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At least 1,477 records · Page 82

Arc jet tests of metallic TPS materials.

Seven thoria dispersed nickel base alloys and one cobalt base alloy, candidates for the Metallic Thermal Protection System for the Space Shuttle Vehicle, were tested simultaneously in an arc jet at a nominal test temperature of 1366 deg K (2000 deg F) and pressure of 0.01 atmospheres. The degradation of the materials after 50 one half-hour cycles in the arc jet simulating Space Shuttle entry conditions was determined utilizing techniques including X-ray diffraction, metallography, and electron beam microprobe.

Centolanzi, F. J.↗

IHE Material and IHE Subassembly Qualification Test Description and Criteria (v. 14.7)

The purpose of the deflagration-to-detonation test is to demonstrate that an IHE material will not undergo deflagration-to-detonation transition (DDT) under stockpile relevant conditions of scale, confinement, and material condition. Inherent in this test design is the assumption that ignition does occur, with onset of deflagration. The test design will incorporate large margins and replicates to account for the stochastic nature of DDT events.

36 MATERIALS SCIENCE↗

Using Isothermal Microcalorimetry to Determine Compatibility of Structural Materials with High-Test Hydrogen Peroxide (HTP) Propellant

High-Test Hydrogen Peroxide (HTP) propellant (equal to or greater than 70%) offers many advantages in space launch applications. However, materials used in construction of propulsion systems must be shown to be compatible with HTP. Isothermal Microcalorimetry (IMC) was used to determine the compatibility of several metallic and non-metallic materials with 90% HTP. The results of these experiments agreed with those from immersion bath tests when the values were converted to % Active Oxygen Loss per week (%AOL/wk).

Gostowski, Rudy↗

Radioactivity Calculator for Research and Test Reactor Neutron-Activated Materials

The Idaho National Laboratory (INL) Nuclear Science User Facility (NSUF) supports nuclear energy-relevant research into the effects of radiation on nuclear fuels and structural materials. The NSUF provides access, at no cost to the researcher, to the Advanced Test Reactor (ATR), the High-Flux Isotope Reactor (HFIR), and other university and national laboratory research and test reactors for radiation effects experiments. Post-irradiation examination of materials poses some difficulties when studying neutron-irradiated materials due to the radioactivity levels of the materials. Inside a test reactor, under high neutron flux, stable materials can activate (capture a neutron) and become unstable or radioactive. These newly created radioactive materials decay, based on their respective half-lives, and emit energetic radiation. Nuclides with short half-lives are able to decay to sufficiently low radiation levels prior to the sample being removed from the reactor. However, nuclides with longer half-lives present a challenge since they must be handled with extreme caution and stored until their radioactivity levels decrease. If immediate examination is required, the examination may take place in a hot cell, which can dramatically increase the cost of the project. The NSUF has access to a variety of hot cells and characterization capabilities at national laboratories, universities, and industrial sites across the United States. In order to estimate the post-irradiation radioactivity levels of materials early in the experiment cycle, we created a radioactivity calculator, hosted on the NSUF web site (nsuf.inl.gov), which will consider three stages of neutron activations and decays for sample materials.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

ETF Grout Expansion: Evaluation of MgO Additions and Struvite Precipitation Protocol for Potential Expansion

The ETF ammonia tolerant grout waste form was developed by the Vitreous State Laboratory (VSL) to stabilize ammonium and thereby prevent emission of ammonia vapor during solidification of an ammonium-rich, concentrated sulfate aqueous waste stream generated at the Hanford Effluent Treatment Facility (ETF). VSL did not observe expansion in samples prepared during the waste form development work. However, Savannah River National Laboratory (SRNL) personnel did encounter expansion, in some cases up to 20+ volume percent expansion in ETF grout samples while preforming work scope to evaluate compositional ranges for ETF brine and of the precipitation and solidification reagent. The work requests can be found in Washington River Protection Services (WRPS) Statement of Work (SOW), Requisitions #: 339922 Revisions 0 and 1, March 11, 2021, and November 2021. Additional evaluation was requested by WRPS SOW Requisitions #: 356730, Revision 1, February 1, 2022, to determine whether differences in the slags or differences in sample preparation protocols used by VSL and SRNL were the cause of the expansion observed in the SRNL samples. G. Chen, WRPS, arranged a materials exchange between VSL and SRNL and coordinated the VSL protocol for grouting and curing 1L of Base Case ETF simulant. Materials were exchanged between VSL and SRNL and both laboratories performed the VSL struvite precipitation-solidification protocol and cured samples for at least 28 days. VSL and SRNL encountered expansion, at varying degrees, in all samples prepared under the material exchange and grouting protocol. Additional material exchange testing between VSL and SRNL and alternative materials evaluation to further investigate the causes of grout expansion and differentiate the effects of various dry materials, grouting procedures, and curing containers was requested by WRPS SOW Requisitions #: 356730, Revision 2, January 10, 2023. Pacific Northwest National Laboratory (PNNL) assembled and distributed materials to both laboratories for testing. Observations from this study indicated variations in MgO additions, water-to-dry mix (dm) ratios and curing containers did not correlate to ETF ammonia grout expansion. In comparison to previous work, SRNL observed the addition rate of NaOH to be a potential factor for the final pH in the struvite precipitation step. In the current testing NaOH was added in bulk (5-10 mL at one time) during the precipitation step. The resulting pH was 7.57-9.15 which is slightly higher than pH observed at a slower addition rate. Additional testing is needed to identify the presence and/or struvite stability in high-pH struvite precipitant ETF ammonia grout samples. Therefore, based on current data, it is unknown if NaOH addition rate is the fundamental cause of grout expansion.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

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.↗

Exit Presentation

Skills Acquired: Tensile Testing: Prepare materials and setting up the tensile tests; Collect and interpret (messy) data. Outgassing Testing: Understand TML (Total Mass Loss) and CVCM (Collected Volatile Condensable Material); Collaboration with other NASA centers. Z2 (NASA's Prototype Space Suit Development) Support: Hands on building mockups of components; Analyze data; Work with others, understanding what both parties need in order to make a run successful. LCVG (Liquid Cooling and Ventilation Garment) Flush and Purge Console: Both formal design and design review process; How to determine which components to use - flow calculations, pressure ratings, size, etc.; Hazard Analysis; How to make design tradeoffs.

Melone, Kate↗

A 6 MW/m 2 High Heat Flux Testing Facility of Irradiated Materials Using Infrared Plasma-Arc Lamps

Assessing the effect of neutron irradiation of plasma-facing materials has been challenging due to both the technical and radiological challenges involved. In an effort to address the radiological challenges, a facility was developed to conduct high heat flux testing (HHFT) of inherently small samples of neutron-irradiated materials. A new line-focus reflector was designed and fabricated at Oak Ridge National Laboratory for a plasma-arc lamp (PAL) to attain a source heat flux of 12 MW/m 2 . The new reflector was fabricated with two ports for monitoring specimen condition during HHFT. At the same operational conditions for PAL, the absorbed heat flux in tungsten was increased from 1.39 MW/m 2 with the uniform irradiance reflector to 5.12 MW/m 2 for the line-focus reflector. This fourfold increase in the heat flux, at the same PAL electrode lifetimes, enabled cost-effective facility operation for a high number of cyclic high heat flux tests. Specifically, the test section is confined to a hemispherical dome, and specimens are bolted directly to a water-cooled copper alloy rod. Temperature measurement in the PAL facility was a main challenge due to a limited line of sight. For the first time in a PAL facility operating at high heat fluxes, the specimen surface temperature was directly measured during HHFT with a pyrometer. Finally, the HHFT data, which were obtained in this upgraded PAL facility, demonstrated the facility readiness for irradiated materials.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

Testing of typical spacecraft materials in a simulated substorm environment

An investigation to determine spacecraft materials characteristics under charging conditions was conducted at the Lewis Research Center substorm simulation facility. The test specimens were spacecraft paints, silvered Teflon, thermal blankets and solar array segments. The samples, ranging in size from 300 to 1,000 sq cm were exposed to monoenergetic electron energies from 2 to 20 keV at a current density of 1 nA sq cm. The samples generally behaved as capacitors with strong voltage gradients at their edges. The charging characteristics of the silvered Teflon, Kapton, and solar cell covers were controlled by the secondary emission characteristics. Insulators that did not discharge were the spacecraft paints and the quartz fiber cloth thermal blanket sample. All other samples did experience discharges when the surface voltage reached -8 to -16 kV. The discharges were photographed. The breakdown voltage for each sample was determined and the average energy lost in the discharge was computed.

Stephens, N. J.↗

Standardization of the carbon-phenolic materials and processes. Vol. 2: Test methods and specifications

Carbon-phenolic composite materials are used in the ablation process in the nozzles of the Space Shuttle Main Engine. The nozzle is lined with carbon cloth-phenolic resin composites. The extreme heat and erosion of the burning propellant are controlled by the carbon-phenolic composite by means of ablation, a heat and mass transfer process in which a large amount of heat is dissipated by sacrificailly removing material from a surface. Phenolic materials ablate with the initial formation of a char. The depth of the char is a function of the heat conduction coefficient of the composite. The char layer is a poor conductor so it protects the underlying phenolic composite from the high heat of the burning propellant. The nozzle component ablative liners (carbon cloth-phenolic resin composites) are tape wrapped, hydroclave and/or autoclave cured, machined and assembled. The tape consists of prepreg broadcloth. The materials flow sheet for the nozzle ablative liners is given. The prepreg is a three component system: phenolic resin, carbon cloth, and carbon filler. This is Volume 2 of the report, Test Methods and Specifications.

Hall, William B.↗

Demonstration of Embedded Sensors in Ceramic Structures

The Transformational Challenge Reactor (TCR) program seeks to demonstrate an advanced 3D printed nuclear reactor core. A binder jet additive manufacturing process is used to fabricate the complex SiC ceramic components of the TCR core. After printing, the components are densified via chemical vapor infiltration (CVI). This process allows complex cavities to be created in which sensors can be placed at strategic locations. Inserting the sensors during the CVI process allows the sensors to be embedded within the component as it is infiltrated. The primary challenge for embedding the sensors is identifying the sensors and sensor sheath materials that can survive the temperatures (>1,000°C) and chemical exposure to H 2 and HCl during CVI. The embedded sensors that are being investigated for use during TCR operation include thermocouples, self-powered neutron detectors, and spatially distributed fiber-optic temperature sensors. This report describes the CVI materials compatibility tests and initial trials for embedding functional sensors. Mo is identified as the most suitable sensor sheath material based on its availability in small diameter tubing, relatively low neutron absorption cross section, and compatibility with H 2 , HCl, and the surrounding SiC matrix at the process temperatures. Amorphous SiO2 fiber-optic samples with Au and Cu metal coatings were successfully embedded in SiC along with bare fibers, although the metal coatings showed some evidence of localized melting during CVI. Initial experiments attempting to embed functional sensors showed that the sensors can be embedded in 3D printed SiC parts, but there are still challenges that must be overcome to ensure that the sensors and sensor sheaths do not fail during CVI. In particular, Nb-sheathed Mo-Nb thermocouples failed at temperatures far lower than expected despite thermodynamic calculations and materials compatibility tests that show the Nb sheath to be compatible with the CVI environment. One potential explanation for the large expansion of the Nb sheath could be related to hydride formation in the lower temperature region of the sheath. Future work will focus on Mo-sheathed thermocouples instead of Nb. The fiberoptic sensors tested during the instrumented experiment broke due to the lack of mechanical protection after their polymer-based coatings were vaporized. Future instrumented experiments will use metal-coated optical fibers for strain sensing to provide additional mechanical protection. However, custom coatings with higher melting points than commercially available Au and Cu might be required. Regardless, fiber-optic sensors are still candidates for spatially distributed temperature measurements since they can be inserted into an embedded metal sheath after CVI.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

Polymers in solar energy utilization

A laser photoacoustic technique (LPAT) has been verified for performing accelerated life testing of outdoor photooxidation of polymeric materials used in solar energy applications. Samples of the material under test are placed in a chamber with a sensitive microphone, then exposed to chopped laser radiation. The sample absorbs the light and converts it to heat by a nonradiative deexcitation process, thereby reducing pressure fluctuations within the cell. The acoustic signal detected by the microphone is directly proportional to the amount of light absorbed by the specimen. Tests were performed with samples of ethylene/methylacrylate copolymer (EMA) reprecipitated from hot cyclohexane, compressed, and molded into thin (25-50 microns) films. The films were exposed outdoors and sampled by LPAT weekly. The linearity of the light absorbed with respect to the acoustic signal was verified.Correlations were established between the photoacoustic behavior of the materials aged outdoors and the same kinds of samples cooled and heated in a controlled environment reactor. The reactor tests were validated for predicting outdoor exosures up to 55 days.

Liang, R. H.↗

Convective Heat Transfer Scaling of Ignition Delay and Burning Rate with Heat Flux and Stretch Rate in the Equivalent Low Stretch Apparatus

To better evaluate the buoyant contributions to the convective cooling (or heating) inherent in normal-gravity material flammability test methods, we derive a convective heat transfer correlation that can be used to account for the forced convective stretch effects on the net radiant heat flux for both ignition delay time and burning rate. The Equivalent Low Stretch Apparatus (ELSA) uses an inverted cone heater to minimize buoyant effects while at the same time providing a forced stagnation flow on the sample, which ignites and burns as a ceiling fire. Ignition delay and burning rate data is correlated with incident heat flux and convective heat transfer and compared to results from other test methods and fuel geometries using similarity to determine the equivalent stretch rates and thus convective cooling (or heating) rates for those geometries. With this correlation methodology, buoyant effects inherent in normal gravity material flammability test methods can be estimated, to better apply the test results to low stretch environments relevant to spacecraft material selection.

Olson, Sandra↗

Development of a Robust Reference Electrode in Aggressive Chemical and Radiation Environments in the Hanford Waste Tanks

The Hanford site stores more than 200 million liters of radioactive and chemically hazardous wastes from the production of weapons materials. The wastes are stored in 177 underground carbon-steel storage tanks, separated between 149 single shell tanks (SSTs) and 28 double shell tanks (DSTs). The DSTs provide critical retrieval and interim storage before the waste is vitrified in the Waste Treatment and Isolation Plant (WTP). The tanks will need to remain in-service far beyond the initial 40-year design life, and effective corrosion control practices must remain in force to extend the tanks’ lifespans. This effort includes direct measurements of corrosion rate (e.g., ultrasonic measurements and corrosion coupons) and electrochemical processes (e.g., linear polarization measurements and open circuit potential measurements). The Hanford site began monitoring the corrosion potential in select DSTs in 2008. Of the 45 reference electrodes that have been installed, 29 have failed and 6 others provided unreliable results. DOE-EM is supporting a 3-year program to develop a chemical and radiation resistant reference electrode for application in the Hanford tanks. The first year of the program focused on understanding the failure mechanism for the reference electrodes and identification of candidate construction materials that would mitigate degradation of the electrodes in the waste environment. During the second year of the program, the objectives were to: 1) test candidate materials under simulated waste conditions, 2) design components that will extend the service life of the electrode, 3) fabricate materials for prototype reference electrodes, and 4) assemble prototype reference electrodes for accelerated testing. The reference electrode is constructed of four principal parts: 1) junction, 2) casing, 3) inner chamber backfill materials, and 4) the sensing wire. Principally, improvements of the junction, casing, and inner chamber backfill materials are being pursued. The junction material at the interface between the waste and the inner chamber of the reference electrode was identified as a critical component in the failure of the reference electrodes. Nine candidate replacement junction materials were tested under simulated waste conditions to evaluate permeation rate. These materials included a variety of polymeric and ceramic materials, some of which were 3-D printed. Thus far, porous polyvinylidene fluoride materials have performed satisfactorily and are being considered for prototype development. The commercial electrode casing materials in general have performed well. Additionally, 3-D printing of chemically and mechanically stable materials is being investigated as a means for further improvement in fabrication consistency. SRNL has also investigated altering the reference electrode design to extend the service life. The new design of the interior of the reference electrode casing creates a longer, more tortuous path between the junction material and the electrode sensing wire. A finite element model was used to optimize the design without adversely impacting the circuit resistance of the electrode during the measurements, thus preserving the measurement accuracy while enhancing the service life. The inner chamber back fill materials are also critical to the performance of the reference electrode. Materials that are resistant to intruding tank waste and provide a conductive path to the sensing wire were investigated. Gel and powder materials that are interspersed with a conductive chloride bearing material were tested for their influence on diffusion and electrode resistance. All the investigated materials and components will be assembled, with collaboration from commercial vendors, to fabricate the initial prototypes. Accelerated testing of the prototypes will be initiated in Year 2 of the program and will be completed in Year 3. A recommendation on the materials of construction and the design of the new robust reference electrode will be presented to the Hanford tank farm facility.

Sykes, Kiana [Savannah River National Laboratory (↗

New Tools for Automating Arcjet Sample Recession Tracking and Analysis

Arcjet Computer Vision (arcjetCV) has been significantly upgraded to enhance accuracy and performance in tracking material recession and shock-material standoff in test videos. These improvements include integrating new machine learning models, developing a specialized edge detection class, and incorporating a more comprehensive training dataset. These upgrades have refined the software’s ability to automate time-resolved recession tracking, making it more precise and reliable for analyzing complex physical processes. In parallel, a new tool called STARscan (Spatial Targeting and Alignment Rig for Scanning) is being developed to capture detailed 3D surface data before and after testing. By comparing these pre- and post-test scans with arcjetCV’s automated video analysis results, users can achieve a more comprehensive assessment of material recession. This method enables cross-validation of results, improving confidence in the analysis of tested materials. The expanded capabilities of arcjetCV have been successfully demonstrated on videos from various facilities, including the NASA Ames arcjets, UIUC’s PlasmatronX, and the VKI Plasmatron. It has been adopted as a new standard for in-situ recession tracking by the Mars Sample Return Project and Orion. ArcjetCV’s improved efficiency and accuracy are critical for reducing testing uncertainties and validating heatshield material performance under extreme conditions. The software’s user-friendly graphical interface ensures ease of use, enabling seamless processing and precise analysis of arcjet videos, providing deeper insights into material behavior in hypersonic environments. ArcjetCV is now available on both PyPI and Conda, allowing easy installation via "pip install arcjetCV" or through the Conda package manager, ensuring broad accessibility and streamlined deployment for users across various platforms.

Ablation↗

A study of the effects of long-term exposure to fuels and fluids on the behavior of advanced composite materials

The periodic testing and evaluation of graphite/epoxy and Kevlar/epoxy material systems after subjecting test specimens to prolonged exposure to several laboratory-controlled environments deemed typical of normal aircraft operations is discussed. It is noted that specimen immersion in water or water-based fluids resulted in the greatest effect on the mechanical properties tested. Also, the environmental fluids showed a tendency to affect Kevlar/epoxy systems at an earlier exposure period than the graphite/epoxy systems. Results also indicate mechanical property strength retention generally being lower for the Kevlar/epoxy systems when compared to the corresponding graphite/epoxy systems in similar environments, after prolonged exposure.

Tanimoto, E. Y.↗

Assessing potential induced radioactivity in materials processed with X-ray energy above 5 MeV: Assessment protocols and practical experience

In accordance with ISO11137-1 section 5.1.2, ‘the potential for induced radioactivity in product shall be assessed’. This article describes how compliance to this requirement may be achieved using qualified test methods. Materials of consideration are conceptually discussed. Results of testing conducted on products processed with a 7.5 MeV X-ray irradiation process are provided. As X-ray becomes more widely used in healthcare sterilization, having standard assessment protocols for activation coupled with a shared database of material test results will benefit all healthcare product manufacturers seeking to avail of this innovative technology.

Kroc, Thomas K.↗

Assessment of Technologies for the Space Shuttle External Tank Thermal Protection System and Recommendations for Technology Improvement - Part III: Material Property Characterization, Analysis, and Test Methods

The objective of this report is to contribute to the independent assessment of the Space Shuttle External Tank Foam Material. This report specifically addresses material modeling, characterization testing, data reduction methods, and data pedigree. A brief description of the External Tank foam materials, locations, and standard failure modes is provided to develop suitable background information. A review of mechanics based analysis methods from the open literature is used to provide an assessment of the state-of-the-art in material modeling of closed cell foams. Further, this report assesses the existing material property database and investigates sources of material property variability. The report presents identified deficiencies in testing methods and procedures, recommendations for additional testing as required, identification of near-term improvements that should be pursued, and long-term capabilities or enhancements that should be developed.

Gates, Thomas S.↗