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DOE OSTI2025

Electrochemical stability and corrosion behavior of Ni-Cr alloy in molten LiCl-KCl salt

This study investigated the electrochemical properties and potential-dependent stability of Cr(II) and Ni(II) in a eutectic LiCl-KCl molten salt at 500 °C under an argon atmosphere using a three-electrode cell configuration with a glassy carbon working electrode, Ag/Ag + reference electrode, and graphite counter electrode. Cyclic voltammetry was employed to characterize the Cr(0)/Cr(II)/Cr(III) and Ni(0)/Ni(II) redox transitions, yielding diffusion coefficients of 0.50 (±0.01) × 10 −5 cm 2 s −1 for Cr(II) and 0.91 (±0.16) × 10 −5 cm 2 s −1 for Ni(II) at 500 °C. The redox stability domains of these species provided insight into the corrosion mechanisms of a Ni-Cr alloy (80–20 wt %) in LiCl-KCl salt. The measured open circuit potential of the alloy corresponded to the range of potentials where the Ni(0) and Cr(II) species are stable, indicating a preferential dissolution of Cr. Immersion testing of the alloy for 336 h confirmed significant Cr depletion (or Ni-enrichment) at the surface layer, corroborating Cr dealloying as the dominant corrosion reaction under open circuit conditions. Additionally, the application of a small anodic overpotential (0.11 V) resulted in selective Cr dissolution while a large anodic overpotential (0.25 V) resulted in co-dissolution of both Cr and Ni. Furthermore, these results demonstrate that the corrosion mechanisms of a Ni-Cr alloy in LiCl-KCl depend upon the applied potential, and thus the redox conditions of the molten salt should be carefully controlled in the design of a redox buffer to mitigate corrosion in molten salt environments.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1982

Failure characteristics of graphite-epoxy structural components loaded in compression

Failure characteristics of compressively loaded graphite-epoxy components are described. Experimental results for both strength-critical laminates and structural components with postbuckling strength are presented. Effects of low speed impact damage and circular holes on compressive strength are discussed. Delamination and shear crippling failure mechanisms that limit the performance of strength-critical laminates are described. Transverse shear and skin-stiffener separation failure mechanisms that limit the performance of components with postbuckling strength are also described. The influence of matrix properties on compressive strength improvements for impact damaged laminates is discussed. Experimental data and results from a failure analysis for strength-critical laminates with cutouts are discussed and compared with impact damage results. Typical postbuckling test results are compared with analytical predictions.

Starnes, J. H., Jr.↗

NASA NTRS1983

Failure characteristics of graphite-epoxy structural components loaded in compression

Starnes, J. H., Jr.↗

NASA NTRS1998

"Long life" DC brush motor for use on the Mars surveyor program

DC brush motors have several qualities which make them very attractive for space flight applications. Their mechanical commutation is simple and lightweight, requiring no external sensing and control in order to function properly. They are extremely efficient in converting electrical energy into mechanical energy. Efficiencies over 80% are not uncommon, resulting in high power throughput to weight ratios. However, the inherent unreliability and short life of sliding electrical contacts, especially in vacuum, have driven previous programs to utilize complex brushless DC or the less efficient stepper motors. The Mars Surveyor Program (MSP'98) and the Shuttle Radar Topography Mission (SRTM) have developed a reliable "long life" brush type DC motor for operation in low temperature, low pressure CO2 and N2, utilizing silver-graphite brushes. The original intent was to utilize this same motor for SRTM's space operation, but the results thus far have been unsatisfactory in vacuum. This paper describes the design, test, and results of this development.

Braun, David↗

NASA NTRS2002

Structural Response of Compression-Loaded, Tow-Placed, Variable Stiffness Panels

Results of an analytical and experimental study to characterize the structural response of two compression-loaded variable stiffness composite panels are presented and discussed. These variable stiffness panels are advanced composite structures, in which tows are laid down along precise curvilinear paths within each ply and the fiber orientation angle varies continuously throughout each ply. The panels are manufactured from AS4/977-3 graphite-epoxy pre-preg material using an advanced tow placement system. Both variable stiffness panels have the same layup, but one panel has overlapping tow bands and the other panel has a constant-thickness laminate. A baseline cross-ply panel is also analyzed and tested for comparative purposes. Tests performed on the variable stiffness panels show a linear prebuckling load-deflection response, followed by a nonlinear response to failure at loads between 4 and 53 percent greater than the baseline panel failure load. The structural response of the variable stiffness panels is also evaluated using finite element analyses. Nonlinear analyses of the variable stiffness panels are performed which include mechanical and thermal prestresses. Results from analyses that include thermal prestress conditions correlate well with measured variable stiffness panel results. The predicted response of the baseline panel also correlates well with measured results.

Wu, K. Chauncey↗

NASA NTRS2013

A Comparison of Materials Issues for Cermet and Graphite-Based NTP Fuels

This paper compares material issues for cermet and graphite fuel elements. In particular, two issues in NTP fuel element performance are considered here: ductile to brittle transition in relation to crack propagation, and orificing individual coolant channels in fuel elements. Their relevance to fuel element performance is supported by considering material properties, experimental data, and results from multidisciplinary fluid/thermal/structural simulations. Ductile to brittle transition results in a fuel element region prone to brittle fracture under stress, while outside this region, stresses lead to deformation and resilience under stress. Poor coolant distribution between fuel element channels can increase stresses in certain channels. NERVA fuel element experimental results are consistent with this interpretation. An understanding of these mechanisms will help interpret fuel element testing results.

Nuclear Propulsion↗

DOE OSTI2020

Experimental Evaluation of Geopolymer, Nano-Modified, and Neat Class H Cement by Using Diametrically Compressive Tests

Abstract Cement is the prime barrier material to maintain zonal isolation during wellbore life-cycle. Different types of the cement have different performances on sealability. The primary objective of this study is evaluation of three types of cement systems, neat Class H, nano-synthetic graphite, and rock-based geopolymer cements, on interfacial bond integrity. Diametrical compressive tests are used on casing–cement–formation systems. Cement performances are tested in a conventional configuration (Berea Sandstone). A universal testing system is utilized to analyze the relationship applied load–axial strain and the digital image correlation (DIC) technique is used to generate the strain field maps. Based on the relationship and DIC results, bond strengths in different cement systems are evaluated. Additionally, microscope images provide insight explanations of the bond from micro-view. Based on the experimental results, failures of all cases initiate and propagate from the casing–cement interface. Then, radial cracks develop through the formation. This is because the mechanical interlocking bonds are formed only at the cement–sandstone interface to enhance the bond strength. The comparison of geopolymer and nano-modified cements with the conventional cement (neat Class H) shows that the unconventional cements have a lower maximum load and higher axial strain before failure of the samples. It indicates that both the two kinds of cements are more ductile than conventional cement and can support more deformation before the initiation of cracks.

Energy & Fuels↗

DOE OSTI2015

AGR-3/4 Final Data Qualification Report for ATR Cycles 151A through 155B-1

This report provides the qualification status of experimental data for the entire Advanced Gas Reactor 3/4 (AGR 3/4) fuel irradiation. AGR-3/4 is the third in a series of planned irradiation experiments conducted in the Advanced Test Reactor (ATR) at Idaho National Laboratory (INL) for the AGR Fuel Development and Qualification Program, which supports development of the advanced reactor technology under the INL ART Technology Development Office (TDO). The main objective of AGR-3/4 irradiation is to provide a known source of fission products for subsequent transport through compact matrix and structural graphite materials due to the presence of designed-to-fail fuel particles. Full power irradiation of the AGR 3/4 test began on December 14, 2011 (ATR Cycle 151A), and was completed on April 12, 2014 (end of ATR Cycle 155B) after 369.1 effective full power days of irradiation. The AGR-3/4 test was in the reactor core for eight of the ten ATR cycles between 151A and 155B. During the unplanned outage cycle, 153A, the experiment was removed from the ATR northeast flux trap (NEFT) location and stored in the ATR canal. This was to prevent overheating of fuel compacts due to higher than normal ATR power during the subsequent Powered Axial Locator Mechanism cycle, 153B. The AGR 3/4 test was inserted back into the ATR NEFT location during the outage of ATR Cycle 154A on April 26, 2013. Therefore, the AGR-3/4 irradiation data received during these 2 cycles (153A and 153B) are irrelevant and their qualification status isnot included in this report. Additionally, during ATR Cycle 152A the ATR core ran at low power for a short enough duration that the irradiation data are not used for physics and thermal calculations. However, the qualification status of irradiation data for this cycle is still covered in this report. As a result, this report includes data from 8 ATR Cycles: 151A, 151B, 152A, 152B, 154A, 154B, 155A, and 155B, as recorded in the Nuclear Data Management and Analysis System (NDMAS). The AGR 3/4 data streams addressed in this report include thermocouple (TC) temperatures, sweep gas data (flow rates, pressure, and moisture content), and Fission Product Monitoring System (FPMS) data (release rates, release to birth rate ratios [R/Bs], and particle failure counts) for each of the twelve capsules in the AGR 3/4 experiment. During Outage Cycle 155A, fourteen flow meters were installed downstream from fourteen FPMS monitors to measure flows from the monitors; qualification status of these data are also included in the report. The final data qualification status for these data streams is determined by a Data Review Committee (DRC) composed of AGR technical leads, Sitewide Quality Assurance (QA), and NDMAS analysts. For ATR Cycles 151A through 154B, the DRC convened on February 12, 2014, reviewed the data acquisition process, and considered whether the data met the requirements for data collection as specified in QA approved INL ART TDO data collection plans. The DRC also examined the results of NDMAS data testing and statistical analyses, and confirmed the qualification status of the data as given in this report. The qualification status of AGR-3/4 irradiation data during the first six cycles were previously reported in INL/EXT-14-31186 document. This report presents data qualification status for the entire AGR-3/4 irradiation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2022

Perspective on “code qualifying” new graphite grades for use in advanced nuclear reactors*

The American Society of Mechanical Engineers (ASME) publishes the Boiler and Pressure Vessel (BPV) Code, which include guidance for the safe development, construction, and operation of boilers and pressure vessels. ASME BPV Code Section III “Rules for Construction of Nuclear Facility Components” Division 5 focuses on “High Temperature Reactors”. Subsection HH, subpart A lists the different materials properties that are to be measured and how those properties change due to different environmental conditions (oxidation and irradiation damage) for a graphite to be accepted for use in a high temperature reactor core (i.e., “Code Qualified”). Currently there are no nuclear graphite grades that are “Code Qualified” (i.e., a reactor designer can select a graphite grade and build their reactor without any additional testing), which is due in part to development of new graphite grades in the last 20 years and the lack of comprehensive programs needed to produce the data for the code cases. This perspective is going to discuss the requirements, as called out in the ASME BPV Code, that are necessary to “code qualify” a nuclear graphite grade but will primarily focus on the practical and technical challenges associated with irradiation-induced property changes and how to address these to assist with getting graphite ready for use in advanced nuclear reactors. These same technical challenges can be expected to arise for other materials being developed for advanced reactor concepts.

advanced nuclear reactors↗

NASA NTRS1991

Temperature effects on high strain rate properties of graphite/epoxy composites

A unidirectional graphite epoxy material (AS4/3501-6) was characterized at strain rates ranging from 5 x 10(exp 6) s(exp -1) to 5(exp -1), at room temperature and at 128 C. Results are presented in the form of stress-strain curves to failure. The longitudinal properties remain nearly unchanged with strain rate and temperature. The transverse modulus increases with strain rate but decreases with temperature. The transverse strength and transverse ultimate tensile strain have a positive rate sensitivity at low rates, which changes to negative at intermediate rates and returns to positive rate sensitivity at the highest rates tested. A temperature-time equivalence principle was applied and master curves were obtained for the transverse mechanical properties. The in-plane shear modulus and in-plane shear strength have a positive rate sensitivity. The ultimate intralaminar shear strain has a positive rate sensitivity at low rates, which changes to negative at high rates. At the elevated temperature of 128 C, the ultimate shear strain is 25 to 30 percent higher than the room temperature value, but its strain rate dependence is moderate.

Yaniv, G.↗

DOE OSTI2021

Effects of 18 O Exchange on Neutron Emission Rates of Aging 238 PuO 2 LWRHUs

The Lightweight Radioisotope Heater Unit (LWRHU) provides about 1 Watt of thermal power to critical electrical and mechanical systems in the extreme temperatures of space, maintaining the operating temperature of the spacecraft’s scientific and general operating equipment. Los Alamos National Laboratory (LANL) designed and tested the LWRHU in the 1970s through early 1980s. The first production campaign at LANL was in the early 1980s in support of the Galileo mission in which over 100 LWRHUs were manufactured. In the mid-1990s, almost 200 LWRHUs were manufactured in support of the Cassini mission. After the primary Cassini manufacturing campaign, the Department of Energy (DOE) approved the fabrication of more than 10 additional LWRHUs as spares in 1998. The LWRHU assembly contains the following components: a fuel pellet, a vented capsule, a pyrolytic graphite insulator, and a fine-weave pierced fabric (FWPF) graphite aeroshell. The fuel pellet is a hot-pressed 238 PuO 2 cylindrical pellet that is sintered to create a ceramic pellet. The pellet is encapsulated in a platinum-rhodium encapsulation. The welded fueled clad is placed inside a pyrolytic graphite thermal insulation to protect the fuel from the heat produced in reentry events. The exterior layer of the LWRHU assembly is the FWPF aeroshell. Before sintering, PuO 2 granules are heated in a furnace at temperatures greater than or equal to 700°C under an enriched 16 O atmosphere in order to reduce trace quantities of 18 O. Because 18 O undergoes an (α,n) reaction, 18 O needs to be removed as much as possible to meet radiation emission requirements set by the Jet Propulsion Laboratory (JPL) and the National Aeronautics and Space Administration (NASA), as well as other agencies. The relative abundances of the oxygen isotopes are indicated by neutron emission rate (NER) measurements. LWRHUs are vented with a sintered platinum frit vent (George 1986). During extraterrestrial operation, the vent in the cladding allows helium from the decay of plutonium to escape and relieves pressure from the system while preventing the solids from escaping (Rinehart 1996, Tate 1982 & 1985). This vent is protected during manufacture by a platinum-30 rhodium cover. The capsule vent is activated by milling a 0.025-inch diameter hole through the protective cover to a nominal depth of 0.015 inches, generally immediately before the LWRHU is loaded into the aeroshell (George 1986). Prior to long-term storage, LWRHUs are vented and thus potentially allow infiltration of 18 O from the ambient atmosphere. Although NER decreases with age due to the reduction in emitted alpha particles, it might be expected that NER reduction is mitigated by the exchange of 18 O. However, this is not necessarily the case and no trend was observed relating NER to age other than the natural decay of 238 Pu (Mulford 2021). The most probable and dominant factor for determining specific NER was manufacturing discrepancies between individual units. It is important to understand the lack of observed 16 O- 18 O exchange and to compare LWRHU pellets as much as possible.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2013

Ellipsometry with polarisation analysis at cryogenic temperatures inside a vacuum chamber

In this paper we describe a new variant of null ellipsometry to determine thicknesses and optical properties of thin films on a substrate at cryogenic temperatures. In the PCSA arrangement of ellipsometry the polarizer and the compensator are placed before the substrate and the analyzer after it. Usually, in the null ellipsometry the polarizer and the analyzer are rotated to find the searched minimum in intensity. In our variant we rotate the polarizer and the compensator instead, both being placed in the incoming beam before the substrate. Therefore the polarisation analysis of the reflected beam can be realized by an analyzer at fixed orientation. We developed this method for investigations of thin cryogenic films inside a vacuum chamber where the analyzer and detector had to be placed inside the cold shield at a temperature of T≈ 90 K close to the substrate. All other optical components were installed at the incoming beam line outside the vacuum chamber, including all components which need to be rotated during the measurements. Our null ellipsometry variant has been tested with condensed krypton films on a highly oriented pyrolytic graphite substrate (HOPG) at a temperature of T≈ 25 K. We show that it is possible to determine the indices of refraction of condensed krypton and of the HOPG substrate as well as thickness of krypton films with reasonable accuracy.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2019

Influence of Austempering Temperature and Time on the Microstructure and Mechanical Properties of Ductile Iron Weldment Using Developed Coated Electrode

Sound welded joints of ductile iron were first made by developing coated electrodes as well as weld procedure. The weldments were then austenitized at 900 °C for 2-h holding time followed by austempering at 300 and 350 °C for three different holding times (1.5, 2 and 2.5 h) at each austempering temperature. The influence of austempering temperature and time on the microstructural and mechanical properties was studied. Microstructural characterization, phase analysis, microhardness and mechanical properties were performed to understand the effect of austempering heat treatment on microstructure, austempering kinetics and mechanical properties of welded joints. In spite of significant variation in microstructures among all the three zones of DI weldment before austempering, the response of both weld metal and HAZ to austempering heat treatment similar to a base metal was noted. However, a significant variation in matrix structures (bainitic ferrite, retained austenite) as well as graphite nodules among the three zones was observed with changing the austempering temperature and holding time. Also, 100% joint efficiency of the welded joints was achieved at both 300 and 350 °C for 2-h holding time. Hardness and charpy impact toughness mostly depended on the volume fraction of retained austenite and carbon content. Based on the results of tensile and charpy impact testing, 350 °C and 2-h holding time could be considered as an optimum austempering condition for ADI weldment.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Experimental Study and Computational Simulations of Key Pebble Bed Thermo-mechanics Issues for Design and Safety

An experimental and computational study, consisting of modeling and simulation (M&S), of key thermal-mechanical issues affecting the design and safety of pebble-bed (PB) reactors was conducted. The objective was to broaden understanding and experimentally validate thermal-mechanic phenomena of nuclear grade graphite, specifically, spheres in frictional contact as anticipated in the bed under reactor relevant pressures and temperatures. The contact generates graphite dust particulates that can subsequently be transported into the flowing gaseous coolent. Under postulated depressurization transients and with the potential for leaked fission products to be adsorbed onto graphite 'dust', there is the potential for fission products to escape from the primary volume. This is a design safety concern. Furthermore, earlier safety assessment identified the distinct possibility for the dispersed dust to combust in contact with air if sufficient conditions are met. Both of these phenomena were noted as important to design review and containing uncertainty to warrant study. The team designed and conducted two separate effects tests to study and benchmark the potential dust-generation rate, as well as study the conditions under which a dust explosion may occure in a standardized, instrumented explosion chamber.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1988

Thermal properties of composites with bismaleimide-vinyl poly(styrylpyridine) blends

Thermal properties, flammability, and selected mechanical properties of eight different graphite composite panels fabricated using four different resin matrices and two types of graphite reinforcement were investigated and compared with the properties of an epoxy composite, MXB 7203. The resin matrices included XU71775/H795, a blend of vinyl poly(styrylpyridine) and bismaleimide; H795, a bismaleimide; Cycom 6162, a phenolic; and PSP 6022M, a poly(styrylpyridine). The graphite fiber was AS-4 used in the form of tape or fabric. It was found that the XU71775/H795 blend with the graphite tape was the optimum design giving the lowest heat release rate, while the control epoxy panel exhibited the highest total heat release and heat release rates, highest smoke and CO evolution, highest mass losses, and lowest oxygen index of all the composites tested.

Kourtides, D. A.↗

DOE OSTI2021

Oxidation behaviors of matrix-grade graphite during water vapor ingress accidents for high temperature gas-cooled reactors

Water ingress into cores of high temperature gas-cooled reactors (HTGRs) can cause serious safety problems in graphitic components, especially for matrix graphite, which is more vulnerable than nuclear graphite. Here in this study, oxidation behaviors of a matrix-grade graphite, ARB-B1, were investigated under simulated water ingress accidental conditions. The oxidation tests were conducted in water vapor/helium mixed atmospheres at elevated temperatures up to 1200 °C. Oxidation rates and activation energy were evaluated by mass loss measurements. The activation energy was 121.5 kJ/mol in the considered temperature range, indicating only one oxidation regime-in-pore diffusion assisted by cracks. The cracks originated from the fabrication process, acting as penetration paths for the oxidant, played an important role in the oxidation behaviors. Ungraphitized binder oxidation occurred at all temperatures, while apparent oxidation of filler particles started from 1100 °C. Moreover, oxidation effects on compressive properties and hardness of the matrix graphite were discussed in terms of oxidized microstructures. This first detailed study on matrix graphite oxidation in water vapor provides important kinetics knowledge and microstructural and mechanical data for accidental scenarios of HTGRs as well as for development of new matrix graphite materials.

36 MATERIALS SCIENCE↗

DOE OSTI2023

ANS MiNES 2023 Poster

The dynamic mechanical properties of four varieties of high purity graphite as well as the depth of penetration (DoP) of a small-scale shaped charge into these grades was experimentally determined. The grades chosen were PCEA, NBG-18, and NBG-25. These grades provide a wide range of physical properties: in density from 1.80 – 1.85 g/cc, in maximum particle size from 10s to 1000s of µm, and in porosity from 18% to 20%. The quasistatic and dynamic compressive strengths of each grade were determined and correlated to their physical properties. The split Hopkinson pressure bar experiments showed both the dynamic strength and dominant shear failure mechanisms. A small scale shaped charge was used to compare the resistance of graphite to hypervelocity jet impacts: the Teledyne RP-4. The RP-4 has a 1.01” outer diameter and 3.44 g of RDX with an RP-80 booster (86 mg PETN + 123 mg RDX). A select number of samples were analyzed using X-Ray Computed Tomography (XCT), allowing for the full characterization of the undisturbed wound channel. A selection of other samples were physically sectioned and wound channels mapped from the sections. In addition to DoP, the wound geometry was characterized in terms of total volume and diameter at different depths. The wound channel characteristics for each grade were correlated to the compressive strengths and physical properties. In several of the test samples, the wound channel diameter was smaller than the diameter of the shaped charge slug just behind where the slug had penetrated the sample. These results indicated that the wound geometry was dependent on the compressive hysteresis behavior of graphite.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Experimental Investigation of the Impact of Cathode Grade on Sludge Formation at the Cathode Block-Aluminum Interface of Hall–Héroult Cells

The presence of resistive sludge on the cathode surface in Hall–Héroult cells can increase the aluminum production costs and reduces cell lifetime. Modern cells with graphitized cathode blocks generally operate satisfactorily but some are exhibiting excessive deposit formation, thus lower performances. Little attention has ever been given to the role of the cathode grade and its properties on sludge formation. In this investigation, five graphitized industrial cathode grades with varying properties are tested on a bench scale aluminum electrolysis setup with cathodic current density of 0.9 A/cm{sup 2}, under a nitrogen atmosphere at 1233 K (960 °C) for 8 hours with initial bath composition of 10 pct alumina, cryolite ratio of 2.2, 5 pct CaF{sub 2} and no point feeding. Postmortem characterization includes Rietveld refinement of deposits, optical microscopy and SEM-EDS observations of the carbon-aluminum interface. Sludge located near the center of the cathode surface was generated during the experiments despite the absence of point feeding. The sludge profile was variable among grades and could be related to the horizontal and vertical thermal conductivities of the blocks. This study has pushed further the understanding of the mechanisms of sludge formation and dissolution concerning the cathode grade properties.

36 MATERIALS SCIENCE↗