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Oxygen Compatibility Testing of Composite Materials

The development of polymer composite liquid oxygen LO2 tanks is a critical step in creating the next generation of launch vehicles. Future launch vehicles need to minimize the gross liftoff weight (GLOW), which is possible due to the 25%-40% reduction in weight that composite materials could provide over current aluminum technology. Although a composite LO2 tank makes these weight savings feasible, composite materials have not historically been viewed as "LO2 compatible." To be considered LO2 compatible, materials must be selected that will resist any type of detrimental, combustible reaction when exposed to usage environments. This is traditionally evaluated using a standard set of tests. However, materials that do not pass the standard tests can be shown to be safe for a particular application. This paper documents the approach and results of a joint NASA/Lockheed Martin program to select and verify LO2 compatible composite materials for liquid oxygen fuel tanks. The test approach developed included tests such as mechanical impact, particle impact, puncture, electrostatic discharge, friction, and pyrotechnic shock. These tests showed that composite liquid oxygen tanks are indeed feasible for future launch vehicles.

Graf, Neil A.

Polymer Matrix Composite Material Oxygen Compatibility

Carbon fiber/polymer matrix composite materials look promising as a material to construct liquid oxygen (LOX) tanks. Based on mechanical impact tests the risk will be greater than aluminum, however, the risk can probably be managed to an acceptable level. Proper tank design and operation can minimize risk. A risk assessment (hazard analysis) will be used to determine the overall acceptability for using polymer matrix composite materials.

Owens, Tom

Promoted-Ignition Testing to Determine the Gaseous Oxygen Compatibility of the Intermetallic Compound 60-NITINOL

The flammability of 60-NITINOL (60 weight percentage Ni and 40 weight percentage Ti) in an oxygen-rich atmosphere is assessed. It is determined that 60-NITINOL burns readily in gaseous oxygen and would not be a good candidate for components exposed to oxygen-rich environments where there may be an ignition source. The results are the same whether the material is tested without heat treatment, after a solution treatment or after furnace annealing. These results provide guidance for materials selection of aerospace turbomachinery components.

intermetallics

Liquid-oxygen compatible, flame-resistant coating.

Polychloroprene rubber composition, using commercially available components, exhibits superior extrusion and durability and is highly flame and corrosion resistant. Material experiences major applications in fields of aeronautics and safety.

Bright, C. W.

Elastomers Compatible With High-Pressure Oxygen

Compatibility increased by fluorination. Report describes experiments aimed at improving compatibility of some fluorinated elastomers with high-pressure oxygen. Such elastomers needed for seals, gaskets, and positive-expulsion devices used with high-pressure oxygen. Oxygen - compatibility tests carried out on five elastomers chosen on the basis of literature survey.

Martin, Jon W.

Materials Safety - Not just Flammability and Toxic Offgassing

For many years, the safety community has focused on a limited subset of materials and processes requirements as key to safety: Materials flammability, Toxic offgassing, Propellant compatibility, Oxygen compatibility, and Stress-corrosion cracking. All these items are important, but the exclusive focus on these items neglects many other items that are equally important to materials safety. Examples include (but are not limited to): 1. Materials process control -- proper qualification and execution of manufacturing processes such as structural adhesive bonding, welding, and forging are crucial to materials safety. Limitation of discussions on materials process control to an arbitrary subset of processes, known as "critical processes" is a mistake, because any process where the quality of the product cannot be verified by inspection can potentially result in unsafe hardware 2 Materials structural design allowables -- development of valid design allowables when none exist in the literature requires extensive testing of multiple lots of materials and is extremely expensive. But, without valid allowables, structural analysis cannot verify structural safety 3. Corrosion control -- All forms of corrosion, not just stress corrosion, can affect structural integrity of hardware 4. Contamination control during ground processing -- contamination control is critical to manufacturing processes such as adhesive bonding and also to elimination foreign objects and debris (FOD) that are hazardous to the crew of manned spacecraft in microgravity environments. 5. Fasteners -- Fastener design, the use of verifiable secondary locking features, and proper verification of fastener torque are essential for proper structural performance This presentation discusses some of these key factors and the importance of considering them in ensuring the safety of space hardware.

Pedley, Michael D.

Elastomer Compatible With Oxygen

Artificial rubber resists ignition on impact and seals at low temperatures. Filled fluoroelastomer called "Katiflex" developed for use in seals of vessels holding cold liquid and gaseous oxygen. New material more compatible with liquid oxygen than polytetrafluoroethylene. Provides dynamic seal at -196 degrees C with only 4 times seal stress required at room temperature. In contrast, conventional rubber seals burn or explode on impact in high-pressure oxygen, and turn hard or even brittle at liquid-oxygen temperatures, do not seal reliably, also see (MFS-28124).

Martin, Jon W.

Liquid oxygen LOX compatibility evaluations of aluminum lithium (Al-Li) alloys: Investigation of the Alcoa 2090 and MMC weldalite 049 alloys

The behavior of liquid oxygen (LOX) compatibility of aluminum lithium (Al-Li) alloys is investigated. Alloy systems of Alcoa 2090, vintages 1 to 3, and of Martin Marietta Corporation (MMC) Weldalite 049 were evaluated for their behavior related to the LOX compatibility employing liquid oxygen impact test conditions under ambient pressures and up to 1000 psi. The developments of these aluminum lithium alloys are of critical and significant interest because of their lower densities and higher specific strengths and improved mechanical properties at cryogenic temperatures. Of the different LOX impact tests carried out at the Marshall Space Flight Center (MSFC), it is seen that in certain test conditions at higher pressures, not all Al-Li alloys are LOX compatible. In case of any reactivity, it appears that lithium makes the material more sensitive at grain boundaries due to microstructural inhomogeneities and associated precipitate free zones (PFZ). The objectives were to identify and rationalize the microstructural mechanisms that could be relaxed to LOX compatibility behavior of the alloy system in consideration. The LOX compatibility behavior of Al-Li 2090 and Weldalite 049 is analyzed in detail using microstructural characterization techniques with light optical metallography, scanning electron microscopy (SEM), electron microprobe analysis, and surface studies using secondary ion mass spectrometry (SIMS), electron spectroscopy in chemical analysis (ESCA) and Auger electron spectroscopy (AES). Differences in the behavior of these aluminum lithium alloys are assessed and related to their chemistry, heat treatment conditions, and microstructural effects.

Diwan, Ravinder M.

Joint Test Report For Validation of Alternatives to Aliphatic Isocyanate Polyurethanes

National Aeronautics and Space Administration (NASA) and Air Force Space Command (AFSPC) have similar missions and therefore similar facilities and structures in similar environments. The standard practice for protecting metallic substrates in atmospheric environments is the application of an applied coating system. The most common topcoats used in coating systems are polyurethanes that contain isocyanates. Isocyanates are classified as potential human carcinogens and are known to cause cancer in animals. The primary objective of this effort was to demonstrate and validate alternatives to aliphatic isocyanate polyurethanes resulting in one or more isocyanate-free coatings qualified for use at AFSPC and NASA installations participating in this project. This joint Test Report (JTR) documents the results of the laboratory and field testing as well as any test modifications made during the execution of the testing. The technical stakeholders agreed upon test procedure modifications documented in this document. This JTR is made available as a reference for future pollution prevention endeavors by other NASA centers, the Department of Defense and commercial users to minimize duplication of effort. All coating system candidates were tested using approved NASA and AFSPC standard coating systems as experimental controls. This study looked at eight alternative coating systems and two control coating systems and was divided into Phase I Screening Tests, Phase II Tests, and Field Testing. The Phase I Screening Tests were preliminary tests performed on all the selected candidate coating systems. Candidate coating systems that did not meet the acceptance criteria of the screening tests were eliminated from further testing. Phase I Screening Tests included: Ease of Application, Surface Appearance, Dry-To-Touch (Sanding), Accelerated Storage Stability, Pot Life (Viscosity), Cure Time (Solvent Rubs), Cleanability, Knife Test, Tensile (pull-off) Adhesion, and X-Cut Adhesion by Wet Tape After a review of the Phase I test results, four of the alternative coating systems showed substandard performance in relation to the Control Systems and were eliminated from the Phase II testing. Due to the interest of stakeholders and time constraints, however, all eight alternatives were subjected to the following Phase II tests, along with field testing at Stennis Space Center (SSC), Mississippi: Hypergol Compatibility, Liquid Oxygen Compatibility, 18-Month Marine Exposure (Gloss Retention, Color Retention, Blistering, Visual Corrosion, Creepage from Scribe, Heat Adhesion), and Field Exposure (6- and 12-month Evaluation for Coating Condition, Color Retention, Gloss Retention). The remaining four alternative coating systems determined to be the best viable alternatives were carried on to Phase II testing that included: Removability, Repairability, Abrasion Resistance, Gravelometer, Fungus Resistance, Accelerated Weathering, Mandrel Bend Flexibility, and Cyclic Corrosion Resistance. Of the systems that continued to Phase II, three (3) alternative coating systems meet the performance requirements as identified by stakeholders. Two (2) other systems, that were not included in Phase II testing, performed well enough on the 18-Month Marine Exposure, the primary requirement for NASA technical standard NASA-STD-5008, Protective Coating of Carbon Steel, Stainless Steel, and Aluminum on Launch Structures, Facilities, and Ground Support Equipment, that they were also considered to be successful candidates. In total, five (5) alternative coating systems were approved for inclusion in the NASA-STD- 5008 Qualified Products List (QPL). The standard is intended to provide a common framework for consistent practices across NASA and is often used by other entities. The standard's QPL does not connote endorsement of the products by NASA, but lists those products that have been tested and meet the requirements as specified.

Lewis, Pattie

Composites for Cryotank Structures. Present and Future: MSFC Perspective

The development of reusable launch vehicle systems for a single stage to orbit vehicle requires vehicles at liftoff with 85% to 94% of its mass consisting exclusively of propellants. These dry mass requirements drive designs to utilize stronger, lighter weight materials for structures. This technology development focus has allowed the introduction of composite materials in lieu of conventional metallic materials due to their higher specific strengths. Composite materials were successfully used for the liquid hydrogen tanks for the DC-XA, and a multi-lobed liquid hydrogen tank will be employed for the X-33. Another potential non-traditional application for composite materials is for liquid oxygen tanks, which is still being investigated. Traditionally, organic materials have been avoided wherever possible, due the potential fire hazard and the fact that composites fail conventional oxygen compatibility requirements. However, the potential weight savings warrant the investigation of the use of polymeric composite materials in oxygen environments. Since composites fail the conventional, time-proven test methods because they are considered flammable by test, we have embarked on an innovative approach to oxygen compatibility testing and evaluation focused on the use environments and attempts to eliminate or "design away" all potential ignition sources. Oxygen compatibility is defined as the ability of a material to coexist with oxygen and potential ignition sources with an acceptable, manageable degree of risk.

Vaughn, Timothy P.

A survey of compatibility of materials with high pressure oxygen service.

The literature on high pressure oxygen compatibility has been surveyed in order to present the existing state of knowledge. Searches have been conducted of NASA and NBS data retrieval systems. In addition, many individuals, active in the field, were contacted in order to retrieve useful unpublished information. Compatibility data, such as mechanical impact, pneumatic impact, ignition temperature, and flash-and-fire point, were compiled for pressures above 200 bar. Lower pressure data were included if they were useful for extrapolation to pressures above 200 bar. These data, too numerous to be given here, are available from the authors. Brief descriptions of the trends of these data are given. Recommendations for additional high pressure studies are included.

Hust, J. G.

Small ultrahigh vacuum compatible hyperthermal oxygen atom generator

The development of a compact, ultrahigh vacuum (UHV) compatible instrument for generating a flux of pure hyperthermal oxygen atoms for NASA applications has been achieved. The instrument combines the mechanisms of O2 dissociation and transport through a hot Ag membrane to provide a continuous source of O atoms to a vacuum interface where they are subsequently emitted into the vacuum space by electron-stimulated desorption (ESD). A flux of neutral O atoms 4.5 X 10(exp 13) cm(exp-2) s(exp-l)(P-3) with a mean ion kinetic energy of approximately 5eV and a full width at half maximum of 4eV was detected at a quadrupole mass spectrometer located 10 cm away. The geometry of the instrument is such that it is mounted on a 7 cm flange and can be tailored in length and orientation to fit most UHV systems. The data presented here are for ESD-controlled conditions where increases in the flux are strictly linear with electron bombardment current. Calculation shows that transport-controlled conditions can be achieved at temperatures as low as 350 C with membrane thicknesses on the order of 10 micron.

Outlaw, R. A.

Replacement of Hydrochlorofluorocarbon (HCFC) -225 Solvent for Cleaning and Verification Sampling of NASA Propulsion Oxygen Systems Hardware, Ground Support Equipment, and Associated Test Systems

Since the 1990's, when the Class I Ozone Depleting Substance (ODS) chlorofluorocarbon-113 (CFC-113) was banned, NASA's rocket propulsion test facilities at Marshall Space Flight Center (MSFC) and Stennis Space Center (SSC) have relied upon hydrochlorofluorocarbon-225 (HCFC-225) to safely clean and verify the cleanliness of large scale propulsion oxygen systems. Effective January 1, 2015, the production, import, export, and new use of HCFC-225, a Class II ODS, was prohibited by the Clean Air Act. In 2012 through 2014, leveraging resources from both the NASA Rocket Propulsion Test Program and the Defense Logistics Agency - Aviation Hazardous Minimization and Green Products Branch, test labs at MSFC, SSC, and Johnson Space Center's White Sands Test Facility (WSTF) collaborated to seek out, test, and qualify a replacement for HCFC-225 that is both an effective cleaner and safe for use with oxygen systems. Candidate solvents were selected and a test plan was developed following the guidelines of ASTM G127, Standard Guide for the Selection of Cleaning Agents for Oxygen Systems. Solvents were evaluated for materials compatibility, oxygen compatibility, cleaning effectiveness, and suitability for use in cleanliness verification and field cleaning operations. Two solvents were determined to be acceptable for cleaning oxygen systems and one was chosen for implementation at NASA's rocket propulsion test facilities. The test program and results are summarized. This project also demonstrated the benefits of cross-agency collaboration in a time of limited resources.

Mitchell, Mark A.

Replacement of HCFC-225 Solvent for Cleaning NASA Propulsion Oxygen Systems

Since the 1990's, when the Class I Ozone Depleting Substance (ODS) chlorofluorocarbon‐113 (CFC‐113) was banned, NASA's rocket propulsion test facilities at Marshall Space Flight Center (MSFC) and Stennis Space Center (SSC) have relied upon hydrochlorofluorocarbon‐225 (HCFC‐225) to safely clean and verify the cleanliness of large scale propulsion oxygen systems. Effective January 1, 2015, the production, import, export, and new use of HCFC‐225, a Class II ODS, was prohibited by the Clean Air Act. In 2012 through 2014, leveraging resources from both the NASA Rocket Propulsion Test Program and the Defense Logistics Agency ‐ Aviation Hazardous Minimization and Green Products Branch, test labs at MSFC, SSC, and Johnson Space Center's White Sands Test Facility (WSTF) collaborated to seek out, test, and qualify a replacement for HCFC‐225 that is both an effective cleaner and safe for use with oxygen systems. Candidate solvents were selected and a test plan was developed following the guidelines of ASTM G127, Standard Guide for the Selection of Cleaning Agents for Oxygen Systems. Solvents were evaluated for materials compatibility, oxygen compatibility, cleaning effectiveness, and suitability for use in cleanliness verification and field cleaning operations. Two solvents were determined to be acceptable for cleaning oxygen systems and one was chosen for implementation at NASA's rocket propulsion test facilities. The test program and results are summarized. This project also demonstrated the benefits of cross‐agency collaboration in a time of limited resources.

Mitchell, Mark A.

Orbit transfer rocket engine technology program: Oxygen materials compatibility testing

Particle impact and frictional heating tests of metals in high pressure oxygen, are conducted in support of the design of an advanced rocket engine oxygen turbopump. Materials having a wide range of thermodynamic properties including heat of combustion and thermal diffusivity were compared in their resistance to ignition and sustained burning. Copper, nickel and their alloys were found superior to iron based and stainless steel alloys. Some materials became more difficult to ignite as oxygen pressure was increased from 7 to 21 MPa (1000 to 3000 psia).

Schoenman, Leonard

Promoted Combustion Behavior of 316 Stainless Steel and 6061 Aluminum Alloys in Elevated Pressure Nitrox Environments

Promoted combustion testing (outlined in the ASTM G124 “Standard Test Method for Determining the Combustion Behavior of Metallic Materials in Oxygen Enriched Atmospheres”) refers to a useful testing method to evaluate how metallic materials will behave when combusted in environments with high oxygen concentrations, elevated pressure, or both. These tests yield data which is useful for engineers and scientists from a variety of industries who need and rely on oxygen systems. Oxygen Compatibility Assessments (OCA’s) are vital for ensuring that materials will be safe for use, and these assessments rely on data from OCA’s or interpolation if a desired pressure/concentration is outside of previously tested bounds. It was identified that these bounds leave out significant areas of data for materials which are tested at high pressures (above 1500 psi) and variable oxygen concentrations (with nitrogen as the diluent gas). For this reason, the authors posited that conducting promoted combustion testing on materials above 1500 psi and in various concentrations of oxygen would be incredibly useful in future analyses for oxygen compatibility with similar environments (such as breathing air) as well as for further understanding of how materials behave at very high pressures (such as 10000 psi). Two materials were selected which are commonly used in industry today - 316 stainless steel and 6061 aluminum – and they were tested and analyzed for the purposes of this study.

oxygen compatibility

Update: Evaluation of Additively Manufactured Metals for Use in Oxygen Systems

Evaluation of Additively Manufactured Metals for Use in Oxygen Systems. Oxygen Compatibility: Additive Manufacturing (AM) is currently and will continue to be, used in oxygen systems; Compatibility studies are a necessity; Risks if not pursued - Equipment Damage, Loss of Mission, Loss of Life; NASA Centers of Excellence leading efforts -White Sands Test Facility (WSTF), Oxygen Compatibility Testing -Marshall Space Flight Center (MSFC), Additive Manufacturing -Glenn Research Center, Metals characterization -NASA Engineering Safety Center (NESC), Statistical Design of Experiments.

Tylka, Jonathan