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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.

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430 records · Page 24
All sourcesNASA NTRSDOE OSTI
DOE OSTI2019

Maximization of thermal conductance at interfaces via exponentially mass-graded interlayers

Here, we propose a strategy to potentially best enhance interfacial thermal transport through solid–solid interfaces by adding nano-engineered, exponentially mass-graded intermediate layers. This exponential design rule results in a greater enhancement than a linearly mass-graded interface. By combining calculations using non-equilibrium Green's functions (NEGF) and non-equilibrium molecular dynamics (NEMD), we investigated the role of impedance matching and anharmonicity in the enhancement in addition to geometric parameters such as the number of layers and the junction thickness. Our analysis shows that the effect on thermal conductance is dominated by the phonon thermalization through anharmonic effects, while elastic phonon transmission and impedance matching play a secondary role. In the harmonic limit, increasing the number of layers results in greater elastic phonon transmission at each individual boundary, countered by the decrease of available conducting channels. Consequently, conductance initially increases with number of layers due to improved bridging, but quickly saturates. The presence of slight anharmonic effects (at very low temperature, T = 2 K) turns the saturation into a monotonically increasing trend. Anharmonic effects can further facilitate interfacial thermal transport through the thermalization of phonons at moderate temperatures. At high temperature, however, the role of anharmonicity as a facilitator of interfacial thermal transport reverses. Strong anharmonicity introduces significant intrinsic resistance, overruling the enhancement in thermal conduction at the boundaries. It follows that at a particular temperature, there exists a corresponding junction thickness at which thermal conductance is maximized.

36 MATERIALS SCIENCE↗
DOE OSTI2021

In situ X-ray imaging of pore formation mechanisms and dynamics in laser powder-blown directed energy deposition additive manufacturing

Directed energy deposition (DED) additive manufacturing (AM) is receiving growing attention in many applications, such as repair, remanufacturing, and fabrication of functionally graded structures. However, the laser-matter interactions and melt pool dynamics in laser DED with powder flow are still unclear, particularly in how pores form and flow inside the melt pool during the process. Understanding the porosity formation mechanisms is critical in the qualification, certification, and overall properties of a DED AM part. Porosity is a common phenomenon and can significantly hinder the quality of DED fabricated parts, as the pores can act as sites of crack nucleation and propagation. Here in this paper, we reveal four types of pore formation mechanisms through in-situ and operando high-speed high-resolution X-ray imaging in the DED AM process. Our results confirm that porosity within the feedstock powder induces pores in the process. We also observed pore formation mechanisms unique to the laser-based, powder-blown DED process as a result of powder delivery, keyhole dynamics, melt pool dynamics, and shield gas. High-speed X-ray images provide direct evidence for pore formation mechanisms and show that the pores related to the interaction between the delivered powder and melt pool are the largest in size in laser-based powder-blown DED AM. These results will guide porosity mitigation, elimination, and control in DED AM.

36 MATERIALS SCIENCE↗
DOE OSTI2014

AGC-3 Experiment Irradiation Monitoring Data Qualification Final Report

The Graphite Technology Development Program will run a series of six experiments to quantify the effects of irradiation on nuclear-grade graphite. The third experiment, Advanced Graphite Creep 3 (AGC-3), began with Advanced Test Reactor (ATR) Cycle 152B on November 27, 2012, and ended with ATR Cycle 155B on April 23, 2014. This report documents qualification of AGC-3 experiment irradiation monitoring data for use by the Very High Temperature Reactor (VHTR) Technology Development Office (TDO) Program for research and development activities required to design and license the first VHTR nuclear plant. Qualified data meet the requirements for data collection and use as described in the experiment planning and quality assurance documents. Failed data do not meet the requirements. Trend data may not meet the requirements, but may still provide some useable information. The report documents qualification of AGC-3 experiment irradiation monitoring data following MCP-2691. This report also documents whether AGC-3 experiment irradiation monitoring data meet the requirements for data collection as specified in technical and functional requirements documents and quality assurance (QA) plans. Data handling is described showing how data are passed from the data collection experiment to the Nuclear Data Management and Analysis System (NDMAS) team. The data structure is described, including data batches, components, attributes, and response variables. The description of the approach to data qualification includes the steps taken to qualify the data and the specific tests used to verify that the data meet requirements. Finally, the current status of the data received by NDMAS from the AGC-3 experiment is presented with summarized information on test results and resolutions. This report addresses all of the irradiation monitoring data collected during the AGC-3 experiment.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Demonstration of Energy-Resolved γ-Ray Detection at Room Temperature by the CsPbCl 3 Perovskite Semiconductor

The detection of gamma-rays at room temperature with high-energy resolution using semiconductors is one of the most challenging applications. The presence of even the smallest amount of defects is sufficient to kill the signal generated from gamma-rays which makes the availability of semiconductors detectors a rarity. Lead halide perovskite semiconductors exhibit unusually high defect tolerance leading to outstanding and unique optoelectronic properties and are poised to strongly impact applications in photoelectric conversion/detection. Here we demonstrate for the first time that large size single crystals of the all-inorganic perovskite CsPbCl 3 semiconductor can function as a high-performance detector for gamma-ray nuclear radiation at room temperature. CsPbCl 3 is a wide-gap semiconductor with a bandgap of 3.03 eV and possesses a high effective atomic number of 69.8. We identified the two distinct phase transitions in CsPbCl 3 , from cubic (Pm-3m) to tetragonal (P4/mbm) at 325 K and finally to orthorhombic (Pbnm) at 316 K. Despite crystal twinning induced by phase transitions, CsPbCl 3 crystals in detector grade can be obtained with high electrical resistivity of similar to 1.7 X 10 9 Ω∙cm. The crystals were grown from the melt with volume over several cubic centimeters and have a low thermal conductivity of 0.6 W m -1 K -1 . The mobilities for electron and hole carriers were determined to similar to 30 cm 2 /(V s). Using photoemission yield spectroscopy in air (PYSA), we determined the valence band maximum at 5.66 +/- 0.05 eV. Under gamma-ray exposure, our Schottky-type planar CsPbCl 3 detector achieved an excellent energy resolution (similar to 16% at 122 keV) accompanied by a high figure-of-merit hole mobility-lifetime product (3.2 x 10 -4 cm 2 /V) and a long hole lifetime (16 mu s). The results demonstrate considerable defect tolerance of CsPbCl 3 and suggest its strong potential for gamma-radiation and X-ray detection at room temperature and above.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1999

Sliding Wear and Fretting Wear of DLC-Based, Functionally Graded Nanocomposite Coatings

Improving the tribological functionality of diamondlike carbon (DLC) films--developing, good wear resistance, low friction, and high load-carrying capacity-was the aim of this investigation. Nanocomposite coatings consisting of an amorphous DLC (a-DLC) top layer and a functionally graded titanium-titanium carbon-diamondlike carbon (Ti-Ti(sub x) C(sub y)-DLC) underlayer were produced on AISI 440C stainless steel substrates by the hybrid technique of magnetron sputtering and pulsed-laser deposition. The resultant DLC films were characterized by Raman spectroscopy, scanning electron microscopy, and surface profilometry. Two types of wear experiment were conducted in this investioation: sliding friction experiments and fretting wear experiments. Unidirectional ball-on-disk sliding friction experiments were conducted to examine the wear behavior of an a-DLC/Ti-Ti(sub x) C(sub y)-DLC-coated AISI 440C stainless steel disk in sliding contact with a 6-mm-diameter AISI 440C stainless steel ball in ultrahigh vacuum, dry nitrogen, and humid air. Although the wear rates for both the coating and ball were low in all three environments, the humid air and dry nitrogen caused mild wear with burnishing, in the a-DLC top layer, and the ultrahigh vacuum caused relatively severe wear with brittle fracture in both the a-DLC top layer and the Ti-Ti(sub x) C(sub y)-DLC underlayer. For reference, amorphous hydrogenated carbon (H-DLC) films produced on a-DLC/Ti-Ti(sub x) C(sub y)-DLC nanocomposite coatings by using an ion beam were also examined in the same manner. The H-DLC films markedly reduced friction even in ultrahigh vacuum without sacrificing wear resistance. The H-DLC films behaved much like the a-DLC/Ti-Ti(sub x) C(sub y)-DLC nanocomposite coating in dry nitrogen and humid air, presenting low friction and low wear. Fretting wear experiments were conducted in humid air (approximately 50% relative humidity) at a frequency of 80 Hz and an amplitude of 75 micron on an a-DLC/Ti-Ti(sub x) C(sub y)-DLC-coated AISI 440C disk and on a titanium-6 wt % aluminum-4 wt% vanadium (Ti-6Al-4V) flat, both in contact with a 9.4-mm-diameter, hemispherical Ti-6Al-4V pin. The resistance to fretting wear and damage of the a-DLC/Ti-6Al-4V materials pair was superior to that of the Ti-6Al-4V/Ti-6AI-4V materials pair.

Miyoshi, K.↗
DOE OSTI2023

FINITE ELEMENT MODEL MESH REFINEMENT EFFECTS ON QUALIFICATION OF NUCLEAR GRADE GRAPHITE COMPONENTS

The American Society of Mechanical Engineers (ASME) provides the full and simplified design-by-analysis probabilistic assessments for determining acceptance of nuclear grade graphite core components. The assessments can be characterized by three parts: (1) a component stress distribution, often determined by a finite element (FE) model; (2) a Weibull probability density function (pdf) that characterizes the experimental tensile strength distribution; and (3) the post-processor, which combines the FE model and the Weibull strength distribution in accordance with the full and simplified assessments to determine component acceptance. It is known that the level of mesh refinement in FE models can affect the modeled component’s calculated stress distribution. Depending on the component geometry, the stress distribution may converge with sufficient refinement. It was previously unknown whether the acceptance decision resulting from the full and simplified assessments might change even with sufficient mesh refinement. This study explores that question using experimental strength results for a dog-bone geometry for two graphite grades, IG-110 and PCEA. The simplified assessment has two criteria that must be met, the first limits the combined membrane stress by the allowable stress and the second limits the peak equivalent stress by the allowable stress scaled by the ratio of flexural to tensile strength. In the application of the simplified assessment, convergence of the peak equivalent stress required extreme mesh refinement, however, the acceptance decision was not affected. It is hypothesized that more complex geometries with stress concentrations may present mesh refinement effects on the simplified assessment acceptance decision. Mesh refinement did affect the acceptance decision in the full assessment for the applied pressure loadings in this study. This work suggests component stress distribution convergence is not a sufficient criteria for POF convergence in the full assessment and that mesh refinement should continue until the POF has converged, especially where the resulting POF is bordering the SRC acceptable POF limit.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2014

AGC-3 Experiment Irradiation Monitoring Data Qualification (Final Report)

The Graphite Technology Development Program will run a series of six experiments to quantify the effects of irradiation on nuclear grade graphite. The third experiment, Advanced Graphite Creep 3 (AGC 3), began with Advanced Test Reactor (ATR) Cycle 152B on November 27, 2012, and ended with ATR Cycle 155B on April 23, 2014. This report documents qualification of AGC 3 experiment irradiation monitoring data for use by the Very High Temperature Reactor (VHTR) Technology Development Office (TDO) Program for research and development activities required to design and license the first VHTR nuclear plant. Qualified data meet the requirements for data collection and use as described in the experiment planning and quality assurance documents. Failed data do not meet the requirements. Trend data may not meet the requirements, but may still provide some useable information. All thermocouples (TCs) functioned throughout the AGC 3 experiment. There was one interval between December 18, 2012, and December 20, 2012, where 10 NULL values were reported for various TCs. These NULL values were deleted from the Nuclear Data Management and Analysis System database. All temperature data are Qualified for use by the VHTR TDO Program. Argon, helium, and total gas flow data were within expected ranges and are Qualified for use by the VHTR TDO Program. Total gas flow was approximately 50 sccm through the AGC 3 experiment capsule. Helium gas flow was briefly increased to 100 sccm during ATR shutdowns. At the start of the AGC 3 experiment, moisture in the outflow gas line was stuck at a constant value of 335.6174 ppmv for the first cycle (Cycle 152B). When the AGC 3 experiment capsule was reinstalled in ATR for Cycle 154B, a new moisture filter was installed. Moisture data from Cycle 152B are Failed. All moisture data from the final three cycles (Cycles 154B, 155A, and 155B) are Qualified for use by the VHTR TDO Program.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2015

Diamond as a solid state micro-fission chamber for thermal neutron detection at the VR-1 research reactor

Diamond exhibits a combination of properties which makes it attractive for neutron detection in hostile conditions. In the particular case of detection in a nuclear reactor, it is resilient to radiation, exhibits a natural low sensitivity to gamma rays, and its small size (as compared with that of gas ionisation chambers) enables fluency monitoring with a high position resolution. We report here on the use of synthetic CVD diamond as a solid state micro-fission chamber with U-235 converting material for in-core thermal neutron monitoring. Two types of thin diamond detectors were developed for this application. The first type of detector is fabricated using thin diamond membrane obtained by etching low-cost commercially available single crystal CVD intrinsic diamond, so called 'optical grade' material. Starting from a few hundred of micrometre thick samples, the sample is sliced with a laser and then plasma etched down to a few tenths of micrometre. Here we report the result obtained with a 17 μm thick device. The detection surface of this detector is equal to 1 mm{sup 2}. Detectors with surfaces up to 1 cm{sup 2} can be fabricated with this technique. The second type of detector is fabricated by growing successively two thin films of diamond, by the microwave enhanced chemical vapour deposition technique, on HPHT single crystal diamond. A first, a film of boron doped (p+) single crystal diamond, a few microns thick, is deposited. Then a second film of intrinsic diamond with a thickness of a few tens of microns is deposited. This results in a P doped, Intrinsic, Metal structure (PIM) structure in which the intrinsic volume id the active part of the detector. Here we report the results obtained with a 20 μm thick intrinsic whose detection surface is equal to 0.5 mm{sup 2}, with the possibility to enlarge the surface of the detector up to 1 cm{sup 2}. These two types of detector were tested at the VR-1 research reactor at the Czech Technical University in Prague. The Training Reactor VR-1 is a pool type (light water) reactor based on UO{sub 2} low enriched uranium. It has a nominal power of 1 kW, and can be operated for a short period up to 5 kW. The arrangement of the reactor pool reactor facilitates access to the core, setting and removal of various experimental samples and detectors, and safe and easy handling of fuel assemblies. The reactor is equipped with two horizontal channels (radial and tangential) and 10 vertical channels, of varying diameters, which can be loaded into various core positions, and one pneumatic transfer system. It is also equipped with several specifically designed educational instrumentation systems that can be used to supply complementary measurements and characterization around the reactor. The reactor is operated by the Department of Nuclear Reactors of the Faculty of Nuclear Sciences and Physical Engineering of the Czech Technical University in Prague. The two detectors were placed in-core through one of the vertical insertion channel. They were coupled to remote placed (5 m BNC cable) classical nuclear charge sensitive electronics. Detection properties of both sensors, including: pulse height spectra of U-235 fission fragments (response linearity with neutron flux, count rate, gamma background, were evaluated varying the power of the reactor from 0.005 W to 500 W. The evolution of the counting rate of the thinned optical grade detector as a function of counting rate of a gas ionization chamber used currently for reactor monitoring shows the very good linearity of the detector over the 5 decades. Similar results were obtained with the PIM detector. Additionally fast transient current signals of the detectors were recorded on a digital storage oscilloscope (DSO) using broad-band amplifier and with a simple bias-T, showing potential use of such sensors for neutron counting with no need of an amplification stage, since non-amplified signals from fission fragments exceeded 4 mV in amplitude. Therefore, one can think of simple neutron counting system by feeding diamond detectors signals directly to the low threshold discriminators. The results obtained on the VR1 will be described and discussed in detail in the paper and associated presentation. The results demonstrate that diamond micro-fission chambers can be used for in-core neutron monitoring, where robust, simple and compact devices are required.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗
DOE OSTI2022

A Novel Process for Carbon Dioxide Conversion to Fuel

In this project, TDA developed a new mixed metal oxide-based sorbent that converts CO2 (captured from coal fired power plants) to CO, which can then be combined with renewable H2 generated by water electrolysis or H2 from steam methane reforming to produce different liquid fuels. TDA’s absorbent-based CO2 conversion process uses a redox process, which splits the catalytic reforming of methane with CO2 reaction into two stages: CO2 reduction to CO and CH4 reforming into H2 and CO which eliminates the equilibrium limitations. The CO produced in the two-stage reactor system can then be further reacted with renewable H2 to produce methanol, naphtha, diesel, or gasoline. We worked with the Advanced Power & Energy Program (APEP) of University of California, Irvine (UCI) to design and develop the liquid fuel synthesis process that is built around this new material. We demonstrated the techno-economic viability of the new sorbent based redox process to convert CO2 into synthesis gas by demonstrating continuous carbon dioxide reduction in a prototype test system for over 585 hours while converting up to 10 kg CO2/day. With the successful completion of the R&D effort, the technology is now ready for a larger pilot-scale demonstration and the technology readiness has been raised from TRL 3 to TRL 5. In collaboration with UCI, we completed a high-fidelity process design and economic analysis. The required sale price (RSP) for gasoline (Case 1 NG-MTG) is $4.91/gal and naphtha and diesel (Case 2 NG-FT) are $4.23/gal and $6.07/gal, respectively, on a 2011 dollar basis. To put these costs in perspective, the California prices in current dollars (with its strict specifications) for regular grade gasoline from last year to current year have varied from a low of $3.10/gal in January 2021 to a high of $5.76/gal in March 2022, while prices for diesel from last year to current year have varied from a low of $3.40/gal in January 2021 to a high of $6.41/gal in May 2022 according to the U.S. Energy Information Agency data. It should be noted that the gasoline and diesel produced by these designs of Case 1 and Case 2 would be of very high quality and both nitrogen and sulfur free. These RSPs are based on a cost of imported electricity of $64/MWh based on the low-end current wind generated electricity cost (Genevieve 2011). This cost is by far the largest component of the variable costs used in computing the RSPs. A sensitivity analysis of these RSPs to the cost of imported electricity shows that the cost of the imported electricity has a significant effect on the RSPs. The life cycle analysis (LCA) shows that the total cradle-to-gate CO2 emissions for both liquid fuels (diesel and gasoline) were negative, indicating that overall more CO2 is consumed than released during production of the fuel from CO2 feed stack for both cases (-296 kgCO2 per MT gasoline for Case 1 and -705 kgCO2 per MT diesel for Case 2). On a cradle-to-grave comparison, the use of diesel produced using TDA’s process (2,457 kgCO2 per MT diesel) would release 37.6% less CO2 compared to petroleum based diesel (3,937 kgCO2 per MT diesel) while the use of gasoline produced using TDA’s process (2,792 kgCO2 per MT gasoline) would release 29.3% less CO2 compared to petroleum based gasoline (3,946 kgCO2 per MT gasoline). With the successful completion of the R&D effort, the technology is now ready for a bench-scale demonstration and the technology readiness has been raised from TRL 3 (Analytical and experimental critical function and/or characteristic proof of concept) to TRL 5 (Laboratory scale similar system validation in relevant environment).

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2015

Fourier plane colorimetric sensing using broadband imaging of surface plasmons and application to biosensing

We demonstrate an optical technique for refractive index and thickness sensing of sub-wavelength-thick dielectric analytes. The technique utilizes the broadband, multimode, directional leakage radiation arising from the excitation of hybrid mode surface plasmons (SP) on low aspect ratio periodic plasmonic substrates with period ≈λ. The approach requires relaxed fabrication tolerances compared to extra ordinary transmission-based sensing techniques, wherein minor shifts in the fabricated dimensions result in a very large change from the designed resonant wavelength. We show that refractive index perturbations due to about 10-nm-thick dielectric can be captured optically by the usage of carefully designed plasmonic substrates, a halogen lamp source, free-space optical components, polarizers, and a low-end, consumer-grade charge coupled device camera. The plasmonic substrates were designed for converting the signature of hybrid mode SP excitation into a transmission peak by utilizing a thin homogeneous metal layer sandwiched between the periodic plasmonic structures and the substrate. The resonance is highly sensitive to the refractive index and thickness of the analyte superstrate. The excitation of hybrid mode SP results in a polarization rotation of 90° of the leaked radiation at resonant wavelength. In order to eliminate the problem of image registration (i.e., placing the same feature in the same pixel of the image, for comparison before and after a change in refractive index) for sensing, we perform the color analysis in the Fourier plane. The change in color of the bright emitted spot with highest momentum, corresponding to the leakage of fundamental SP mode, was used to measure the changes in refractive index, whereas the number and color of spots of lower momenta, corresponding to higher-order Fabry Perot modes, was used to measure the variation in thickness. We further show that the Fourier plane analysis can also be used to sense the index of thicker dielectrics, where real plane image analysis may fail to sense index perturbations, simply due to superposition of different modes in the real plane images of such substrates. Control experiments and analysis revealed a refractive index resolution of 10{sup –5} RIU. The results were correlated with simulations to establish the physical origin of the change in the fundamental mode and higher-order modes due to the refractive index and thickness of analyte. As a demonstration of an application and to test the limits of sensing, the substrates were used to image the surface functionalization using 2-nm-thick 11-mercaptoundecanoic acid and immobilization of 7-nm-thick mouse anti-human IgG antibody. In biological systems, where a priori knowledge about a process step is available, where accurate chemical composition testing is not necessary or possible, the presented method could be used to study the surface changes using a label-free sensing mechanism.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗
DOE OSTI2017

Dynamic Uniaxial Compression of HSLA-65 Steel at Elevated Temperatures

Here, the dynamic response of a high-strength, low alloy Grade 65 (HSLA-65) steel, used by the United States Navy for ship hull construction, is investigated under dynamic uniaxial compression at temperatures ranging from room temperature to 1000 °C using a novel elevated temperature split-Hopkinson pressure bar. These experiments are designed to probe the dynamic response of HSLA-65 steel in its single α-ferrite phase, mixed α + γ-austenite phase, and the single γ-austenite phase, as a function of temperature. The investigation is conducted at two different average strain rates—1450 and 2100/s. The experimental results indicate that at test temperatures in the range from room temperature to lower than 600 °C, i.e. prior to the development of the mixed α + γ phase, a net softening in flow strength is observed at all levels of plastic strain with increase in test temperatures. As the test temperatures are increased, the rate of this strain softening with temperature is observed to decrease, and at 600 °C the trend reverses itself resulting in an increase in flow stress at all strains tested. This increase in flow stress is understood be due to dynamic strain aging, where solute atoms play a distinctive role in hindering dislocation motion. At 800 °C, a (sharp) drop in the flow stress, equivalent to one-half of its value at room temperature, is observed. As the test temperature are increased to 900 and 1000 °C, further drop in flow stress are observed at all plastic strain levels. In addition, strain hardening in flow stress is observed at all test temperatures up to 600 °C; beyond 800 °C the rate of strain hardening isobserved to decrease, with strain softening becoming dominant at temperatures of 900 °C and higher. Moreover, comparing the high strain rate stress versus strain data gathered on HSLA 65 in the current investigation with those available in the literature at quasi-static strain rates, strain-rate hardening can be inferred. The flow stress increases from 700 MPa at 8 × 10 -4 /s to 950 MPa at 1450/s and then to 1000 MPa at 2100/s at a strain of 0.1. Finally, optical microscopy is used to understand evolution of microstructure in the posttest samples at the various test temperatures employed in the present study.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Initial ASME code rule analysis on Simple and Full assessment

ASME & ASTM codes present simple and full assessment methodologies to qualify nuclear grade graphite components. This report explains the theory behind the statistical portion of the codes and describes the issues discussed in a 2020 workshop in the simple assessment, as well as the full assessment. The methodology for the full assessment was developed by Hindley []. He used a validation methodology to match the experimental average failure load of test specimens from several geometries to the calculated 50% POF load to tune the grouping criteria parameters based on an RMSE penalty function. The grouping criteria consists of a minimum volume to satisfy the weakest link theory of the Weibull distribution and a minimum stress range parameter. Hindley’s work found a minimum link volume of 10 times the grain size and a stress range parameter of 7% [satisfy the validation requirements. Several studies found that the link volume of 10 times the grain size was not satisfactory for the volume grouping criteria for graphite grades with fine grains. ASME 2021 code adopted a new volume grouping criteria based on fracture toughness for calculation of the process zone volume. However, errors were found in the ASME 2021 code process zone volume equation and the question is now open as to what volume grouping criteria is satisfactory. This report presents results from sensitivity studies that were done to evaluate the volume grouping criteria effect on the full assessment POF. This report also presents results from sensitivity studies on other aspects of the code that affect the POF, the mesh size and the choice of the Weibull threshold parameter. All three sensitivity studies: the volume grouping criteria, the mesh size, and the threshold parameter choice are found to affect the component qualification decision for components of structural reliability class 1 (SRC-1). The sensitivity analysis results are presented in the body of the report for NBG-18, which is the same grade of graphite as Hindley used in his thesis. Results from NBG-17, IG-110, 2114, and PCEA are presented in the Appendix. For NBG-18, it was found that increasing the threshold increases the POF, finer meshes result in higher POFs, and that smaller link volume requirements lead to higher POFs (which is inconsistent with Hindley’s findings). This report proposes a new validation study similar to Hindley’s []. The purpose of the new validation study is to tune the threshold, mesh size and grouping criteria based on results from multiple grades of graphite, including finer grain graphites T220 (1-3 microns) and NG-CT-50 (5 microns). The test specimens will be broken at 3 labs, such that we can measure between lab measurement variability, with at least 5 test specimens per lab such that the within lab uncertainty can also be measured. Hindley’s validation method tried matching the average experimental load with the median. The future study will attempt to match failures at lower percentiles, which would be closer to the SRC POF limit. We are currently looking into what geometries make sense and the best method to measure multi-axial stress states. These design decisions are still being set.

36 MATERIALS SCIENCE↗
DOE OSTI2016

AGC-4 Experiment Irradiation Monitoring Data Qualification Interim Report

The Graphite Technology Development Program is running a series of six experiments to quantify the effects of irradiation on nuclear grade graphite. The fourth experiment, Advanced Graphite Creep 4 (AGC 4), began with Advanced Test Reactor (ATR) cycle 157D on May 30, 2015, and has been irradiated for two cycles. The capsule was removed from the reactor after ATR cycle 158A, which ended on January 2, 2016, due to interference with another experiment. Irradiation will resume when the interfering experiment is removed from the reactor. This report documents qualification of AGC 4 experiment irradiation monitoring data for use by the Advanced Reactor Technologies (ART) Technology Development Office (TDO) Program for research and development activities required to design and license the first HTR nuclear plant. Qualified data meet the requirements for use as described in the experiment planning and quality assurance documents. Failed data do not meet the requirements and provide no useable information. Trend data may not meet all requirements, but still provide some useable information. Use of Trend data requires assessment of how any deficiencies affect a particular use of the data. All thermocouples (TCs) have functioned throughout the AGC-4 experiment. All temperature data are Qualified for use by the ART TDO Program. Argon, helium, and total gas flow data were within expected ranges and are Qualified for use by the ART TDO Program. Discharge gas line moisture values were consistently low during cycle 157D. At the start of cycle 158A, gas moisture briefly spiked to over 600 ppmv and then declined throughout the cycle. Moisture values are within the measurement range of the instrument and are Qualified for use by the ART TDO Program. Graphite creep specimens were subjected to one of three loads, 393, 491, or 589 lbf. For a brief period during cycle 157D between 12:19 on June 2, 2015 and 08:23 on June 11, 2015 the load cells were wired incorrectly resulting in missing stack load data. Missing stack loads were estimated from measured ram pressures using regression equations developed from the existing data from cycle 157D. Estimated stack loads during this period are considered to be an accurate representation of actual load applied to the stacks. These loads deviate slightly from the planned loads. This deviation does not prevent the data from being Qualified for use, but must be taken into account when analyzing the effect of load on creep. Stack displacement increased consistently throughout the first two cycles with total displacement ranging from 0.4 to 0.8 in. During ATR outages, a set of pneumatic rams raised the stacks of graphite creep specimens to ensure the specimens were not stuck within the test train. This stack raising was performed twice. All stacks were raised successfully each time. The load and displacement data are Qualified for use by the ART TDO Program.

36 MATERIALS SCIENCE↗
NASA NTRSDate not supplied

In-Lab Rapid Analytical Detection of Lunar Volatiles By Universal Gas Analyzer With Comparison to GC-MS System

Introduction: The curation of permanently shadowed regions (PSRs) [1] on the lunar surface is centered around studies based upon the observed volatiles from the LCROSS mission [2]. The rapid detection of important volatile gases and vapors present in planetary bodies and Astromaterials by a standalone analytical device is an area of intense research interest in our group and Planetary Exploration & Astromaterials Research Laboratory (PEARL) facility and this work is relevant to the future preparation of viable lunar simulants for testing curation efforts down the road. The groundbreaking results obtained from the LCROSS Mission [2] open the requirements for the direct detection of volatiles present in regolith materials collected from the lunar surface. The mass spectrometry of volatile chemicals is a general technique that utilizes a set of instruments that creates charged ions from a gaseous chemical species and measures the intensities vs. mass-to-charge ratio (m/z) [3]. In this context, we discuss in-lab experimental results and procedures for rapid qualitative analysis of main LCROSS volatiles (water, H2S, NH3, CO2, and CH3OH) by a Universal Gas Analyzer (UGA) instrument. Additionally, the instrument performance was evaluated by measuring the isotopic abundance ratio of atmospheric Ar-40 to Ar-36 present in room air since, argon is a relevant gas in planetary studies as it can provide an insight and reference point to isotope studies [4]. Additional, cross comparisons were attempted and made between the two instruments to develop a robust analytical technique by comparing mass spectral data for H2S headspace samples with a Trace-1310/ ISQ 7000 (ThermoFisher Scientific.) GC-MS system. Background: The benchtop UGA System is equipped with an SRS UGA 300 quadrupole mass spectrometer designed and built by Stanford Research Systems [5]. This system can be configured for several types of gaseous chemical analysis. The inlet line continuously samples gases at low flow rates (several milliliters per minute) through a capillary limiting the intake pressure making the instrument ideal for online analysis of select gases and/or room atmosphere. Moreover, in our current UGA system, a change in composition at the inlet can be detected in about 200 milliseconds and a complete spectrum is acquired (for a range of 1-100 amu) in under 45 sec with masses measured at rates up to 25 msec per point [5]. This system provides a quick upstream analytical data that we can then compare to results obtained by our GC-MS system. Sample Preparation: Small volume (2-4 mL) of analyte sample was taken in a 10 mL glass vial and sealed with a crimped cap and purged with pure Ar or N2 gas to displace air from the top. The headspace sample was scanned by the UGA instrument at analog, histogram, and pressure vs. time modes. The isotopic abundance ratio for 40Ar-to-36Ar was estimated by measuring partial pressure vs. time scans and setting the mass at 40 and 36 respectively. Results and Discussions: In this work, we have investigated the applicability of the UGA system by qualitative analysis of a series of LCROSS volatiles measured individually. Fig. 1 demonstrates a set of vertically offset spectra for the partial pressures measured as a function of mass-to-charge (m/z) ratios. The average acquisition time for each spectrum was less than a minute suggesting that the UGA system is ideal for quick analysis of geochemical volatiles. For the cross-comparison, we analyzed an H2S headspace sample by a Trace-1310/ISQ-7000 system and compared mass spectral data with previously measured UGA histogram scan data (Fig. 2). In both cases, major peak positions are the same, however, the intensities of fragment ions ([1H132S]+ and [32S]+) are higher for UGA suggesting that the fragment ionization process is stronger in UGA compared to that of GC-MS. To investigate how the integrated area under each chromatogram varies with the headspace sample volume, a set of five H2S headspace samples with increasing volumes was analyzed by the GC-MS system (Fig. 3, inset). A small volume (e.g., 200 to 1000 µL) of H2S/H2O vapor was withdrawn from a 20 mL stock sample vial containing ~5 mL of 0.4% H2S in water by a gas-tight syringe and added to another 20 mL vial filled with argon and analyzed by the GC-MS system. Finally, the UGA detector sensitivity was evaluated by calculating the atmospheric 40Ar-to-36Ar isotopic abundance ratio in room air by running a partial pressure vs. time scan with setting the atomic mass at 40, and 36. Fig. 4(a) shows a ~25 min duration “P vs. time” scan for 40Ar (plot for 36Ar is not shown). The partial pressure values (~100 points) were corrected by subtracting the corresponding background pressure value for 37Ar and utilized to calculate 40Ar-to-36Ar isotopic abundance ratios as shown by Fig. 4b. The average isotopic abundance ratio is ~306 with a 2*STDEV ~13. This abundance ratio is significantly close to the previously reported value of 298.56 [6] and the ratio obtained by our GC-MS system (303 for a UHP grade Ar sample). Conclusions: Our study strongly evidenced that the benchtop UGA system is a valuable analytical tool for the detection of major LCROSS volatiles. The rapid scanning capability, the inexpensiveness of the whole system, and impressive detection sensitivity prove its worthiness as an essential device for advanced geochemical applications. Moreover, cross comparisons with the GC-MS provide important bridges into advanced curatorial efforts into the future. References: [1] Bickel, V.T., et al. (2021) Nat Commun 12, 5607. [2] Colaprete, A., et al. (2010) Science, 330, 463-468. [3] Glavin, D. P. et al. (2012) 2012 IEEE Aerospace Conference, 1-11. [4] Willett, C. D., et al. (2022) Geochimica et Cosmochimica Acta 329, 119-134. [5] Operation Manual and Programming Reference. (2018) Universal gas Analyzers, Stanford Research Systems. [6] Lee, J. Y., et al. (2006) Geochimica et Cosmochimica Acta 70, 4507–4512. Notes: (4 figures are attached with text as shown by the attached file)

Curation↗
DOE OSTI2016

A New Method for Low Cost Production of Titanium Alloys for Reducing Energy Consumption of Mechanical Systems

This project investigated an innovative manufacturing process intended to minimize the cost of production of titanium materials and components, and increase the adoption of Ti components for energy consuming applications, such as automobiles. A key innovation of the proposed manufacturing approach is a novel Ti powder sintering technology for making titanium materials with ultrafine grain microstructure in the as-sintered state with minimum, or an absence, of post-sintering processes. The new sintering technology is termed Hydrogen Sintering and Phase Transformations (HSPT), and constitutes a promising manufacturing technology that can be used to produce titanium (Ti) materials and components in a near-net-shape form, thus also minimizing machining costs. Our objective was to meet, or possibly surpass, the mechanical property levels for ASTM B348 Grade 5 for wrought Ti-6Al-4V. Although specific applications call for varying mechanical property requirements, ASTM B348 was created for the demanding applications of the aerospace industry, and is the established standard for Ti-6Al-4V. While the primary goal was to meet, or exceed this standard, the team also had the goal of demonstrating this could be done at a significantly lower cost of production. Interim goals of the project were to fully develop this novel sintering process, and provide sufficient baseline testing to make the method practical and attractive to industry. By optimizing the process parameters for the sintering of titanium hydride (TiH 2 ) powders in a hydrogen atmosphere and controlling the phase transformations during and after sintering, the HSPT process was expected to reduce the energy consumption, and thus cost, of making Ti alloys and fabricating Ti components. The process was designed such that no high temperature melting is required for producing Ti alloys; little or no post-sintering processing is needed for producing desired microstructures (and therefore enhanced mechanical properties), and finally, minimum machining is needed to fabricate finished Ti components. An energy analysis within this report provides more detail, but calculated values indicate that the HSPT process is less than half as energy intensive as conventional wrought processing, while producing mechanical properties that are comparable. In addition to the energy savings anticipated from the industrial production of Ti components, a second prong of energy savings resides in the use phase of components produced, primarily from use in the transportation sector. Titanium has a number of material qualities appropriate for the auto industry, particularly low mass and corrosion resistance. By reducing the weight of automobiles and other vehicles, energy costs and CO 2 production will be reduced over the lifetime of the vehicles, and components in corrosive environments on vehicles, such as exhaust systems and other under carriage parts, may not have to be replaced during a vehicle’s lifetime. Our analysis indicates that by replacing only 5.6 kg of steel parts in an auto with Ti components across the entire US fleet would save approximately 486 million gallons of gasoline per year. This correlates to a reduction of 3.6 million metric tons of CO 2 per year. The potential for replacing many more of the steel parts in automobiles with lighter weight titanium components is clear. The project was very successful overall, meeting all milestones and surpassing project goals in terms of mechanical properties and microstructures produced. In addition to tensile properties, fatigue properties were emphasized in the project work. Powder metallurgy processes often have porosity to some degree in their final microstructure, and porosity is a well-known cause of crack initiation and low fatigue performance. Although many automobile applications do not undergo fatigue stress regimes, many others do encounter cyclic stress, and design criteria in the latter case require good fatigue properties. Production and testing of HSPT parts showed excellent tensile properties and fracture toughness, and fatigue properties that exceeded all previously reported powder metallurgy Ti methods, overlapping with wrought processed values. Fatigue limits exceeded 500 MPa and tensile strength exceeded 1,000 MPa while maintaining good ductility. Microstructures produced during the project period easily surpassed pre-project expectations. In addition to producing very fine grains in the as-sintered state (without post sintered thermo-mechanical work), porosity was reduced and industrially relevant microstructures previously undemonstrated in any other powder metallurgy titanium method were produced using HSPT materials. These microstructures, both bi-modal and globularized, were produced with simple post-sinter heat treatments, but without the need for energy intensive mechanical work. The employed heat treatments expanded the available mechanical property range (tensile strength vs. ductility) of the HSPT system in Ti-6Al-4V. The project has resulted in the publication, thus far, of five refereed journal articles and five conference proceedings papers, as well as a patent application, two dissertations and a master’s thesis. Two additional journal articles are currently under review, and at least three others are currently in preparation, with several additional students anticipated to graduate within the coming year. Presentations and papers were a particular focus of the second half of the project, once significant experimentation had been performed and analyzed. As part of our efforts to disseminate information of our results, the Ti research teams within Prof. Fang’s and Prof. Chandran’s research groups had a strong presence at the 13th World Conference on Ti, August 16-20, 2015, in San Diego. Several research groups in the US and in Europe are now performing experiments using the HSPT process. Accompanying efforts to bring HSPT to the Ti community at large, and industry in particular, work has continued with our partners and with other interested industrial Ti users and producers, including Boeing and GKN (a major powder metallurgy parts manufacturer). Commercialization has been a central focus of the final phase of the project, and Reading Alloys signed a provisional licensing agreement in summer of 2015. They are currently seeking an appropriate customer with which to pursue initial parts manufacturing efforts. Other licensing options and partners are continuing to be pursued. The promise of lightweight, strong and corrosion resistant Ti alloys with long fatigue lifetimes for automobile or transportation applications has been the vision of the metal industry since titanium came to the attention of scientists and engineers. The sole limitation of realizing these goals has been cost, which is primarily a function of energy used in production. The HSPT process was shown through this work to be capable of realizing this goal, and facilitating the practical use of titanium in US automotive and other industries.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2020

AGC-4 Experiment Irradiation Monitoring Data Qualification Final Report

The Graphite Technology Development Program ran a series of six experiments to quantify the effects of irradiation on nuclear grade graphite. This report focuses on the fourth experiment, Advanced Graphite Creep 4 (AGC 4). The Advanced Reactor Development (ARD) Technology Development Office (TDO) Program for research and development activities require documentation of qualified monitoring data to design and license the first high-temperature reactor nuclear plant. Qualified data meets the requirements for use as described in the experiment planning and quality assurance documents. Failed data do not meet the requirements and provide no useable information. Trend data may not meet all requirements but still provide some useable information. Use of Trend data requires assessment of how any deficiencies affect a particular use of the data. AGC-4 began with Advanced Test Reactor (ATR) Cycle 157D on May 30, 2015. After irradiating the graphite for two cycles, the capsule was removed from the reactor after ATR Cycle 158A, which ended on January 2, 2016, due to interference with another experiment. Irradiation was resumed with Cycle 162A on October 7, 2017 after the interfering experiment was removed from the reactor. AGC-4 irradiation completed by the end of Cycle 166B on January 10, 2020. Between Cycles 162A and 166B, AGC-4 capsule was removed from the reactor core during two Powered Axial Locator Mechanism (PALM) Cycles 163A and 165A to avoid overheating. All thermocouples (TCs) have functioned throughout the AGC-4 experiment. A total of 9,256,184 out of all 11,167,213 temperature records (or 82.9%) are Qualified for use by the ARD Program and 1,911,029 missing values are Failed. Argon, helium, and total gas flow data were within expected ranges, except only eight out-of-range values occurred during outages. A total of 21,240,627 out of all 22,288,5103 gas flow rates (or 92.8%) are Qualified for use by the ARD Program and 1,644,476 are Failed records mostly due to missing values. Discharge gas line moisture values were consistently low during full ATR power, except for 162B, when moisture content was increasing to more than 200 ppmv by the end of this cycle. During outages, moisture content reached as high as 700 ppmv. 1,089,941 out of a total of 1,107,331 moisture values (or 98.4%) are within the measurement range of the instrument and are Qualified for use by the ARD Program and 17,390 missing moisture values are Failed. Graphite creep specimens were subjected to one of three loads: 393, 491, or 589 lbf. For a brief period during Cycle 157D between 12:19 on June 2, 2015, and 08:23 on June 11, 2015, the load cells were wired incorrectly, resulting in missing stack load data. Missing stack loads were estimated from measured ram pressures using regression equations developed from the existing data from Cycle 157D. Estimated stack loads during this period are considered to be an accurate representation of actual load applied to the stacks. These loads deviate slightly from the planned loads. This deviation does not prevent the data from being Qualified for use but must be taken into account when analyzing the effect of load on creep. 6,095,728 out of a total of 6,403,985 moisture values (or 95.2%) are within the measurement range of the instrument and are Qualified for use by the ARD Program and 308,257 missing load values are Failed. Stack displacement increased consistently throughout the eight cycles, with total displacement reached highest value of 2.4 in by the end of irradiation. During ATR outages, a set of pneumatic rams raised the stacks of graphite creep specimens to ensure the specimens were not stuck within the test train. This stack raising was performed seven times throughout irradiation. All stacks were raised successfully each time. 4,744,974 out of a total of 6,094,513 displacement values (or 77.9%) are within the measurement range of the instrument and are Qualified for use by the ARD Program and 1,349,539 displacement values are Failed mostly due to missing values. Analyses were conducted on correlations between TCs to look for trends and step changes that might indicate instrument degradation or failure. Correlation analysis was used to identify instances when TCs form short circuits, referred to as virtual junctions, which result in TCs reporting temperatures from some location in the capsule other than the location where they were intended to read. No evidence of virtual junctions was found. Analyses were also conducted on control charts of temperature differences of between two TCs, which are expected to behave consistently throughout the entire irradiation period. Upward or downward trend over time indicates at least one TC in the pair was drifted. Examining control charts for all 66 possible pairs out of twelve TCs installed in the AGC-4 capsules reveal no clear drift failures occurred, except unstable behavior of two TCs in Zone 3, TC-7 and TC-8, over irradiation time. In conclus

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗