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Resistance of sample is measured with aid of usual electrical test instruments applied to electrical contacts provided at ram and anvil assemblies. Temperature differential is established between ram and anvil for measurement of Seebeck coefficient. Voltage generated across sample is detected at electrical contacts.
This paper describes measurements which were performed on a sample of radome material in the Electromagnetic Properties Measurements Laboratory (EPML). The purpose of the measurements described in this paper was to determine the one-way transmission loss through the flat panel of radome material for a frequency range of 84 to 94 GHz, for varying incidence angles. The panel, which was manufactured by Norton Performance Plastics Corporation, was provided to the EPML by TRW. The size of the panel is 40 in x 36 in x 0.422 in and consists of a foam material with one side coated with a smooth white coating (this side will be referred to as the front side). The dielectric properties of the foam material from the inside of the panel were also determined at X-band (8.2-12.4 GHz). The W-band free space measurements are presented first, followed by the X-band dielectric properties measurements.
The development of high temperature containerless processing equipment and the design and evaluation of associated systems required for microgravity materials processing and property measurements are discussed. Efforts were directed towards the following task areas: design and development of a High Temperature Acoustic Levitator (HAL) for containerless processing and property measurements at high temperatures; testing of the HAL module to establish this technology for use as a positioning device for microgravity uses; construction and evaluation of a brassboard hot wall Acoustic Levitation Furnace; construction and evaluation of a noncontact temperature measurement (NCTM) system based on AGEMA thermal imaging camera; construction of a prototype Division of Amplitude Polarimetric Pyrometer for NCTM of levitated specimens; evaluation of and recommendations for techniques to control contamination in containerless materials processing chambers; and evaluation of techniques for heating specimens to high temperatures for containerless materials experimentation.
Scanning transmission electron microscopy (STEM) allows for imaging, diffraction, and spectroscopy of materials on length scales ranging from microns to atoms. By using a high-speed, direct electron detector, it is now possible to record a full two-dimensional (2D) image of the diffracted electron beam at each probe position, typically a 2D grid of probe positions. These 4D-STEM datasets are rich in information, including signatures of the local structure, orientation, deformation, electromagnetic fields, and other sample-dependent properties. However, extracting this information requires complex analysis pipelines that include data wrangling, calibration, analysis, and visualization, all while maintaining robustness against imaging distortions and artifacts. In this paper, we present py4DSTEM, an analysis toolkit for measuring material properties from 4D-STEM datasets, written in the Python language and released with an open-source license. We describe the algorithmic steps for dataset calibration and various 4D-STEM property measurements in detail and present results from several experimental datasets. We also implement a simple and universal file format appropriate for electron microscopy data in py4DSTEM, which uses the open-source HDF5 standard. We hope this tool will benefit the research community and help improve the standards for data and computational methods in electron microscopy, and we invite the community to contribute to this ongoing project.
The limiting shear stress shear rheological model was applied to property measurements pursuant to the use of the constitutive equation and the application of the constitutive equation to elastrohydrodynamic (EHD) traction. Experimental techniques were developed to subject materials to isothermal compression which is similar to the history the materials were subjected to in EHD contacts. In addition, an apparatus was developed for measuring the shear stress-strain behavior of solid lubricating materials. Four commercially available materials were examined under pressure. They exhibit elastic and limiting shear stress behavior similar to that of liquid lubricants. The application of the limiting shear stress model to traction predictions was extended employing the primary materials properties measured in the laboratory. The shear rheological model was also applied to a Grubin-like EHD inlet analysis for predicting film thicknesses when employing the limiting shear stress model material behavior.
Thermal protection systems (TPS) protect spacecraft from the heating associated with hypersonic flight through a planet’s atmosphere. The materials are subjected to extreme heating and the overall system must be engineered to reliably protect the spacecraft structure during atmospheric entry. The talk will introduce TPS and describe three NASA-led efforts to develop TPS materials and manufacturing processes. The first effort studied thermally stable ceramic aerogels for use in thermal barriers and high temperature seals. A design framework for such materials is proposed, linking the thermal stability performance data with existing material property measurements. The second project, Additive Manufacturing of Thermal Protection Systems (AMTPS), developed an automated, additive approach for ablative heat shield manufacturing. Novel material systems and manufacturing methods were developed to reduce the time required to manufacture ablative TPS heat shields. The third effort tackles a critical challenge of material obsolescence for silica fiber based reusable TPS. The properties and performance of heritage silica fiber are quantified and compared to modern alternatives to support qualification for flight. The talk will also describe other work in TPS conducted by the Thermal Design Branch at NASA JSC and opportunities for students and faculty to get involved with NASA.
Mechanical testing campaigns are required to qualify materials for advanced reactor conditions, yet economical and safety limitations restrict the number of standardized mechanical tests that can be performed. Reducing the size of the sample is one approach to addressing these challenges and to accelerating testing. Previous research has shown that smaller mechanical test samples produce higher yield and ultimate stress values compared to values measured from standard sample sizes: the “smaller is stronger” effect. Specimens used in accelerated material testing campaigns must reflect bulk material performance to enable engineering scale material property measurement. The objective of this research project was to determine if engineering scale mechanical behavior—the yield stress—could be measured with micro-tensile test samples smaller than traditional standard testing geometries. The relationship between yield stress and sample size was explored with two different nuclear-relevant structural materials: Zircaloy-4 and tungsten. Mechanical testing of both metals demonstrated decreasing yield stress values with increasing sample gauge size across three different sizes. Yield stress values from the largest gauge size, fabricated with a femto-second laser ablation system, approach bulk material yield stress values reported in published literature. Preliminary analysis of the tungsten samples indicates the yield stress value depends on the grain characteristics within the gauge section, in addition to the gauge size. Accompanying modeling efforts, including response surface generation and crystal plasticity approaches, further demonstrated that the size of the sample gauge section alone cannot explain the change in yield stress values.
The Mars Entry, Descent, and Landing Instrumentation (MEDLI2) sensor suite collected data during entry of the Mars 2020 Perseverance rover into Mars’ atmosphere. This suite included a network of MEDLI2 Instrumented Sensor Plugs (MISPs). Each MISP was comprised of a cylinder made of Thermal Protection System (TPS) material with 1-3 embedded thermocouples (TCs), and it was flush mounted into the heatshield or backshell. Data from these in-depth TCs were used to reconstruct the aeroheating environment of the vehicle throughout entry. Surface heating was posed as an inverse problem, with the goal of estimating the surface heating by minimizing an objective function of the difference between MISP temperature measurements during flight and the temperature predictions derived from the Fully Implicit Ablation and Thermal response (FIAT) program. Given an aerothermal environment, FIAT calculates the material response and provides in-depth temperatures throughout the TPS material. To achieve the reverse, an internal tool called FIAT_Opt runs through multiple different environments until the output temperature at the TC depth closely matches the flight data. 95% confidence intervals on the reconstructed surface heating were obtained using Monte Carlo analysis, in which uncertainties in the thermocouple depth and the TPS material properties (e.g., density, thermal conductivity, heat capacity, emissivity) based on flight-lot material testing were included. A variance decomposition method using Sobol indices was employed to assess the sensitivity of the reconstructed peak heating to the TC placement and material property uncertainties. Variance decomposition was found to require tens of thousands of FIAT_Opt runs in order for the Sobol indices to converge. With a single FIAT_Opt run taking on the order of 40 minutes, the required number of computations would take months to complete, even if using multiple CPUs. To mitigate this problem, three machine learning models (ridge regression with cross-validation, random forest regression, and a deep neural network) were trained and tested using the 2000 Monte Carlo runs that were already completed. A subset of 1600 runs were used to train the model (i.e., training set), while the remaining 400 runs were used as the test set. The predictions from the deep neural network (DNN) on the test set showed nearly perfect agreement to the actual values computed with FIAT_Opt (R2 > 0.99). Using the DNN as a surrogate model, the variance decomposition using 50,000 runs was completed within minutes. The resulting Sobol indices showed that the reconstructed peak surface heating was most sensitive to the uncertainties in the thermal conductivity (ST = 0.37) and heat capacity (ST = 0.26). This method can be leveraged to provide requirements for material property measurements needed to improve the accuracy of surface heating prediction and ultimately lead to the reduction of design margins in the future. This presentation will include background on the MEDLI2 suite; the method used for inverse heating estimation; the way that material property uncertainties were accounted for using Monte Carlo analysis; a brief background on variance decomposition; the motivation for using machine learning in this context; how a neural network was trained on the data to enable variance decomposition in a fraction of the time; and the variance decomposition results for one of the MISPs.
High purity graphite will be used for core components within most High Temperature Reactor (HTR) designs. Several "high tech” industries currently utilize synthetic, high-purity, commercially available graphite components to fabricate photovoltaic cells, semi-conductors, optical fibers, and other high value electronic industry products. New advanced HTR designs are also interested in using these graphite grades for long-term, internal core component applications. Consequently, the US Department of Energy, Advanced Reactor Technologies (DOE-ART) program has spent several years testing different high purity graphite grades for potential use within these new nuclear reactor designs. A significant part of that effort has been in the development and improvement of American Society for Testing and Materials (ASTM) test standards specifically for nuclear graphite grades. Nearly all ASTM test standards have either been developed or improved by the DOE-ART program over the past 25 years. The ART program continues to assist in the development of new ASTM test standards in support of the future commercial HTR fleet currently being designed and built in the USA. The newest effort undertaken by ART is the development of high temperature mechanical testing practices that may be acceptable for a future ASTM test standard (or guide) for this critical material property measurement.
This characterization plan describes the thermal, physical, and mechanical measurement techniques that will be used to characterize graphite samples being tested in the fourth Advanced Graphite Creep experiment (AGC-4). Instruments, fixtures, and methods are currently in place for both pre and postirradiation material property measurements of bulk density, thermal diffusivity, coefficient of thermal expansion, elastic modulus, and electrical resistivity. Postirradiation testing procedures used to characterize the samples are described and discussed in the plan. Where they exist, American Society for Testing and Materials (ASTM) International testing standards will apply to the tests. Any departure from ASTM International testing standards or the approved laboratory procedures are documented within this characterization plan. Deviations that occur during testing will be documented in data reports.
Formulation control is key to achieving consistent target properties of energetic materials, as feedstock variations and slight deviations in the ratios of different ingredients can have major effects on final product properties, particularly in dense pastes with high particle loading >65 vol.%. In large‐scale operations, it is imperative to either correct or remove batches of material that perform outside baseline property specifications as early as possible to avoid unnecessary processing of suboptimal material. Quality monitoring is the practice of measuring material properties during processing using process analytical technologies as opposed to only testing the properties of the final product; it is a key principle in the quality‐by‐design frameworks used for designing formulations and manufacturing processes. Herein, a process analytical technology method for correlating material properties of dense pastes directly after mixing in a Resonant Acoustic Mixer to motor data is developed and used to detect differences in the particle content of dense paste formulations. This method was also capable of detecting variations in powder feedstock properties, such as particle packing efficiency, and is sensitive enough to detect changes of 2 wt.% in the total solids content of the formulation. The techniques presented herein show excellent promise for use as a process analytical technology capable of quantifying formulation effects on material movement modes during resonant acoustic mixing.
A generic list of Space Station surfaces and candidate material types is provided. Environmental exposures and performance requirements for the different Space Station surfaces are listed. Coating materials and the processing required to produce a viable system, and appropriate environmental simulation test facilities are being developed. Mass loss data from the original version of the atomic oxygen test chamber and the improved facility; additional environmental exposures performed on candidate materials; and materials properties measurements on candidate coatings to determine the effects of the exposures are discussed. Methodologies of production, and coating materials, used to produce the large scale demonstration articles are described. The electronic data base developed for the contract is also described. The test chamber to be used for exposure of materials to atomic oxygen was built.
Recent efforts were made to parametrize an aluminum alloy at cryogenic temperatures to calibrate finite element models simulating material deformation. Digital image correlation (DIC) was used to measure material properties using front/back strains of specimens during tensile tests. Data acquired from DIC was compared to physical extensometer measurements. Two camera pairs (front and back) were mounted via aluminum extrusion to the exterior of an environmental chamber of a hydraulic test stand. Images were taken through single-pane optical glass windows of the environment chamber. Positive pressure bags encased the cameras, attaching to the perimeter of the glass to keep out moisture and prevent windows from frosting. Figure 1 shows the environmental setup and the camera setup during cryogenic testing. Some of the challenges during testing at cryogenic temperatures include the gaseous flow of liquid nitrogen in the optical path of the mounted cameras, frost buildup on the windows as seen in Figure 1b, and frost on the test coupon. The temperature gradient present during the introduction of liquid nitrogen into the chamber can increase the projection error of images captured of the specimen. Figure 2 shows the estimated projection error from DIC as a function of temperature during the cool down process. This presentation addresses some of the concerns and observations when using DIC for testing at cryogenic temperatures using methods of isolated camera system and techniques for maintaining the glass panel clear from frost.
Commercially available polymer thin fdms with thickness of 15 microns or less were evaluated for potential application as the gas envelope material of balloons and other inflated vehicles. Films on this thickness scale are of interest for Earth and Mars ballooning as well as many gossamer space structures. Due to the uniqueness of these missions relative to typical uses of these materials, application-specific materials properties measurements were made. We evaluated numerous polymer chemistries, plus a few variations within one chemistry. The data show that there are often trade-offs among the different materials, such as with polyesters and polyimides having greater stiffness (modulus) but lower tear propagation resistance than polyethylene. Sections of polyethylene films can be joined by heat sealing, while adhesives and their accompanying mass penalty must be used with polyesters and polyimides. When the analysis temperature is reduced to 190 K, polyethylenes display dramatically increased stiffness and yield point, while the increase for other materials is more modest. The data also show that manufacturing processes can significantly affect film properties. To emphasize the need for application-specific properties assessment, we discuss two recent applications using these materials.
Destructive techniques to monitor nuclear reactor component health may not always be available during service, as they are time-consuming and often require pre-installed inspection coupons. Non-destructive evaluation (NDE) techniques can bridge this gap by rapidly identifying the state of mission-critical reactor components, via inference between NDE-measurable material properties and those of ultimate interest, such as ductility and toughness. Here, we demonstrate one such inference about the health of thermally aged cast austenitic stainless steels. Observations of surface acoustic wave peak (SAW) splitting correlate with spinodal decomposition-induced embrittlement as destructively measured by Charpy impact energy. Elastodynamic calculations and molecular dynamics simulations of the effects of spinodal decomposition on elastic moduli support that the new acoustic modes present are due to stiffening in the δ-ferrite domains. Finally, this discovery enables one to probe structure-property relationships in materials in a greatly accelerated manner, suggesting that similar inference methods can be used to determine material fitness-for-service, or to quickly uncover new structure-property relationships.
With the increasing number of 100 s GPa experiments in the diamond anvil cell (DAC), improved accuracy in secondary pressure calibrations to extreme pressures is essential. The rhenium equation of state has been proposed as a pressure calibrant via x-ray diffraction with potentially broad applications as it is commonly used as a gasket material in DAC experiments. In this work, we conducted Raman spectroscopy experiments on rhenium in the DAC and report the pressure shift of the E2g mode, a refined high-pressure C44 and mode-Grüneisen parameter above 200 GPa. We used flat, beveled, and toroidal diamond anvils under quasi-hydrostatic and non-hydrostatic conditions. By measuring the E2g mode from the culet edge to the center, we analyzed pressure distribution based on culet type and distance from the anvil center. The shift in the E2g mode can be expressed as a function of pressure, and diamond edge measurements appear reliable across all anvil types. Comparing the center and edge pressures reveals anvil cupping, offering insights into predicting or preventing anvil failure during materials properties measurements at extreme conditions.
This report documents all pre-irradiation examination material-property measurement data for graphite specimens that are going to be used within the first high dose graphite (HDG) -1 irradiation capsule. The two new HDG capsules signify a major change to the AGC Experiment. HDG-1 and HDG-2 will replace the last two Advanced Graphite Creep (AGC) capsules (AGC-5 and AGC-6) which were designed to irradiate graphite at the extreme upper operational temperatures for a very-high-temperature reactor (VHTR) design, 1100°C. These very high temperature AGC-5 and AGC-6 capsules have been repurposed to re-irradiated specimens (from AGC-2, AGC-3, and AGC-4) at the lower temperatures of 600°C and 800°C. HDG-1 will be irradiated at 600°C and HDG-2 will be irradiated at 800°C. By re-irradiating the previous AGC specimens a total maximum neutron dose of around 15 dpa (displacements per atom) can be achieved for all major graphite grades at irradiation temperatures of 600°C and 800°C. Specimens in the HDG-1 capsule are made up of previously irradiated specimens from the AGC-2 capsule and unirradiated specimens prepared for the now discontinued AGC-5 capsule. Utilizing the irradiated specimens, a maximum neutron dose of around 15 dpa is anticipated. These new maximum dose levels will provide irradiated material property data over a total neutron dose range of 1-15 dpa at a temperature of 600°C when combined with the previous AGC-1 and AGC-2 irradiation data. This will provide quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades for use within high temperature reactor designs. Similar to previous AGC test trains, HDG-1 includes the major graphite grades (IG-110, NBG-17, NBG-18, PCEA, and 2114) as well as adding the very fine-grain grade IG-430 which is of interest to the Molten Salt Reactor (MSR) designs. Also new to the HDG-1 capsule are 90 smaller geometry specimens designated as pencil specimens. These specimens take up only one third the space of a standard creep size specimen. This increased number of specimens will enhance property measurement statistics because they will provide 3 times the control specimen data at a position that would otherwise only have a single measurement.
This report documents all pre-irradiation examination material-property measurement data for graphite specimens that are going to be used within the first high dose graphite (HDG) -1 irradiation capsule. The two new HDG capsules signify a major change to the AGC Experiment. HDG-1 and HDG-2 will replace the last two Advanced Graphite Creep (AGC) capsules (AGC-5 and AGC-6) which were designed to irradiate graphite at the extreme upper operational temperatures for a very-high-temperature reactor (VHTR) design, 1100°C. These very high temperature AGC-5 and AGC-6 capsules have been repurposed to re-irradiated specimens (from AGC-2, AGC-3, and AGC-4) at the lower temperatures of 600°C and 800°C. HDG-1 will be irradiated at 600°C and HDG-2 will be irradiated at 800°C. By re-irradiating the previous AGC specimens a total maximum neutron dose of around 15 dpa (displacements per atom) can be achieved for all major graphite grades at irradiation temperatures of 600°C and 800°C. Specimens in the HDG-1 capsule are made up of previously irradiated specimens from the AGC-2 capsule and unirradiated specimens prepared for the now discontinued AGC-5 capsule. Utilizing the irradiated specimens, a maximum neutron dose of around 15 dpa is anticipated. These new maximum dose levels will provide irradiated material property data over a total neutron dose range of 1-15 dpa at a temperature of 600°C when combined with the previous AGC-1 and AGC-2 irradiation data. This will provide quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades for use within high temperature reactor designs. Similar to previous AGC test trains, HDG-1 includes the major graphite grades (IG-110, NBG-17, NBG-18, PCEA, and 2114) as well as adding the very fine-grain grade IG-430 which is of interest to the Molten Salt Reactor (MSR) designs. Also new to the HDG-1 capsule are 90 smaller geometry specimens designated as pencil specimens. These specimens take up only one third the space of a standard creep size specimen. This increased number of specimens will enhance property measurement statistics because they will provide 3 times the control specimen data at a position that would otherwise only have a single measurement.