electron leakage, or current leakage, flow from the fabric. A static charge pattern is initially laid down by the electron beam current flow. The static charge makes up the current leakage flow which initially slightly heats up the fabric. The initially laid down surface charge leaks a small amount of current. The rate at which the current charge leaks from the fabric controls how fast the fabric heats up. As the ceramic fabric is heated it begins to outgass primarily from contamination/impurities atoms or molecules on and below the fabric surface. The contaminant gases ionize to create extra charge carriers and multiply a current of electrons. The emitted gas which ionized in the electron leakage flow promotes further leakage. Thus, the small leakage of charge from the fabric surface is enhanced by outgassing. When the electron beam current makes up the lost current, the incoming electrons heat the fabric and further enhance the outgassing. The additional leakage promotes additional heating up of the ceramic fabric. The electrons bound to the ceramic fabric surface leak off more and more as the surface gets hotter promoting even greater leakage. The additional electrons that result also gain energy in the field and produce further electrons. Eventually the process becomes unstable and accelerates to the point where a hole is burned through the fabric.

Fragomeni, James M.↗

Secondary Volcanically-Induced Lunar Atmosphere and Lunar Volatiles: 3-D Modeling and Analysis

The fact that the Moon could have a transient secondary atmosphere due to volcanic outgassing has been known for some time, though typically such an atmosphere was believed to be extremely thin (~10-8 bar) [1]. But recent research by Needham and Kring (NK) [2] suggests that during the peak of volcanic activity ~3.5 Ga such a volcanically-outgassed atmosphere could reach ~10-2 bar of surface pressure. In similar research Wilson et al. [3] proposed a more conservative estimate, arguing that the thickness of such an atmosphere would depend on the intervals between major eruptions and may not exceed microbar densities. In either case a collisional atmosphere could be present, which would control transport of outgassed volatiles (such as H2O) and their deposition in polar regions, where they could be preserved until modern day frozen in permanently shadowed regions (PSR) or buried beneath the regolith. Here we study such a hypothetical atmosphere to investigate its stability, meteorological properties and the effect on transport of volatiles. We use the ROCKE-3D planetary 3-D General Circulation Model (GCM)[4]. The insolation and orbital parameters were set to conditions 3.5 Ga. The atmospheric composition, based on the list of outgassed species presented by NK in combination with our estimates for atmospheric escape, condensation and the results from our 1-D chemistry model, was chosen to be either CO-dominated or CO2-dominated (depending on atmospheric temperature). In this study we restricted ourselves to relatively "thick" lunar atmospheres of 1-10 mb, though we believe that our results will scale to thinner atmospheres as well. We present the results for ground and atmospheric temperature for modeled atmospheres over a wide parameter space. In particular we consider different atmospheric compositions (CO or CO2 dominated), a set of atmospheric pressures from 1 mb to 10 mb and a set of obliquities from 0o to 40o. We also present an experiment of a single major eruption [5] and show that in just 3 years ~80% of the outgassed water is deposited in polar regions. This demonstrates the efficiency of such an atmosphere in delivering volatiles. We argue that a secondary lunar atmosphere could play a significant role in forming volatile deposits currently observed in the polar regions of the Moon.

Lunar atmospheres↗

Materials testing for spacecraft use

A technique has been developed for determining the outgassing characteristics of materials intended for spacecraft use. A measurement of the total mass loss (TML) and of the collected volatile condensable materials (CVCM) is used as a guide for selecting those materials low in outgassing. The data were used to compare the outgassing from two conductive black paints. In addition, the apparatus was also used in an attempt to simulate expected launch temperatures by collecting the outgassed molecules on a glass plate, which simulates a nearby thermal control surface. The glass plate was then irradiated in vacuum by simulated sunlight. Transmittance patterns of the clean glass plate and also with the condensed material on it were compared with the transmittance pattern after irradiation of the condensate. The transmittance patterns showed a drastic change. The resultant discoloration indicated the detrimental effects of the contamination and aided in selecting the better conductive paint. Additional tests utilizing an aluminized mirror collector plate have been run to show the effect of irradiation upon the CVCM from certain different classes of materials often used on spacecraft.

Park, J. J.↗

Direct simulation Monte Carlo technique for modeling of the environment in the vicinity of the Space Shuttle Orbiter

A program for analyzing the flowfield parameters in the neighborhood of the Space Shuttle Orbiter has been developed. The program uses the direct simulation Monte Carlo method, which is a completely probabilistic Monte Carlo technique capable of analyzing 3-dimensional steady or unsteady flow with prescribed internal and external boundary conditions. The freestream flux densities incident on the external flowfield boundaries are calculated from the drifting Maxwellian gas properties of the freestream. The flux entering the flowfield from the internal boundary is calculated from the outgassing flux density distribution over the Shuttle external surface and the prescribed discrete source fluxes. This technique produces a numerical flowfield solution which is the probabilistic equivalent of a complete solution of the time-dependent, 3-dimensional Boltzmann equation. Flowfield results are presented for the following configurations: (1) Shuttle angles of attack of 0 and 90 deg, (2) freestream density 10 to the 9th - 10 to the 11th per cu cm, (3) Shuttle outgassing flux density, and (4) operation of the aft downfiring vernier Reaction Control System (RCS) engine. Results are presented for column density distribution of outgassed and engine species and for the flux density of outgassed and engine species incident on the Shuttle bay and the windshield.

Melfi, L. T., Jr.↗

Contamination Measurements During Ius Thermal Vacuum Tests in A Large Space Chamber

The levels of contamination that originate from inside the IUS equipment support section (ESS) due to outgassing from electronics components and wiring operating at elevated temperatures (80-160 F) were investigated. Pressure was measured inside and outside the ESS. Mass deposition measurements were made with quartz crystal microbalances (QCM) facing into and away from ESS vents. The OCM's were operated at -50 C and -180 C using thermoelectrically and cryogenically cooled QCM's. Gaseous nitrogen flow inside the ESS was used to obtain the effective molecular flow vent area of the ESS, which was evaluated to be 359 sq cm (56 sq in) compared to the 978 sq cm (150 sq in) estimated by an earlier atmosphere pressure billowing test. The total outgassing rate of the ESS materials at a temperature of 60 C (140 F) decays with a time constant of 11.5 hours based on pressure measurements during the hot cycle. A time constant of 22 hours was estimated for the fraction of the outgassing which will condense on a -50 C surface. In contrast, the time constant is only 10.1 hours for the outgassing material which condenses on a surface at -180 C. A surface at -180 C collects approximately one half of the material vented from the ESS which impinges on it. Pressure measurements show very good correlation with the mass deposition measurements.

C R Mullen↗

Screening and tests of materials for space applications

The outgassing properties of materials and other considerations on materials acceptance for space applications are discussed. The uses of the outgassing data for the evaluation of important performance characteristics of a space system are indicated. The deficiencies and advantages of the ASTM-E595-77 test method and materials acceptance criteria are discussed. Also discussed are the advantages for the selection of the materials and the uses of the data provided by the long-term measurements of the outgassing rates and surface re-emission of materials. The paper concludes that the results of the ASTM method with additional derived data on the material properties can be used for the initial evaluation of a space system's characteristics. Materials data on outgassing and re-emission rates at various temperatures obtained from the more expensive, long-term QCM and TGA measurements should be obtained when a detailed analysis of a system is suggested based on the various considerations discussed in the paper.

Scialdone, J. J.↗

Thermal-vacuum response of polymer matrix composites in space

This report describes a thermal-vacuum outgassing model and test protocol for predicting outgassing times and dimensional changes for polymer matrix composites. Experimental results derived from 'control' samples are used to provide the basis for analytical predictions to compare with the outgassing response of Long Duration Exposure Facility (LDEF) flight samples. Coefficient of thermal expansion (CTE) data are also presented. In addition, an example is given illustrating the dimensional change of a 'zero' CTE laminate due to moisture outgassing.

Tennyson, R. C.↗

The Design of a Remotely Operated Shutter (ROS) for Thermal Vacuum Testing

Space-flight hardware is required to meet specific outgassing criteria under vacuum conditions in order to reduce the risk of contaminating sensitive optics and spacecraft components. Under certain circumstances, it is desirable to measure the contamination levels that are being released from all surfaces of the test payload. This certification is often accomplished with a Total Outgassing Measurement (TOM) box. The TOM box has one 103.2 square centimeter (16 square inch) opening and one 4.84 square centimeter (0.75 square inches) opening. The larger opening allows contaminants to easily escape the box during the hardware bakeout phase. The smaller opening provides a limited conductance path for outgassed contaminants during the certification phase. A Thermoelectric Quartz Crystal Microbalance (TQCM) monitors the contamination levels inside the box to provide the total outgassing measurement. During transition from the bakeout phase to the certification phase, the TOM box is reconfigured to close the larger opening. For previous certifications, the vacuum chamber was returned to ambient conditions and the larger conductance port was closed manually. The ROS system eliminates the need to enter the chamber by remotely closing the large TOM box opening. Substantial schedule and cost savings are achieved through the use of this system. The ROS system consists of three main components; a shutter, a motion actuator, and an actuator controller. Each of these components was selected or designed to operate in an extreme-temperature and vacuum environment while providing a high level of reliability. Different types of motion actuators were considered for driving the shutter. Design parameters for the actuator included material properties, force capability, reliability, and cost.

Hale, Kathleen L.↗

Insitu Calibration of Quartz Crystal Microbalances

Computer models that predict the rate at which molecular contamination will deposit on optical surfaces typically use outgassing source terms, measured with quartz crystal microbalances, as a basis for the prediction. The American Society of Testing and Materials, Standard Test Method for Contamination Outgassing Characteristics of Spacecraft Materials (Method E-1559), is probably the best know technique used by the aerospace community to measure the outgassing rates or source terms of materials. A simple method for the insitu calibration of quartz crystal microbalances, based on the heat of enthalphy of Adipic Acid, has been developed and demonstrated by the Marshall Space Flight Center, Environmental Effects Group. The calibration has been demonstrated over a sample temperature range of 25 to 66 degrees Celsius and deposition rates of 7 x 10 (exp -11) grams/cm(sup 2)-s and greater, for several measurement system configurations. This calibration technique is fully compatible with the American Society for Testing and Materials, Method E-1559, as well as other methodology. The calibration requires no modification of outgassing facilities employing an effusion cell and does not degrade the performance or function of typical vacuum systems.

Albyn, Keith↗

Space Environmental Effects Knowledgebase

This report describes the results of an NRA funded program entitled Space Environmental Effects Knowledgebase that received funding through a NASA NRA (NRA8-31) and was monitored by personnel in the NASA Space Environmental Effects (SEE) Program. The NASA Project number was 02029. The Satellite Contamination and Materials Outgassing Knowledgebase (SCMOK) was created as a part of the earlier NRA8-20. One of the previous tasks and part of the previously developed Knowledgebase was to accumulate data from facilities using QCMs to measure the outgassing data for satellite materials. The main object of this current program was to increase the number of material outgassing datasets from 250 up to approximately 500. As a part of this effort, a round-robin series of materials outgassing measurements program was also executed that allowed comparison of the results for the same materials tested in 10 different test facilities. Other programs tasks included obtaining datasets or information packages for 1) optical effects of contaminants on optical surfaces, thermal radiators, and sensor systems and 2) space environmental effects data and incorporating these data into the already existing NASA/SEE Knowledgebase.

Wood, B. E.↗