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Elevated Temperature Graphite Mechanical Testing

High purity graphite will be used for core components within most High Temperature Reactor (HTR) designs. Several "high tech” industries currently utilize synthetic, high-purity, commercially available graphite components to fabricate photovoltaic cells, semi-conductors, optical fibers, and other high value electronic industry products. New advanced HTR designs are also interested in using these graphite grades for long-term, internal core component applications. Consequently, the US Department of Energy, Advanced Reactor Technologies (DOE-ART) program has spent several years testing different high purity graphite grades for potential use within these new nuclear reactor designs. A significant part of that effort has been in the development and improvement of American Society for Testing and Materials (ASTM) test standards specifically for nuclear graphite grades. Nearly all ASTM test standards have either been developed or improved by the DOE-ART program over the past 25 years. The ART program continues to assist in the development of new ASTM test standards in support of the future commercial HTR fleet currently being designed and built in the USA. The newest effort undertaken by ART is the development of high temperature mechanical testing practices that may be acceptable for a future ASTM test standard (or guide) for this critical material property measurement.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

An investigation of fracture behaviors of NBG-18 nuclear graphite using in situ mechanical testing coupled with micro-CT

Nuclear graphite contains defects spanning from nanoscale basal cracks to sub-mm scale voids. This study aims to establish an experimental method to investigate pre-existing defects and 3-D crack growth inside nuclear graphite, NBG-18. Three-point bending tests were performed on single-edge notched beam specimens with and without coupling with micro-CT. The fracture toughness was measured to be 1.17 ± 0.06 MPa $\sqrt{{m}}$. Cracks were observed to initiate from the pores and thermal cracks on the edge of the notch and then defect or twist to grow along the pre-existing defects. Crack bridging, defection, and twisting were the primary toughening mechanisms. The crack resistance curve exhibited a trend of rising-plateau-rising that can be related to the interaction of crack front and the pre-existing defects. In conclusion, the results highlight the capability of laboratory micro-CT-based experimental method for the visualization of multi-scale defect interactions, which remains to be a challenge in the characterization of nuclear graphite.

36 MATERIALS SCIENCE↗

Evaluating alternate test techniques to characterize mechanical properties in nuclear-grade graphites - 18421

The deployment of graphite as a core structural material in the very high temperature reactor (VHTR) design presents a number of challenges with regard to accurate property and performance assessments. In the United States Advanced Reactor Technologies (ART) program, candidate VHTR graphite grades are being evaluated not only with respect to irradiated property values, but also with a focus on comprehensive data sets that explicate the property variability inherent to nuclear-grade graphites. The large data sets being compiled on baseline physical and mechanical properties provide a means not only to quantify variability within and between major graphite grades, but also to evaluate test techniques utilized on irradiated specimens that are severely limited in size and geometry. Detailed appraisals of emerging mechanical test techniques that either (a) fall outside of the prescribed test size and configuration constraints in order to be assembled into irradiation capsule such as the three-point bend test on sub-sized cylinders or (b) are not yet fully evaluated and standardized by ASTM International such as the Brazilian disc splitting tensile strength test can be more accurately generated when a broad comparison is possible that leverages multiple mechanical tests on full-size specimens using approved standards. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Initial Split Disk Mechanical Testing Studies with a Digital Image Correlator

Nuclear graphite plays a pivotal role in the advanced reactor program. Consequently, developing a viable method to measure and evaluate small samples is essential. The Digital Image Correlation (DIC) technique allows for the examination of much smaller components in real-time applications, particularly concerning reactor capsule design and placement within the reactor. These samples become crucial for understanding the behavior of nuclear graphite before and after radiation exposure. They serve as a means to analyze changes and effectively measure the mechanical strength properties, which may or may not alter following irradiation.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Mechanical behavior analysis using small-size graphite disc compression testing with digital image correlation methods

The ASTM International Standard Test Method for Tensile Stress-Strain of Carbon and Graphite (ASTM C749) requires dog-bone shaped specimens. Unfortunately, specimen sizes required in ASTM C749 are much too large for irradiation within a test reactor and are incompatible with irradiation capsule volumes, molten salt degradation facilities, or oxidation apparatus. The ASTM International Standard Test Method for Tensile Strength Estimate by Disc Compression of Manufactured Graphite (ASTM D8289) was developed as an alternative that provides a means for testing tensile properties using smaller specimens when geometric constraints are present. However, the important stress–strain relation throughout the test loading history that could be recorded using ASTM C749 is lost by using ASTM D8289 because of the difficulties involved with using traditional strain gauges or extensometers on such a small specimen. In this work, a digital image correlation (DIC) method, which uses a full-field noncontact surface displacement measurement technique, was applied along with the ASTM D8289 splitting tensile test on eight small samples of graphite grade Mersen 2114 to track their deformation during compressive loading. Initial results showed that the DIC technique can measure the surface displacement/strain on these small (Ø6 × 3 mm) graphite specimens with high accuracy and good repeatability, indicating that the DIC technique, combined with the small-disc splitting tensile test in ASTM D8289, can capture the strain evolution in the test. In conclusion, further comparison of measured strains with analytical and numerical simulation results provides additional understanding of the mechanical behaviour of this nuclear graphite material in complex stress states.

36 MATERIALS SCIENCE↗

Machining Graphite Specimens from Sub- Blocks for Baseline Characterization

The Advanced Reactor Technologies (ART) Baseline Graphite Characterization program at the Idaho National Laboratory (INL) is performing a comprehensive evaluation of inter-billet variations in as-produced nuclear-grade graphite. To accomplish this, over 500 mechanical test specimens are machined from a single billet. A typical graphite billet is approximately 6 feet long by 2 feet in diameter or 2 ft square and weighs approximately 1500 pounds. Initially the full-size billets are pre-sectioned into sub-blocks that can be easily handled and shipped. In this SOW, 44 pre-labeled sub-blocks will be machined into mechanical test specimens by the supplier. These sub-blocks are supplied and shipped by the purchaser to the supplier.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

AGC 3 Irradiated Material Properties Analysis

This report documents the analysis of the irradiated material property data from the Advanced Graphite Creep (AGC)-3 graphite specimens. This is the third in a series of six irradiation test trains planned as part of the AGC experiment to fully characterize the neutron irradiation effects and radiation creep behavior of current nuclear graphite grades. The AGC-3 capsule was irradiated in the Idaho National Laboratory Advanced Test Reactor at a nominal temperature of 800°C, beginning with irradiation Cycle 152B on November 28, 2012 and ending with Cycle 155B on April 12, 2014, with a total received dose range of 0.9–3.7 dpa. Larger creep and control specimens located more centrally in the capsule received a dose of 1.0 – 3.7 dpa. AGC-3 was designed to provide irradiation conditions similar to AGC-1 and AGC-2 capsules (similar graphite grades tested, specimen dimensions, mechanical loading conditions) but at a different nominal irradiation temperature of 800°C. AGC-3 was irradiated for a short duration to provide material property values at lower dose levels. AGC-4 will have a longer duration and provide material property values at higher dose levels. After irradiation, material property and dimensional strain measurements were conducted on all AGC-3 specimens (from 11 nuclear graphite grades) using the same equipment and approved standards as were conducted before irradiation. The specimen loading configuration for all graphite grades within AGC-3 followed a similar pattern as earlier AGC capsules to provide easy future comparison of all irradiated material property data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Baseline Characterization Database Verification Report ? NBG-17 Billet V104

The purpose of this report is to present data collected in the Baseline Graphite Characterization Program, which is directly tasked with supporting the Idaho National Laboratory’s (INL’s) research and development efforts on the Advanced Reactor Technologies (ART) Program. This program populates a comprehensive database that reflects the baseline properties of nuclear-grade graphite regarding individual grade, billet, and position within individual billets. The physical- and mechanical-property information being collected will be transferred to the Nuclear Data Management and Analysis System (NDMAS), and that database will help populate the handbook of property data available to member nations of the Generation-IV International Forum. Transfer of these data from the applicable technical lead to the dissemination databases available to other end users requires a full review of the test procedures and data-collection efforts through an analysis of the multiple summary spreadsheets and values being collected. This report represents the analysis for NBG-17 Billet V104 and facilitates release of associated data to the NDMAS custodians. Millions of raw data points have been collected during testing and quantification analyses for these billets. The summary scalar property values and supplementary traceability data are collected into comprehensive spreadsheets. Data sets are composed of single billets of graphite for any given grade, organized by mechanical test-specimen type, and further subdivided into individual spreadsheet tabs according to the specific test or evaluation being performed. A direct analysis of properties was not conducted, and this report does not provide information on the validity or performance characteristics of the graphite itself. Rather, this report is intended as a verification of the completeness of actual data collected in accordance with PLN-3467, “Baseline Graphite Characterization Plan: Electromechanical Testing,” [1] and PLN-3348 “Graphite Mechanical Testing” [2] and their representation of the measurement and test results with sole regard to the graphite billets under evaluation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Comparison between the Strength Levels of Baseline Nuclear-Grade Graphite and Graphite Irradiated in AGC-2

This report details the initial comparison of mechanical strength properties between the cylindrical nuclear-grade graphite specimens irradiated in the second Advanced Graphite Creep (AGC-2) experiment with the established baseline, or unirradiated, mechanical properties compiled in the Baseline Graphite Characterization program. The overall comparative analysis will describe the development of an appropriate test protocol for irradiated specimens, the execution of the mechanical tests on the AGC-2 sample population, and will further discuss the data in terms of developing an accurate irradiated property distribution in the limited amount of irradiated data by leveraging the considerably larger property datasets being captured in the Baseline Graphite Characterization program. Integrating information on the inherent variability in nuclear-grade graphite with more complete datasets is one of the goals of the VHTR Graphite Materials program. Between “sister” specimens, or specimens with the same geometry machined from the same sub-block of graphite from which the irradiated AGC specimens were extracted, and the Baseline datasets, a comprehensive body of data will exist that can provide both a direct and indirect indication of the full irradiated property distributions that can be expected of irradiated nuclear-grade graphite while in service in a VHTR system. While the most critical data will remain the actual irradiated property measurements, expansion of this data into accurate distributions based on the inherent variability in graphite properties will be a crucial step in qualifying graphite for nuclear use as a structural material in a VHTR environment.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

Baseline Characterization Database Verification Report – NBG-18 Billet 635-4

This engineering calculations and analysis report is a validity evaluation of the physical and mechanical property databases collected on a billet of nuclear grade graphite (i.e., NBG-18 Billet 635-4) in support of the Advanced Reactor Technologies Baseline Graphite Characterization Program. Millions of raw data points that have been collected during testing and quantification analyses for these billets, the summary scalar property values and supplementary traceability data are collected into comprehensive spreadsheets. Data sets are comprised of single billets of graphite for any given grade, organized by mechanical test specimen type and further subdivided into individual spreadsheet tabs according to the specific test or evaluation being performed. This report is not a direct analysis of properties and will not provide information on the validity or performance characteristics of the graphite itself. Rather, it is intended as a verification of the completeness of actual data collected in accordance with PLN-3467, “Baseline Graphite Characterization Plan: Electromechanical Testing,” and its representation of the measurement and test results with sole regard to the graphite billets under evaluation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Investigation of nonlinear mechanical behavior of two superfine-grained graphites with DIC assisted disc splitting test

Using standardized uniaxial tensile test specimens is not practical due to the limited volumes in irradiation capsules, molten salt degradation facilities, or oxidation apparatus. The ASTM International Standard Test Method for Tensile Strength Estimate by Disc Compression of Manufactured Graphite (ASTM D8289) was developed to provide a convenient way for estimating tensile strength. Unlike the traditional uniaxial tensile test in ASTM C749 (International Standard Test Method for Tensile Stress–Strain of Carbon and Graphite), which uses dog-bone shaped specimens larger than 12.95 mm × 120.65 mm, the ASTM D8289 standard uses smaller discs with diameters of 6–12.7 mm. A digital image correlation (DIC) system, which uses a full-field noncontact surface displacement measurement technique, was applied along with the ASTM D8289 disc splitting test on IG-110 samples and compared with previous measurements from Mersen 2114 samples. Results confirmed that the DIC technique can measure the surface displacement/strain on these small (Ø6 mm × 3 mm) graphite specimens with good repeatability. However, Mersen 2114 and IG-110 samples exhibited strain discrepancies when DIC measurements were compared with analytical and finite element simulation values. The loading history and strain results also indicated different mechanical behaviors between Mersen 2114 and IG-110, particularly the nonlinear behavior of the IG-110 samples. Good agreement was observed by comparing the splitting tensile strengths of two superfine-grained grades with results from other work. The specimen size effect is discussed when comparing the splitting tensile strength with corresponding uniaxial tensile strength of these two graphite grades.

Lin, Lianshan [ORNL] (ORCID:0000000203399219)↗

A study of graphite-epoxy laminate failures due to high transverse shear strains using the multi-span-beam shear test procedure

The multi-span-beam shear test procedure is used to study failure mechanisms in graphite-epoxy laminates due to high transverse shear strains induced by severe local bending deformations in test specimens. Results of a series of tests on specimens with a variety of stacking sequences, including some with adhesive interleaving, are presented. These results indicate that laminates with stacking sequences with several + or - 45 and 90 deg plies next to each other are more susceptible to failures due to high transverse shear strains than laminates with + or - 45 and 0 deg plies next to each other or with + or - 45 deg plies next to layers of adhesive interleaving. Results of these tests are compared with analytical results based on finite elements.

Jegley, Dawn C.↗

Baseline Characterization Database Verification Report – 2114 Billet A20568

This ECAR provides the results of a validity evaluation of the physical and mechanical property data collected on a billet of nuclear-grade graphite (i.e., 2114 Billet A20568) in support of the ART Baseline Graphite Characterization Program.1,2 Millions of raw data points have been collected during testing and quantification analyses for these billets. The summary scalar property values and supplementary traceability data are collected into comprehensive spreadsheets. Data sets are composed of single billets of graphite for any given grade, organized by mechanical test-specimen type, and further subdivided into individual spreadsheet tabs according to the specific test or evaluation being performed. A direct analysis of properties was not conducted, and this report does not provide information on the validity or performance characteristics of the graphite itself. Rather, this report is intended as a verification of the completeness of actual data collected in accordance with PLN-3467, “Baseline Graphite Characterization Plan: Electromechanical Testing,”3 and their representation of the measurement and test results with sole regard to the graphite billets under evaluation.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NDMAS Portal Updates

Overview of current ART-GCR Data, including fuel fabrication, irradiation monitoring, fuel and graphite, post-irradiation examination, graphite characterization, high temperature metals mechanical tests, methods validation data (including: HTTR, NSTF, and HTTF), addition of AGR fuel data, other GCR and related data, updated high temperature metals, ongoing and upcoming work, users guide, and the link to those interested in access to NDMAS.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Baseline Graphite Characterization

Baseline Graphite Characterization: Purpose of Baseline, Mechanical Baseline Tests, Physical Properties Tests, Methodology, Baseline progress, Density, Ultimate Tensile Strength, PCEA Ultimate Tensile Strength, Split Disc Tests, Compression Tests, Flexural Tests, and Coefficient of Thermal Expansion.

22 - GENERAL STUDIES OF NUCLEAR REACTORS↗

Investigation of static and cyclic bearing failure mechanisms for GR/EP laminates

Static, cyclic load (fatigue), and residual strength testing of graphite-epoxy (GR/EP) and aluminum pin bearing joints was completed to study bearing failure mechanisms. Parameters investigated included static strength, failure mode, fatigue life, hole growth, joint stiffness, and residual strength. Comparative evaluation of these results show that the MIL-HDBK-5 convention for the definition of bearing strength can be used for GR/EP materials while maintaining the same, or improved, level of structural integrity shown for metal joints.

Walter, R. W.↗

Graphene oxide-silica nanohybrids as fillers for PA6 based nanocomposites

Graphene oxide (GO) was prepared by oxidation of graphite flakes by a mixture of H{sub 2}SO{sub 4}/H{sub 3}PO{sub 4} and KMnO{sub 4} based on Marcano's method. Two different masterbatches containing GO (33.3%) and polyamide-6 (PA6) (66.7%) were prepared both via solvent casting in formic acid and by melt mixing in a mini-extruder (Haake). The two masterbatches were then used to prepare PA6-based nanocomposites with a content of 2% in GO. For comparison, a nanocomposite by direct mixing of PA6 and GO (2%) and PA6/graphite nanocomposites were prepared, too. The oxidation of graphite into GO was assessed by X-ray diffraction (XRD), Micro-Raman spectroscopy, scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) analyses. All these techniques demonstrated the effectiveness of the graphite modification, since the results put into evidence that, after the acid treatment, interlayer distance, oxygen content and defects increased. SEM micrographs carried out on the nanocomposites, showed GO layers totally surrounded by polyamide-6, this feature is likely due to the strong interaction between the hydrophilic moieties located both on GO and on PA6. On the contrary, no interactions were observed when graphite was used as filler. Mechanical characterization, carried out by tensile and dynamic-mechanical tests, marked an improvement of the mechanical properties observed. Photoluminescence and EPR measurements were carried out onto nanoparticles and nanocomposites to study the nature of the interactions and to assess the possibility to use this class of materials as semiconductors or optical sensors.

77 NANOSCIENCE AND NANOTECHNOLOGY↗

Flammabilities Of Graphite-Reinforced Composites

Report describes tests and comparisons of flammabilities, thermal properties, and selected mechanical properties of composite materials made of epoxy and other matrices reinforced by graphite fibers. Composites also compared with baseline epoxy/fiberglass composite. Considers such properties as limiting oxygen index, smoke evolution, products of thermal degradation, total heat release, heat-release rate, loss of mass, spread of flames, resistance to ignition, and thermal stability.

Kourtides, Demetrius A.↗