SEARCH · Search NASA
Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.
Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.
Moisture-induced agining and degradation are continuing concerns in long-term storage and use of silicone materials. The silica fillers frequently used to provide mechanical reinforcement in silicone formulations have a high affinity for H2O and act as a source of moisture outgassing later when placed in dry or vacuum applications.
Despite its importance for the global cycling of carbon, there are still large gaps in our understanding of the processes driving annual and seasonal carbon fluxes in the high-latitude Southern Ocean. This is due in part to a historical paucity of observations in this remote, turbulent, and seasonally ice-covered region. Here, we use autonomous biogeochemical float data spanning 6 full seasonal cycles and with circumpolar coverage of the Southern Ocean, complemented by atmospheric reanalysis, to construct a monthly climatology of the mixed layer budget of dissolved inorganic carbon (DIC). We investigate the processes that determine the annual mean and seasonal cycle of DIC fluxes in two different zones of the Southern Ocean—the Sea Ice Zone (SIZ) and Antarctic Southern Zone (ASZ). We find that, annually, mixing with carbon-rich waters at the base of the mixed layer supplies DIC which is, in the ASZ, either used for net biological production or outgassed to the atmosphere. In contrast, in the SIZ, where carbon outgassing and the biological pump are weaker, the surplus of DIC is instead advected northward to the ASZ. In other words, carbon outgassing in the southern Antarctic Circumpolar Current (ACC), which has been attributed to remineralized carbon from deep water upwelled in the ACC, is also due to the wind-driven transport of DIC from the SIZ. These results stem from the first observation-based carbon budget of the circumpolar Southern Ocean and thus provide a useful benchmark to evaluate climate models, which have significant biases in this region.
Even though a generalized moisture outgassing modeling has been established and published in a peer-reviewed venue for as-received silica-filled silicones, it is still not yet intuitive for use in engineering/scientific applications. A simplification of the mathematics down to a practical level and illustration of how to do it would be beneficial to the practitioners in the field. In this report, simplified and more intuitive demonstrations of how to use the generalized outgassing kinetics for the prediction of H 2 O release from as-received and previously vacuum-baked silicones will be illustrated.
Outgassing of 3D printed and casted silica-filled silicones was studied using a standard ASTM E-595 procedure and a modified Soreq’s method that allows very sensitive measurements of the outgassing kinetics even at low temperatures, 20 – 50 °C. We studied three different silica-filled silicones, non-porous cased M9787, and 3D printed LL50 and 40P materials. The present report shows that vacuum outgassing products of polysiloxane-based materials include multiple species. In addition to chemisorbed and physisorbed water outgassing, previously studied by TPD, polymer fragments of varying sizes evaporate as well. The chemical composition of the condensable volatile species collected on a Germanium substrate, was analyzed by FTIR. It was shown that all studied materials produce mostly PDMS-based outgassing products that form stable droplet-like structure on the Ge substrate. The highest amount of the condensable volatile species was measured for LL50. Isothermal TGA in nitrogen atmosphere of the LL50 material was compared to the standard vacuum outgassing. The results of TGA showed lower mass loss and higher water regain. The kinetics of the outgassing at relatively low temperatures of 20, 30 and 50 °C was studied using Thermoelectric Quartz Crystal Microbalance (TQCM). The TQCM surface was held at -10 °C to enhance condensation of the outgassed moisture. The analysis presented here, when combined with the extensive previous work on moisture outgassing, provides a better understanding of the aging mechanism of polysiloxane-based materials. In this work we show that outgassing techniques, usually applied for qualification of polymers for space-related applications, may be used as a complementary method to study thermal degradation and aging of silica-based silicones. Our results indicate that the long-term degradation mechanics and thermal degradation products depend primarily on the chemical composition of silicone-based material and only slightly affected by the manufacturing process. Surprisingly, the surface-to-volume ratio of the 3D printed vs. casted/molded materials showed only minor effect on the outgassing kinetic parameters.
A solar panel array with more than ten years space exposure was removed from the Mir core module in November 1997, and an eight panel section was returned to Earth in January 1998. Several solar cells were removed from panel eight of the returned array and placed in a high vacuum system with a residual gas analyzer (200 amu mass spectrometer) and a cold finger. Similar unflown solar cells of the same vintage were later obtained from Energia. Several of the unflown cells were also placed in the vacuum system and outgassed residues were collected on the LN2 cold finger. Almost 3 mg of outgassed residue was collected -from a string of three unflown solar cells over a period of 94 hours under vacuum. The collected residue was weighed with a microbalance, and then the residue was analyzed by FTIR spectroscopy, and by gas chromatograph-mass spectroscopy. About 25 outgassed constituents were separated by the gas chromatograph, and a high-resolution mass spectrum was obtained of each constituent. Molecular identifications have been made for the constituents. The constituents are primarily cyclic siloxanes, and several of the constituents are isomers of the same molecule. Most of the outgassed constituents have a molecular mass of about 500 amu. Almost one mg of residue was extracted from one sq cm of coverglass/adhesive from a flown solar cell by soaking in isopropyl alcohol for 30 minutes. The gas chromatograph separated about 20 constituents. The constituents are mostly cyclic siloxanes with linear branches, hydrocarbons, and phthalates. The typical molecular mass is about 600 amu. These identifications of specific outgassing molecules have resulted in a more complete understanding of the SiO(x) contamination on the Mir solar cell coverglasses, and on the MEEP experiment trays and optical specimens during the Shuttle-Mir Phase One flight experiment program. Adjusted outgassing rates based on the data reported here, and/or measured outgassing rates and specific molecular identifications of ISS hardware samples are needed to input into model predictions of induced environment effects of the ISS.
The Origins, Spectral Interpretation, Resource Identification, and Security–Regolith Explorer (OSIRIS-REx) spacecraft launched on September 8, 2016, beginning a seven-year journey to return at least 60 g of asteroid material from (101955) Bennu to Earth. During the outbound cruise, Doppler tracking of the spacecraft observed a small but measurable acceleration when the sample return capsule (SRC) was first placed in sunlight. Subsequent analysis determined that outgassing from the SRC is the most likely cause for the acceleration. This outgassing received combined engineering and scientific attention because it has potential implications both for spacecraft navigation performance and for contamination of the collected samples. Thermal modeling, laboratory studies of SRC materials, and monitoring of the acceleration are all consistent with H2O as the main component of the outgassing. Dedicated, in-flight campaigns continued to expose the SRC to sunlight until the acceleration dropped to the acceleration noise floor. Any residual amounts of H2O outgassing are not considered to be a hazard with regards to mission operations or pristine sample acquisition. The sample stow procedure has been updated to ensure that no direct line of site exists between any residual outgassing and the samples during future operations. Similar outgassing of the Stardust SRC probably also occurred. No adverse contamination of Stardust samples was observed that could be associated with this process. Future missions that use similar reentry vehicles should consider procedures to test for and, if necessary, mediate such outgassing after launch.
The Origins, Spectral Interpretation, Resource Identification, and Security–Regolith Explorer (OSIRIS-REx) spacecraft launched on September 8, 2016, beginning a seven-year journey to return at least 60 g of asteroid material from (101955) Bennu to Earth. During the outboundcruise, Doppler tracking of the spacecraft observed a small but measurable acceleration when the sample return capsule (SRC) was first placed in sunlight. Subsequent analysis determined that outgassing from the SRC is the most likely cause for the acceleration. This outgassing received combined engineering and scientific attention because it has potential implications both for spacecraft navigation performance and for contamination of the collected samples. Thermal modeling, laboratory studies of SRC materials, and monitoring of the acceleration are all consistent with H2O as the main component of the outgassing. Dedicated, in-flight campaigns continued to expose the SRC to sunlight until the acceleration dropped to the acceleration noise floor. Any residual amounts of H2O outgassing are not considered to be a hazard with regards to mission operations or pristine sample acquisition. The sample stow procedure has been updated to ensure that no direct line of site exists between any residual outgassing and the samples during future operations. Similar outgassing of the Stardust SRC probably also occurred. No adverse contamination of Stardust samples was observed that could be associated with this process. Future missions that use similar reentry vehicles should consider procedures to test for and, if necessary, mediate such outgassing after launch.
The outgassing properties of bare and magnetite-coated AISI 1020 low-carbon steel vacuum chambers were evaluated to establish material selection criteria for extreme high vacuum applications, namely, to explore the possibility of using these materials to build next-generation spin-polarized photoelectron guns. Water outgassing measurements using the throughput method revealed that the magnetite-coated chamber exhibited five times lower outgassing at room temperature prior to baking, but this advantage disappears after 80 °C baking. Hydrogen outgassing measurements demonstrated significant differences after intensive heat treatment: the bare low-carbon steel vacuum chamber achieved a specific outgassing rate of 9.6 × 10 −16 Torr L s −1 cm −2 after 400 °C/50 h bake plus additional heat treatment at lower temperatures, 25 times lower than the magnetite-coated low-carbon steel chamber. Residual gas analysis showed >99% hydrogen composition after heat treatment for both materials, with carbon species below detection limits for bare low-carbon steel versus 0.8% for magnetite-coated surfaces. These measurements indicate that properly conditioned bare low-carbon steel can achieve the <10 −12 Torr pressures required for next-generation spin-polarized photogun applications. In conclusion, the paper includes various analysis techniques intended to explain observed behaviors: isotherm analysis of pump-down plots, Arrhenius analysis of hydrogen outgassing rate data, and residual gas composition tracking.
A universal outgassing model for all silica-filled silicones would allow researchers to make moisture outgassing predictions for many different silica-filled silicones using the same sets of kinetic parameters (but with different intensities for the outgassing constituents). In FY 2020, we succeeded in developing such a model for outgassing in a vacuum/dry environment after ~ 1-2 hours of room temperature vacuum pump. That means the FY2020 model does not account for the low temperature diffusional moisture outgassing during the first few hours under vacuum pump. In FY 2021, we have used the experimental technique of dynamic vapor sorption together with the modified Page diffusion model to measure and quantify the low temperature (i. e. room temperature) diffusional moisture release to complete our universal moisture outgassing model for silica-filled silicones from low temperatures to high temperatures.
Fermi National Accelerator Laboratory (Fermilab) is a world leader in designing and operating particle accelerators for nuclear and particle physics research. These accelerators rely on electric fields to propel particle beams, which are then directed and focused using magnetic fields. To ensure these beams travel without interference, they must move through an ultra-high vacuum environment, typically around 10⁻⁹ torr. Maintaining such a vacuum requires materials with exceptionally low outgassing rates. 316L stainless steel is a common material choice for vacuum systems due to its low outgassing rates, excellent corrosion resistance, non-magnetic properties, and high mechanical strength. When manufactured using traditional methods like machining, extrusion, and casting, the vacuum properties of 316L stainless steel are well understood. However, the behavior of 316L stainless steel produced through additive manufacturing, such as Direct Metal Laser Sintering (DMLS), is not as well documented. This study aims to determine the outgassing rate of 316L stainless steel fabricated using DMLS. The investigation focuses on measuring the outgassing rates of 1.5 2 vacuum reducers and evaluating the effects of surface preparation techniques, such as mechanical polishing and electropolishing, on the outgassing performance. Understanding the outgassing performance of 3D-printed 316L stainless steel could enable Fermilab engineers to adopt this fabrication method for producing complex parts designed for ultra-high vacuum environments. These advancements have the potential to benefit projects, such as the Long-Baseline Neutrino Facility (LBNF) and the Proton Improvement Plan-II (PIP-II), by improving design flexibility and fostering innovation in accelerator development.
Standardized techniques for outgassing tests are developed and set forth for use in the screening of materials for aerospace instruments with cooled sensors, optics, and/or detectors. Materials for optical instruments are discussed in terms of molecular outgassing, and material-outgassing test results are presented which relate to several test conditions. The existing outgassing standard is found to be inadequate, and revised outgassing standards related to four application levels are given. The test protocols are designed for the development of materials for optical instruments that operate in environments with temperatures below 20 C. Consideration is also given to potential molecular contamination in the space environment and to outgas screening of instruments with a variety of sensor/optics/detector temperatures. The standards are designed for use with existing outgassing-test data as well as contamination analyses relating to the instrument being tested.
As a laboratory for scientific research, the International Space Station has been in Low Earth Orbit for nearly 20 years and is expected to be on-orbit for another 10 years. The ISS has been maintaining a relatively pristine contamination environment for science payloads. Materials outgassing induced contamination is currently the dominant source for sensitive surfaces on ISS and modeling the outgassing rate decay over a 20 to 30 year period is challenging. Materials outgassing is described herein as a diffusion-reaction process using ASTM E 1559 rate data. The observation of -1/2 (diffusion) or non-integers (reaction limited) as rate decay exponents for common ISS materials indicate classical reaction kinetics is unsatisfactory in modeling materials outgassing. Non-randomness of reactant concentrations at the interface is the source of this deviation from classical reaction kinetics. A diffusion limited decay was adopted as the result of the correlation of the contaminant layer thicknesses on returned ISS hardware, the existence of high outgassing silicone exhibiting near diffusion limited decay, and the confirmation of non-depleted material after ten years in the Low Earth Orbit.Keywords: Materials Outgassing, ASTM E 1559, Reaction Kinetics, Diffusion, Space Environments Effects, Contamination
The arrival of the Nanoracks Airlock to the International Space Station (ISS) has provided the ISS program the capability to dispose of common trash items. The concept of operations involved the crew bagging up those items into a trash bag and then utilizing the robotic arm and the airlock to jettison the trash bag. Because of the unknown thermal vacuum stability of some of the items, a molecular contamination concern was raised by the ISS program as the trash is exposed to vacuum upon the evacuation of air from the airlock and the robotic arm moving the airlock to its jettison location. In order to characterize the representative outgassing rates for ISS trash, thermal vacuum testing was performed at White Sands Test Facility. Trash was sorted into a “lower” outgassing bag and a “mixed” bag. The “mixed” trash bag contained more items that were suspected to be not vacuum stable. Load cells were chosen as the primary means for measuring mass loss. A sharp decay in the outgassing rate was observed in the first 30 minutes followed by a slower decay. As expected, the “mixed” bag lost more mass. While Quartz Crystal Microbalances (QCMs) are often utilized to measure long term outgassing rates and the sticking coefficients of contaminants at different operating temperatures for vacuum stable materials, these measurements proved difficult due to the amount and the inclusion of materials with suspect thermal vacuum stability. Because of high rates of material outgassing, the facility was unable to maintain the CQCM temperature setpoint of 80 K QCMs.. The QCMs operating at the warmer temperatures also saturated on occasion due to high levels of condensed matter. Though testing was able to confirm high risk of outgassing contamination for the program, true sticking coefficients could not be determined, available measurements are provided herein.
Earth's atmosphere, crust and mantle have evolved together through continuous geochemical exchange throughout Earth's history. Constraints on the transport of volatile elements and compounds between these reservoirs are crucial for understanding how Earth could have stayed habitable for extended periods of time. In this work, we present a new forward model of He, Ne and Ar in the mantle, crust and atmosphere. We explore concentrations of noble gases at the end of accretion, bulk silicate Earth K/U ratios, crustal growth scenarios, and upper mantle processing rates throughout Earth's history. We search for parameter combinations that simultaneously satisfy observational constraints on present-day mantle 4 He/ 3 He and 40 Ar/ 36 Ar (sensitive to mantle outgassing and continental crust growth, which depletes the mantle of U, Th and K), atmospheric 20 Ne/ 22 Ne (which tracks the mix of outgassed vs. delivered Ne in the atmosphere), and atmospheric 40 Ar/ 36 Ar in the past and today (sensitive to volatile delivery, mantle outgassing and crustal growth). Leveraging this intertwined set of noble gas abundances and isotopic compositions yields new constraints on initial noble gas abundances in the mantle and on the proportions of atmospheric volatiles originating from delivery by impact degassing, mantle outgassing, and degassing of the continental crust. We find that atmospheric Ar isotopic evolution is primarily sensitive to the mantle processing rate history; the atmospheric Ar isotopic record should therefore not be used to reconstruct continental crust growth, but instead provides valuable insights into mantle processing rates. Our model predicts a measurably low 20 Ne/ 22 Ne ratio of ~9.7 in Archean atmospheric samples. Most of atmospheric primordial 36 Ar was directly delivered by chondritic bodies and not transferred to the atmosphere during an intense early episode of mantle outgassing. Nitrogen delivered by impact degassing could account for the present-day atmospheric nitrogen inventory.
Background Extreme ultraviolet (EUV) photoresists play a pivotal role in advancing nanopatterning technologies by balancing image quality and sensitivity. The outgassing behavior of photoresist thin films under EUV and deep ultraviolet (DUV) exposure reveals chemical details relevant to their performance. Aim Here, we focus on utilizing an analytical technique not previously used in photolithography, the tabletop cavity ring-down spectrometer, to investigate outgassing dynamics in EUV photoresists, enabling precise chemical identification and deeper insights into resist processing. Approach The spectrometer’s enhanced laser path length (∼ 20 km) and broadband absorption capabilities in the C–H overtone region allow for sensitive and temporally resolved detection of mixtures of outgassed species. Using a model resist comprising a polymer matrix with a photoacid generator and quencher, we analyzed the influence of time delays between exposure and post-exposure bake (PEB) as well as storage under varying environmental conditions. Results Suppression of isobutylene outgassing and thickness loss was observed with extended delays between exposure and PEB, potentially linked to water absorption and acid deactivation. The technique proved highly effective in distinguishing subtle chemical differences between processing stages. Conclusions Delay times and their environmental conditions, particularly humidity, reduce outgassing and thickness loss of photoresists during PEB, suggesting decreased acid-driven deprotection. This can potentially impact sensitivity, defectivity, and roughness of resist patterns, necessitating precise monitoring and control.
Extreme ultraviolet (EUV) photoresists play a pivotal role in advancing nanopatterning technologies by balancing image quality and sensitivity. The outgassing behavior of photoresist thin films under EUV and deep ultraviolet (DUV) exposure reveals chemical details relevant to their performance. This study focuses on utilizing an analytical technique not previously used in photolithography, the tabletop cavity ring-down spectrometer, to investigate outgassing dynamics in EUV photoresists, enabling precise chemical identification and deeper insights into resist processing. The spectrometer’s enhanced laser path length (~20 km) and broadband absorption capabilities in the CH overtone region allow for sensitive and temporally resolved detection of outgassed species. Using a model resist comprising a polymer matrix with a photoacid generator and quencher, we analyzed the influence of time delays between exposure and Post-Exposure Bake (PEB) as well as storage under varying environmental conditions. Suppression of isobutylene outgassing and thickness loss was observed with extended delays between exposure and PEB, potentially linked to water absorption and acid deactivation. The technique proved highly effective in distinguishing subtle chemical differences between processing stages. Delay times and their environmental conditions, particularly humidity, reduce outgassing and thickness loss of photoresists during PEB, suggesting decreased acid-driven deprotection. This can potentially impact sensitivity, defectivity, and roughness of resist patterns, necessitating precise monitoring and control.
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.
A large amount of chemical analysis data involving identification of outgassing products from spacecraft, experiment modules, and support equipment accumulated at the Goddard Space Flight Center over the past ten years were reduced to a computer compatible format and subjected to a variety of relevant program operations. From these data a list of the most troublesome outgassing species were compiled and several useful and interesting materials' correlations were developed. The frequency of occurrence totals show that in aerospace program, di(2-ethyl hexyl) phthalate (DEHP) is the most often found individual species in outgassing samples and that esters are the leading generic class of compounds. The effectiveness of this data bank was demonstrated by the good correlations between materials and their outgassing products for solar panel bakeouts and cable bakeouts. However, trends in frequency of occurrence of many compounds were demonstrated where no correlation could be established. In the case of the class of compounds called aliphatic hydrocarbons, it is shown that the number of instances of significant outgassing due to these materials is increasing.