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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

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As-Run Physics Analysis for the AGC-4 Experiment Irradiated in the ATR

This Engineering Calculations Analysis Report (ECAR) documents the results of the Advanced Test Reactor (ATR) detailed physics analyses performed to calculate the displacements per atom (DPA) and the fast neutron fluence (E > 0.1 MeV) of the Advanced Graphite Creep (AGC) experiment, AGC-4, irradiated in the ATR East Flux Trap (EFT) (see Figure 1) during ATR Cycle 157D, 158A, 162A, 162B, 164A, 164B, 166A, and Cycle 166B. This ECAR also reports the neutron and photon heat rates for the materials of the AGC-4 experiment for ATR Cycle 158A (timestep 19), which provides to the maximum heating. The results for these evaluations and analysis are reported herein. The AGC-4 as-run specimen neutron fast fluence (E > 0.1 MeV), DPA, and material heat rate calculations were performed using a general-purpose Monte Carlo N-Particle (MCNP) code. All calculated results are tabulated herein.

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AGC-4 As-Run Uncertainty Analysis

The concept of measuring neutron flux (or fluence rate) with activation foils has existed since the late 1940s and is a well-used methodology. Activation foils are selected for their unique isotopic cross sections that create reaction products with desirable properties: relatively simple radioactive decay scheme, measurable quantities of gamma-rays or betas, and half-lives appropriate for the irradiation and decay durations of the experiment. The activation materials, deemed flux wires, fluence wires, dosimeters, or flux foils, are fabricated to have a mass appropriate for the irradiation as well so the measurement using a radiation detector following the irradiation is sufficient but not overwhelming in terms of total activity. Activation measurement results are expressed in terms of reaction rate, which can then be used to “adjust” the neutron spectrum. The Advanced Graphite Creep (AGC)-4 experiment contained 26 flux wire packages, each containing an iron and a niobium wire inside a vanadium capsule. For all stackup positions, the value of fast to thermal neutrons is higher than expected, but the total neutron fluence is near the predicted value of ~2 x 1022 n/cm2. As compared to the predicted neutron spectrum, there are four takeaways in the results as compared to the predicted ATR irradiation: 1) Additional fast (fission) neutrons present, 2) Spectrum hardening due to temperature, 3) Spectrum hardening due to container attenuation, 4) Total neutron fluence is close to predicted values. Since the neutron energy spectrum is a key parameter when attributing neutron damage in materials, the adjusted energy-dependent spectrum and the total neutron fluence results from the dosimeters can be incorporated for future calculations.

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As-Run Thermal Analysis for the AGC-4 Experiment Irradiated in the ATR

The Advanced Graphite Capsule (AGC) irradiation experiment will provide irradiation creep rate data for the new graphite proposed for the Next Generation Nuclear Plant (NGNP) program. The fourth experiment in the series (AGC-4) was designed to irradiate various types of graphite specimens at a temperature of 900 ºC and targeted displacements per atom (DPA) of 6. This experiment has been irradiated in the east flux trap of the Advanced Test Reactor (ATR) during the cycles of 157D, 158A, 162A, 162B, 164A, 164B, 166A, and 166B. Temperatures were monitored using twelve thermocouples (TC) located at various elevations in the reactor core, and variable helium-argon gas mixtures were used for gas gap temperature control of the specimens. The purpose of this Engineering Calculation and Analysis Report (ECAR) is to calculate the specimen temperature after the model is calibrated by the measured TC data with the as-run heating rates of the components, DPA of the graphite, and the gas mixture compositions during the experiment. As-run specimen mean temperature and the tolerance will be obtained.

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AGC-4 Specimen Post-Irradiation Examination Data Interim Report

This interim report documents preliminary results of the post-irradiation examination material property testing from the fourth advanced graphite creep (AGC), AGC 4, capsule specimens. This is the fourth of 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 to moderate dose levels (=7 dpa). The AGC 4 capsule was irradiated in the Idaho National Laboratory Advanced Test Reactor at a nominal temperature of 800°C and to a peak dose of 8 dpa. Half of the AGC-4 specimens were subjected to compressive stresses to induce irradiation creep. Post-irradiation testing and measurement results are reported with the exception of thermal testing, which is still in progress, and irradiation mechanical strength testing. Additionally, some specimens initially deemed too hot to be examined in the ART Graphite laboratory may still be measured. The data reported includes specimen dimensions for both stressed and unstressed specimens to establish the irradiation creep rates, mass and dimensional data necessary to derive density, elastic constants (Young?s modulus, shear modulus, and Poisson?s ratio) from ultrasonic time of flight velocity measurements, Young?s modulus from the fundamental frequency of vibration, and electrical resistivity. A more complete evaluation of trends in the material property changes, as well as irradiation-induced creep due to the irradiation environment and applied load on the specimens, will be discussed later in AGC 4 post-irradiation examination analysis reports.

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AGC-4 Specimen Post-Irradiation Examination Data Interim Report

This interim report documents preliminary results of the post-irradiation examination material property testing from the fourth advanced graphite creep (AGC), AGC 4, capsule specimens. This is the fourth of 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 to moderate dose levels (=7 dpa). The AGC 4 capsule was irradiated in the Idaho National Laboratory Advanced Test Reactor at a nominal temperature of 800°C and to a peak dose of 8 dpa. Half of the AGC-4 specimens were subjected to compressive stresses to induce irradiation creep. Post-irradiation testing and measurement results are reported with the exception of thermal testing, which is still in progress, and irradiation mechanical strength testing. Additionally, some specimens initially deemed too hot to be examined in the ART Graphite laboratory may still be measured. The data reported includes specimen dimensions for both stressed and unstressed specimens to establish the irradiation creep rates, mass and dimensional data necessary to derive density, elastic constants (Young?s modulus, shear modulus, and Poisson?s ratio) from ultrasonic time of flight velocity measurements, Young?s modulus from the fundamental frequency of vibration, and electrical resistivity. A more complete evaluation of trends in the material property changes, as well as irradiation-induced creep due to the irradiation environment and applied load on the specimens, will be discussed later in AGC 4 post-irradiation examination analysis reports.

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AGC-4 Disassembly Report

The Advanced Reactor Terminology Graphite Research and Development program is currently measuring irradiated material property changes in several grades of nuclear graphite to predict behavior and operating performance within the core of these new high temperature reactor designs. The Advanced Graphite Creep (AGC) experiment, consisting of six irradiation capsules, will generate the irradiated graphite performance data for the Very High Temperature Reactor operating conditions. All six capsules in the experiment conducted at Idaho National Laboratory will be irradiated in the Advanced Test Reactor, disassembled in the Hot Fuel Examination Facility, and examined at the Idaho National Laboratory Research Center. This is the disassembly report describing the disassembly, shipment, post irradiation inspection, and storage of the graphite specimens contained within the AGC 4 irradiation test series capsule (the fourth irradiation capsule of the series). AGC 4 was irradiated in the Advanced Test Reactor (ATR) East Flux Trap (EFT) during ATR Cycle 157D, 158A, 162A, 162B, 164A, 164B, 166A, and Cycle 166B. Approximately 3.6 dpa was achieved. Desired experiment temperatures were exceeded by at least 100C during the second Cycle of irradiation due to the insertion of the KJRR experiment. The capsule was removed from the ATR and transferred to the Hot Fuel Examination Facility on May 15, 2020 and eventually unloaded into the Hot Fuel Examination Facility (HFEF) Decon Cell through Penetration 2D on February 26, 2021. It was moved to the HFEF Main Cell Window 3M for disassembly on March 15, 2021. Disassembly and specimen extraction began March 18, 2021, and packaging of the graphite specimens was completed on April 16, 2021. Several anomalies were noted, specifically that the radiological dose rates were nominally an order of magnitude higher than that of the previous AGC experiments. This report summarizes the disassembly of the AGC 4 experiment.

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AGC-4 Disassembly Report

The Advanced Reactor Terminology Graphite Research and Development program is currently measuring irradiated material property changes in several grades of nuclear graphite to predict behavior and operating performance within the core of these new high temperature reactor designs. The Advanced Graphite Creep (AGC) experiment, consisting of six irradiation capsules, will generate the irradiated graphite performance data for the Very High Temperature Reactor operating conditions. All six capsules in the experiment conducted at Idaho National Laboratory will be irradiated in the Advanced Test Reactor, disassembled in the Hot Fuel Examination Facility, and examined at the Idaho National Laboratory Research Center. This is the disassembly report describing the disassembly, shipment, post irradiation inspection, and storage of the graphite specimens contained within the AGC 4 irradiation test series capsule (the fourth irradiation capsule of the series). AGC 4 was irradiated in the Advanced Test Reactor (ATR) East Flux Trap (EFT) during ATR Cycle 157D, 158A, 162A, 162B, 164A, 164B, 166A, and Cycle 166B. Approximately 3.6 dpa was achieved. Desired experiment temperatures were exceeded by at least 100C during the second Cycle of irradiation due to the insertion of the KJRR experiment. The capsule was removed from the ATR and transferred to the Hot Fuel Examination Facility on May 15, 2020 and eventually unloaded into the Hot Fuel Examination Facility (HFEF) Decon Cell through Penetration 2D on February 26, 2021. It was moved to the HFEF Main Cell Window 3M for disassembly on March 15, 2021. Disassembly and specimen extraction began March 18, 2021, and packaging of the graphite specimens was completed on April 16, 2021. Several anomalies were noted, specifically that the radiological dose rates were nominally an order of magnitude higher than that of the previous AGC experiments. This report summarizes the disassembly of the AGC 4 experiment.

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Summary of Graphite Data Stored within NDMAS

The Graphite Technology Development Project provides data to support the design of graphite core components within specific reactor service conditions of the next generation of high-temperature, gas-cooled nuclear reactors. Physical, mechanical, and thermal properties of nuclear grade graphite were characterized for specimens that were unirradiated, irradiated, and irradiated under various stress conditions. The material properties include diameter, length, mass, density, compressive strength, tensile strength, flexural strength, modulus, resistivity, thermal diffusivity, and thermal expansion coefficient. Baseline graphite specimens are unirradiated from different grades (2114, IG-110, NBG-17, NBG-18, and PCEA) and different types used in different characterization tests (compressive, flexural, tensile, one-inch cylinder, and quarter-inch cylinder). The Advanced Graphite Creep (AGC) irradiation specimens are from a much larger number of grades and cylinder types (creep, piggyback, and pencil). For baseline graphite, characterization data for 7,756 specimens extracted from thirteen graphite billets were captured to the NDMAS database. For AGC experiments, four irradiation campaigns have been completed: AGC-1, AGC-2, AGC-3, and AGC-4. The ongoing HDG-1 (High-Dose Graphite) experiment, which began irradiation with Cycle 168B on August 26, 2020, includes specimens previously irradiated in AGC-2 in addition to the specimens originally destined for AGC-5.. Besides the characterization data, the AGC data includes irradiation monitoring and physics data representing the irradiation conditions of AGC specimens. Currently, all data for AGC-1, AGC-2, and AGC-3 have been captured to the NDMAS database. Only AGC-4 pre-irradiation and irradiation monitoring data have been captured, and HDG-1 pre-irradiation data are in process of being captured for unirradiated specimens. To date, a total of 38,149 material property records have been captured into NDMAS database for baseline and AGC specimens. All characterization data are qualified for use according to their perspective data verification reports. For the AGC irradiation campaigns, a total of 41,502 qualified physics calculation records were added for AGC-1, AGC-2, and AGC-3. Finally, a total of 173,698,505 AGC irradiation monitoring data records (thermocouple temperature, gas flow rate, gas pressure, gas moisture, applied load, and specimen displacement) have been captured to NDMAS; the majority of those records (~94%) are qualified data records.

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AGC Experiment Status

AGC Experiment Status to include: History and status of the AGC-4, Review of the AGC experiment, AGC graphite grades and samples, The AGC-4 capsule and specimens, and HDG-1 and HDG-2. Description of the Experiment, AGC graphite grades and samples, AGC-1 Test Train, AGC-1 Test Train Design Features, New AGC Irradiation Schedule (2018) and update in schedule, Irradiation and disassembly history, present and future status, and shipment and initial PIE. Initial PIE strategy, recovered specimens, PIE results, and status of experiments.

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ART Graphite R&D Program Status - 2020

Structure of the program Graphite material issues of interest How do things fit together Status of the program Baseline AGC Experiment Update AGC-4 and HDG-1 Irradiation Oxidation Modeling ASME Code development Discussion of how the data can be used Modeling behavior of core components Licensing/code development Interaction with vendors Collaborations (domestic and international)

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HDG-1 Graphite Preirradiation Data Package Report

This report documents all pre-irradiation examination material-property measurement data for graphite specimens that are going to be used within the first high dose graphite (HDG) -1 irradiation capsule. The two new HDG capsules signify a major change to the AGC Experiment. HDG-1 and HDG-2 will replace the last two Advanced Graphite Creep (AGC) capsules (AGC-5 and AGC-6) which were designed to irradiate graphite at the extreme upper operational temperatures for a very-high-temperature reactor (VHTR) design, 1100°C. These very high temperature AGC-5 and AGC-6 capsules have been repurposed to re-irradiated specimens (from AGC-2, AGC-3, and AGC-4) at the lower temperatures of 600°C and 800°C. HDG-1 will be irradiated at 600°C and HDG-2 will be irradiated at 800°C. By re-irradiating the previous AGC specimens a total maximum neutron dose of around 15 dpa (displacements per atom) can be achieved for all major graphite grades at irradiation temperatures of 600°C and 800°C. Specimens in the HDG-1 capsule are made up of previously irradiated specimens from the AGC-2 capsule and unirradiated specimens prepared for the now discontinued AGC-5 capsule. Utilizing the irradiated specimens, a maximum neutron dose of around 15 dpa is anticipated. These new maximum dose levels will provide irradiated material property data over a total neutron dose range of 1-15 dpa at a temperature of 600°C when combined with the previous AGC-1 and AGC-2 irradiation data. This will provide quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades for use within high temperature reactor designs. Similar to previous AGC test trains, HDG-1 includes the major graphite grades (IG-110, NBG-17, NBG-18, PCEA, and 2114) as well as adding the very fine-grain grade IG-430 which is of interest to the Molten Salt Reactor (MSR) designs. Also new to the HDG-1 capsule are 90 smaller geometry specimens designated as pencil specimens. These specimens take up only one third the space of a standard creep size specimen. This increased number of specimens will enhance property measurement statistics because they will provide 3 times the control specimen data at a position that would otherwise only have a single measurement.

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AGC 4 Graphite Specimen Postirradiation Characterization Plan

This characterization plan describes the thermal, physical, and mechanical measurement techniques that will be used to characterize graphite samples being tested in the fourth Advanced Graphite Creep experiment (AGC-4). Instruments, fixtures, and methods are currently in place for both pre and postirradiation material property measurements of bulk density, thermal diffusivity, coefficient of thermal expansion, elastic modulus, and electrical resistivity. Postirradiation testing procedures used to characterize the samples are described and discussed in the plan. Where they exist, American Society for Testing and Materials (ASTM) International testing standards will apply to the tests. Any departure from ASTM International testing standards or the approved laboratory procedures are documented within this characterization plan. Deviations that occur during testing will be documented in data reports.

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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.

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ART Advance Graphite Creep (AGC) Irradiation Experiment

ART Advance Graphite Creep (AGC) Irradiation Experiment topics of discussion include: Schedule, AGC Experiment Update, AGC-4 Status, Anticipated areas data will be used, and Vendor specific irradiation capsule. This includes NRC/Licensing questions on irradiation behavior, behavior model development, and other collaborations.

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HDG-1 Graphite Preirradiation Data Package Report

This report documents all pre-irradiation examination material-property measurement data for graphite specimens that are going to be used within the first high dose graphite (HDG) -1 irradiation capsule. The two new HDG capsules signify a major change to the AGC Experiment. HDG-1 and HDG-2 will replace the last two Advanced Graphite Creep (AGC) capsules (AGC-5 and AGC-6) which were designed to irradiate graphite at the extreme upper operational temperatures for a very-high-temperature reactor (VHTR) design, 1100°C. These very high temperature AGC-5 and AGC-6 capsules have been repurposed to re-irradiated specimens (from AGC-2, AGC-3, and AGC-4) at the lower temperatures of 600°C and 800°C. HDG-1 will be irradiated at 600°C and HDG-2 will be irradiated at 800°C. By re-irradiating the previous AGC specimens a total maximum neutron dose of around 15 dpa (displacements per atom) can be achieved for all major graphite grades at irradiation temperatures of 600°C and 800°C. Specimens in the HDG-1 capsule are made up of previously irradiated specimens from the AGC-2 capsule and unirradiated specimens prepared for the now discontinued AGC-5 capsule. Utilizing the irradiated specimens, a maximum neutron dose of around 15 dpa is anticipated. These new maximum dose levels will provide irradiated material property data over a total neutron dose range of 1-15 dpa at a temperature of 600°C when combined with the previous AGC-1 and AGC-2 irradiation data. This will provide quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear graphite grades for use within high temperature reactor designs. Similar to previous AGC test trains, HDG-1 includes the major graphite grades (IG-110, NBG-17, NBG-18, PCEA, and 2114) as well as adding the very fine-grain grade IG-430 which is of interest to the Molten Salt Reactor (MSR) designs. Also new to the HDG-1 capsule are 90 smaller geometry specimens designated as pencil specimens. These specimens take up only one third the space of a standard creep size specimen. This increased number of specimens will enhance property measurement statistics because they will provide 3 times the control specimen data at a position that would otherwise only have a single measurement.

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DOE ART Graphite R&D Program

Graphite overview: Material science, supply chain facts, nuclear material science, licensing thoughts

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