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Friction and wear of nuclear graphite exposed to molten FLiNaK salt environment

This report formally documents the completion of the Advanced Reactor Technologies Level 3 Milestone (M3TG-25OR0501104), “Initiate graphite wear studies of graphite samples exposed to molten salt environment,” due August 1, 2025. The report summarizes the ongoing activities aimed at characterizing the friction and wear behavior of graphite in molten LiF–NaF–KF (FLiNaK) salt environment. The wear and friction behavior of self-mated ET-10 nuclear graphite were tested at varying temperatures (550°C and 650°C), contact loads (40 and 80 N) and sliding speeds (1 and 10 mm/s) in a controlled argon environment. The results were compared to the wear and friction behavior of the same graphite material in a dry argon environment. This report presents initial studies on the friction and wear behavior of graphite in sliding contact mode, with future work focused on investigating the graphite matrix materials, as well as rolling and impact contact modes. The outcomes of this report could provide insights into assessing the integrity of the graphitic components of pebble-bed fluoride salt–cooled high-temperature reactors (PB-FHRs) to enhance their safe operation.

22 GENERAL STUDIES OF NUCLEAR REACTORS

Research on Graphite Reinforced Glass Matrix Composites

This report contains the results obtained in the first twelve months of research under NASA Langley Contract NAS1-14346 for the origination of graphite-fiber reinforced glass matrix composites. Included in the report is a summary of the research by other investigators in this area. The method selected to form the composites consisted of pulling the graphite fiber through a slurry containing powdered glass, winding up the graphite fiber and the glass it picks up on a drum, drying, cutting into segments, loading the tape segment into a graphite die, and hot pressing. During the course of the work, composites were made with a variety of graphite fibers in a C.G.W. 7740 (Pyrex) glass matrix. The graphite fibers used included Hercules HMS, Hercules HTS, Thornel 300S, and Celanese DG-102 and, of these, the Hercules HMS and Celanese DG-102 graphite fibers in C.G.W. 7740 gave the most interesting but widely different results. Hercules HMS fiber in C.G.W. 7740 glass (Pyrex) showed an average four-point flexural strength of 848 MPa or 127,300 psi. As the test temperature was raised from room temperature to 560 C in argon or vacuum, the strength was higher by 50 percent. However, in air, similar tests at 560 C gave a severe loss in strength. These composites also have good thermal cycle properties in argon or vacuum, greatly increased toughness compared to glass, and no loss in strength in a 100 cycle fatigue test. Celanese DG-102 fiber in C.G.W. 7740 glass (Pyrex) had a much lower flexural strength but did not suffer any loss in this strength when samples were heated to 560 C in air for 4 hrs.

Bacon, J. F.

Research on graphite reinforced glass matrix composites

High levels of mechanical performance in tension, flexure, fatigue, and creep loading situations of graphite fiber reinforced glass matrix composites are discussed. At test temperatures of up to 813 K it was found that the major limiting factor was the oxidative instability of the reinforcing graphite fibers. Particular points to note include the following: (1) a wide variety of graphite fibers were found to be comparable with the glass matrix composite fabrication process; (2) choice of fiber, to a large extent, controlled resultant composite performance; (3) composite fatigue performance was found to be excellent at both 300 K and 703 K; (4) composite creep and stress rupture at temperatures of up to 813 K was limited by the oxidative stability of the fiber; (5) exceptionally low values of composite thermal expansion coefficient were attributable to the dimensional stability of both matrix and fiber; and (6) component fabricability was demonstrated through the hot pressing of hot sections and brazing using glass and metal joining phases.

Prewo, K. M.

Graphite fiber reinforced glass matrix composites for aerospace applications

The graphite fiber reinforced glass matrix composite system is described. Although this composite is not yet a mature material, it possesses low density, attractive mechanical properties at elevated temperatures, and good environmental stability. Properties are reported for a borosilicate glass matrix unidirectionally reinforced with 60 volume percent HMS graphite fiber. The flexural strength and fatigue characteristics at room and elevated temperature, resistance to thermal cycling and continuous high temperature oxidation, and thermal expansion characteristics of the composite are reported. The properties of this new composite are compared to those of advanced resin and metal matrix composites showing that graphite fiber reinforced glass matrix composites are attractive for aerospace applications.

Prewo, K. M.

Post-irradiation examination of AGR-3/4 TRISO fuel compacts using three-dimensional X-ray computed tomography

The AGR-3/4 irradiation tests combined the third and fourth planned irradiation experiments in the US Department of Energy’s Advanced Gas Reactor (AGR) testing campaign of tri-structural isotropic (TRISO) fuel compacts. In this article, we present post-irradiation examination (PIE) using X-ray computed tomography (XCT) of two unirradiated and two irradiated compacts from the AGR-3/4 irradiation tests. The irradiated compacts studied (compact 7–1 and compact 12–4) represent the upper and lower limit of burnup within the AGR-3/4 irradiation experiment. This article presents a detailed quantitative analysis on the post-irradiation structure of TRISO fuel compacts. Various quantitative parameters including shape, size, and packing of kernels, and their spatial distribution, were utilized to gain insights into the structural changes caused by irradiation. The equivalent diameter and sphericity were found to increase and decrease, respectively, in irradiated compact 7–1 due to its higher burnup. Nearest neighbor distance between fuel kernels decreased after irradiation, suggesting irradiation-induced shrinkage of graphitic matrix. Furthermore, each compact in AGR-3/4 irradiation tests contained 20 designed-to-fail (DTF) fuel particles that were meant to act as a source of fission product release to the experiment test train. Furthermore, in the present work, all DTF fuel particles in the four compacts studied were identified, and it was found that they exhibited larger kernel swelling in compact 12–4 and smaller kernel swelling in compact 7–1, compared to the driver particles.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Study of the dissociation of molecular hydrogen

Dissociators used to obtain an RF plasma discharge for hydrogen masers and the test system used for operation and evaluation of the dissociators are described. A compact sorption cartridge using a graphite matrix is tested as part of a hydrogen scavenging system. Testing of a vacuum enclosed hydrogen dissociator suitable for long term operation in space is described.

Vessot, R. F. C.

AGR Fuel Oxidation Testing Summary and Plans

This presentation describes the goals, scope, and plans for oxidation testing of (primarily irradiated) AGR TRISO fuels and related materials (such as graphite and graphitic matrix material). This presentation will be given at the annual program review meeting for the Gas-cooled Reactor program hosted at INL starting on July 16.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Post-irradiation 1600°C Heating Test of AGR-1 UCO Fuel Kernels

Five bare kernels were selected from the U.S. Advanced Gas Reactor (AGR) 1 irradiation experiment Compact 5-3-1 to perform post-irradiation safety tests. The safety test involved heating the kernels in the Fuel Accident Condition Simulator (FACS) furnace in the inert atmosphere to a peak temperature of 1600°C and isothermally holding at this temperature for about 47 hours while collecting fission products released. This test was to assess the retention of fission products in bare kernels without the effects of the other TRISO layers (buffer, IPyC, SiC, and OPyC) or the graphitic matrix material. The bare kernels released nearly 100% of cesium and antimony, while they were able to maintain about 30% of europium, 50% of strontium, and the majority of cerium and ruthenium. In addition, about 48% of the calculated inventory of Kr-85 released during the test, indicating that kernels were capable of retaining a considerable fraction of fission gas K-85 during irradiation.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Fuel performance analysis of fully-resolved TRISO compact

The TRi-structural ISOtropic (TRISO) fuel multilayered coating structure offers multiple barriers to fission product release, enhancing safety and performance. The heterogeneous nature of TRISO fuel compacts, comprising thousands of randomly distributed coated fuel particles embedded in a graphite matrix, creates intricate stress fields and thermal gradients that cannot be accurately modeled using simplified one-dimensional or homogenized approaches. Consequently, three-dimensional modeling enables the prediction of fuel compact dimensional changes, internal pressure buildup, and fission product transport pathways under diverse irradiation and thermal conditions. This capability facilitates detailed analysis of particle-to-particle interactions, matrix cracking mechanisms, and the statistical distribution of coating failures, which directly impact fuel performance and safety margins. This capability is particularly critical for advanced reactors, such as high-temperature gas-cooled reactors and other Generation IV reactor designs where TRISO fuel operates at elevated temperatures and burn-up levels. This work introduces a novel method to generate an optimized packing of TRISO compacts and a complete 3D mesh with random distribution of TRISO particles, which are discretized into each coating component layer.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

3D TRISO particle-explicit compact meshing

The TRI-structural ISOtropic (TRISO) layered fuel particle is a robust nuclear fuel form offering enhanced safety and performance for advanced reactor concepts, including high-temperature gas-cooled reactors and other Generation IV designs. These poppy-seed-sized particles are embedded in a graphite matrix to form fuel elements that must withstand elevated temperatures and high burn-up levels. The heterogeneous nature of these fuel elements — comprising thousands of randomly distributed TRISO particles — produces complex stress fields and thermal gradients that one- and two-dimensional models cannot accurately capture. While three-dimensional modeling has improved predictions of dimensional changes, internal pressure buildup, and fission product transport under irradiation, current approaches rely on homogenized material properties that are known to have considerable divergence from experimental observations. This work presents a methodology for optimized random packing of TRISO fuel compacts and full three-dimensional mesh generation within the BISON fuel performance code, with each particle coating layer individually discretized. The resulting mesh was demonstrated through heat conduction simulations under representative in-reactor operating conditions, showing strong agreement with expected behavior. This capability enables detailed analysis of particle-to-particle interactions, matrix cracking mechanisms, and the statistical distribution of coating layer failures — all of which directly govern fuel performance and safety margins.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS

Space environmental effects on LDEF low Earth orbit exposed graphite reinforced polymer matrix composites

The Long Duration Exposure Facility (LDEF) was deployed on April 7, 1984 in low earth orbit (LEO) at an altitude of 482 kilometers. On board experiments experienced the harsh LEO environment including atomic oxygen (AO), ultraviolet radiation (UV), and thermal cycling. During the 5.8 year mission, the LDEF orbit decayed to 340 kilometers where significantly higher AO concentrations exist. LDEF was retrieved on January 12, 1990 from this orbit. One experiment on board LDEF was M0003, Space Effects on Spacecraft Materials. As a subset of M0003 nearly 500 samples of polymer, metal, and glass matrix composites were flown as the Advanced Composites Experiment M0003-10. The Advanced Composites Experiment is a joint effort between government and industry with the Aerospace Corporation serving as the experiment integrator. A portion of the graphite reinforced polymer matrix composites were furnished by the Boeing Defense and Space Group, Seattle, Washington. Test results and discussions for the Boeing portion of M0003-10 are presented. Experiment and specimen location on the LDEF are presented along with a quantitative summary of the pertinent exposure conditions. Matrix materials selected for the test were epoxy, polysulfone, and polyimide. These composite materials were selected due to their suitability for high performance structural capability in spacecraft applications. Graphite reinforced polymer matrix composites offer higher strength to weight ratios along with excellent dimensional stability. The Boeing space exposed and corresponding ground control composite specimens were subjected to post flight mechanical, chemical, and physical testing in order to determine any changes in critical properties and performance characteristics. Among the more significant findings are the erosive effect of atomic oxygen on leading edge exposed specimens and microcracking in non-unidirectionally reinforced flight specimens.

George, Pete

Burning characteristics and fiber retention of graphite/resin matrix composites

Graphite fiber reinforced resin matrix composites were subjected to controlled burning conditions to determine their burning characteristics and fiber retention properties. Two types of burning equipment were used. Small samples were burned with a natural gas fired torch to study the effects of fiber orientation and structural flaws such as holes and slits that were machined into the laminates. Larger laminate samples were burned in a Heat Release Rate Calorimeter. Unidirectional epoxy/graphite and polyimide/graphite composites and boron powder filled samples of each of the two composite systems were burn tested and exposed to a thermal radiation. The effects of fiber orientation, flaws, and boron filler additives to the resins were evaluated. A high char forming polyimide resin was no more effective in retaining graphite fibers than a low char forming epoxy resin when burning in air.

Bowles, K. J.

Burning characteristics and fiber retention of graphite/resin matrix composites

Graphite fiber reinforced resin matrix composites were subjected to controlled burning conditions to determine their burning characteristics and fiber retention properties. Small samples were burned with a natural gas fired torch to study the effects of fiber orientation and structural flaws such as holes and slits that were machined into the laminates. Larger laminate samples were burned in a modified heat release rate calorimeter. Unidirectional epoxy/graphite and polyimide/graphite composites and boron powder filled samples of each of the two composite systems were burn tested. The composites were exposed to a thermal radiation of 5.3 Btu/sq ft-sec in air. Samples of each of the unfilled composite were decomposed anaerobically in the calorimeter. Weight loss data were recorded for burning and decomposition times up to thirty-five minutes. The effects of fiber orientation, flaws, and boron filler additives to the resins were evaluated. A high char forming polyimide resin was no more effective in retaining graphite fibers than a low char forming epoxy resin when burned in air. Boron powder additions to both the polyimide and the epoxy resins stabilized the chars and effectively controlled the fiber release.

Bowles, K. J.

Styrene-terminated polysulfone oligomers as matrix material for graphite reinforced composites - An initial study

Results pertaining to graphite reinforced composites containing styrene-terminated oligomers as the matrix material are summarized. The processing parameters are determined and the properties of the resulting composite are evaluated. In terms of solvent impregnation techniques, CH2Cl2 is the preferred solvent due to its easy removal during the prepreg drying and consolidation steps.

Garcia, Dana

Research on graphite reinforced glass matrix composites

A composite that can be used at temperatures up to 875 K with mechanical properties equal or superior to graphite fiber reinforced epoxy composites is presented. The composite system consist of graphite fiber, uniaxially or biaxially, reinforced borosilicate glass. The mechanical and thermal properties of such a graphite fiber reinforced glass composite are described, and the system is shown to offer promise as a high performance structural material. Specific properties that were measured were: a modified borosilicate glass uniaxially reinforced by Hercules HMS graphite fiber has a three-point flexural strength of 1030 MPa, a four-point flexural strength of 964 MPa, an elastic modulus of 199 GPa and a failure strain of 0.0052. The preparation and properties of similar composites with Hercules HTS, Celanese DG-102, Thornel 300 and Thornel Pitch graphite fibers are also described.

Bacon, J. F.

Glass matrix composites. I - Graphite fiber reinforced glass

An experimental program is described in which graphite fibers of Hercules HMS and HTS, Thornel 300, and Celanese DG-12 were used to reinforce, both uniaxially and biaxially, borosilicate pyrex glass. Composite flexural strength distribution, strength as a function of test temperature, fracture toughness and oxidative stability were determined and shown to be primarily a function of fiber type and the quality of fiber-matrix bond formed during composite fabrication. It is demonstrated that the graphite fiber reinforced glass system offers unique possibilities as a high performance structural material.

Prewo, K. M.

New bismaleimide matrix resins for graphite fiber composites

Two new bismaleimide resins based on the N,N'-m-phenylene-bis(m-amino-benzamide) structure have been synthesized and characterized. The mixtures of the two resins gave better handling, processing, mechanical, and thermal properties in graphite composites than did the individual resins. The mechanical strength of the cured graphite composites prepared from the 1:1 copolymer of the two bismaleimide resins was excellent at both ambient and elevated temperatures. The physical and mechanical properties of the composites from the new bismaleimide matrix resin systems are compared with conventional composites based on epoxy and other bismaleimide systems. The copolymer system provides another method for improving bismaleimide resins.

Hsu, M.-T. S.