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HDG-1 Experiment Irradiation Monitoring Data Qualification Final Report

SUMMARY The U.S. Department of Energy (DOE) Advanced Reactor Technologies (ART) Graphite Research and Development (GRD) Program is conducting a series of six experiments to quantify the effects of irradiation on nuclear-grade graphite. This report documents the qualification of irradiation monitoring data for the fifth experiment, High Dose Graphite-1 (HDG-1). Qualified monitoring data are required by the ART program to support the design and licensing of the first high-temperature reactor (HTR) nuclear plant. Data are classified as Qualified if they meet the usage requirements described in the experiment planning and quality assurance (QA) documents, Failed if they do not meet those requirements and provide no usable information, or Trend if they do not fully meet all requirements but still provide useful information subject to an assessment of how any deficiencies may affect a particular use of the data. HDG-1 irradiation began with Advanced Test Reactor (ATR) Cycle 168B on August 24, 2020, and concluded after Cycle 173C on January 27, 2025. The HDG-1 capsule was removed from the reactor core twice—during core internal change (CIC) Cycle 170A and powered axial locator mechanism (PALM) Cycle 172A—to prevent overheating of the graphite specimens during high-power PALM cycles. The capsule was therefore irradiated during a total of seven normal ATR cycles: 168B, 169A, 171A, 171B, 173A, 173B, and 173C. Irradiation monitoring data evaluated in this report include thermocouple (TC) temperature, gas flow rate, gas moisture, gas pressure, specimen load, and graphite stack displacement. Temperature. A total of 14,508,065 TC temperature records were captured. Of these, 13,901,785 (95.8%) are Qualified and 606,280 (4.2%) are Failed. The principal source of failed temperature data was the instrument failure of TC-9 (Zone 2) on June 24, 2024, and TC-10 (Zone 1) on July 5, 2024, near the end of Cycle 173A, which resulted in 595,554 Failed readings. An additional 379 missing values and 10,347 slightly negative values from TC-13 during ATR outages are also Failed. Neither TC-9 nor TC-10 was used as a temperature-control TC, and their failures did not compromise capsule condition monitoring. Correlation analysis of all 13 TCs found no evidence of virtual junction formation. Control chart analysis revealed clear downward drift of approximately 80°C for TC-6 (Zone 3) relative to other stable TCs, and possible downward drift of approximately 60°C for TC-13 relative to the Zone 5 control TC (TC-1), though TC-13 remained consistent with the Zone 2 control TC (TC-12). Gas flow. A total of 20,088,090 gas flow rate records were captured. Of these, 19,941,463 (99.3%) are Qualified and 146,627 (0.7%) are Failed due to missing values. All argon, helium, and total gas flow data were within expected ranges throughout the irradiation. Gas moisture. A total of 1,116,005 outlet gas moisture values were captured. Of these, 1,101,421 (98.7%) are Qualified and 14,584 (1.3%) are Failed, comprising 14,556 out-of-range values and 28 missing values. The out-of-range moisture values exceeded 22,000 ppmv for approximately 1 week at the beginning of Cycle 173A, when accumulated moisture evaporated after the capsule was retrieved from water storage during PALM Cycle 172A and reinserted into the east flux trap. Moisture levels returned to below 25 ppmv for the remaining three cycles, and the transient high-moisture event did not affect the integrity of specimen irradiation. Gas pressure. A total of 7,812,035 gas pressure values were captured. Of these, 6,642,048 (85.0%) are Qualified and 1,169,987 (15.0%) outlet pressure values are Failed, comprising 718,537 zero outlet pressure values due to sensor failure from Cycle 168B through Cycle 171B, 54,550 missing values, and 396,900 too-low outlet pressure values, ranging from 1.1 to 1.6 psia after sensor replacement during Cycle 173A. Load. A total of 6,696,030 load values were captured. Of these, 6,694,580 (99.98%) are Qualified and 1,450 (0.02%) are Failed due to missing values. Applied loads to the six specimen stacks were stable throughout the irradiation. Stack displacement. A total of 6,696,030 displacement values were captured. Of these, 5,713,297 (85.32%) are Qualified and 3,781 (0.06%) are Failed due to missing values. Stack displacement increased consistently throughout the irradiation, reaching approximately 3.08 in. for Channels 5 and 6 by the end of irradiation. 978,952 (14.62%) substantially elevated displacements observed for Channel 6 beginning in Cycle 171A and for Channel 5 beginning in Cycle 173A are assigned Trend status. Raising pressure. A total of 1,115,999 raising pressure values were captured. Of these, 1,115,430 (99.95%) are Qualified and 569 (0.05%) are Failed due to missing values. Ram pressure. A total of 6,696,030 ram pressure values were captured. Of these, 6,692,249 (99.95%) are Qualified and 3,484 (0.05%) are Failed due to missing values. Stack raising was perf

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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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HDG-1 Fiber Bragg grating data analysis

The main goal of the High dose graphite 1 Advanced test reactor experiment was to study nuclear grade graphite at high fluences. Additional supplementary optical fiber instrumentation was added to this long duration experiment for instrumentation development purposes. The supplementary instrumentation consisted of two pure silica core, fluorine doped cladding optical fibers each etched with 9 fiber Bragg gratings, one fiber being heat treated for 9 hours at 750 C and 16 hours at 750 C, the other being heat treated for 24 hours at 550 C and 48 hours at 650 C. Fiber Bragg gratings are known to have issues of measurement drift when in high temperature and high radiation environments like what is encountered in the Advanced test reactor. At the culmination of this experiment, the optical fibers saw ~1.3E21 n/cm2 total fluence, which is at the highest fluences that fiber Bragg gratings have been studied to date. Reported here is the analysis of this data including radiation induced shift and changes in sensitivity.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN

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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Radiation damage study of POCO ZXF-5Q graphite for neutrino production targets using 4.5 MeV helium ions

To address the challenges of increased beam power and target survivability associated with next-generation particle production beam lines, high dose, high-energy proton beam conditions are simulated using irradiation from low-energy ion beams. A low-energy ion irradiation study of POCO ZXF-5Q graphite under conditions similar to those of the NuMI NT-02 neutrino production target at the Fermi National Accelerator Laboratory is reported. Helium ion irradiation was performed at 100 ∘ C to a maximum damage level of 0.9 displacements per atom (DPA). Irradiation induced hardening, swelling of the irradiated region, inter-plane lattice expansion, and intraplane lattice contraction with increasing ion fluence was observed using micromechanical (nanoindentation, atomic force microscopy) and electron microscopy (high-resolution imaging, selected area diffraction) characterization. Similar changes were also observed in post irradiation examination of the NT-02 target indicating that ion irradiation can be a valuable tool for estimating radiation damage in proton beam targets. Caution must be exercised though, because the hardening, lattice alteration, and swelling occur to different magnitudes for a given damage level. The observed hardening and embrittlement were greater for ion irradiated graphite. For He ion irradiated samples the lattice spacing changes were smaller at low damage levels (78% less expansion and 71% less contraction at 0.1 DPA) and larger at high damage levels (38% more expansion and 5% more contraction at 0.9 DPA) relative to that observed in the NT-02 target. The magnitude of swelling was 8.5× greater under ion irradiation which is influenced by the differing damage gradients and inclusion of implanted He ions in the region of interest.

43 PARTICLE ACCELERATORS

Development of mesopores in superfine grain graphite neutron-irradiated at high fluence

Microstructural changes induced by neutron irradiation of superfine grain graphite G347A (Tokai Carbon, Japan) were examined by nitrogen adsorption at 77K and by three microscopy techniques (SEM, TEM and FIB-SEM tomography). The specimens were irradiated at doses of up to 30 dpa, covering stages before and after the turnaround fluence at three temperatures (300, 450, 750 °C) of their irradiation envelope. The initial graphite densification at low fluences did not produce any detectable effect in the pore size range (<350 nm) measured by gas adsorption. However, graphite irradiated at high fluences, after turnaround, showed severe structural changes. At all three temperatures and high irradiation fluences, gas adsorption revealed significant increase of the volume of narrow mesopores (<5–20nm) and up to five times increase of BET surface area, both in linear relationship with the relative volume expansion. Analysis of microscopy images showed multiplication of fine macropores (>50 nm) at high irradiation fluences and more structural changes on multiple scales, from nanometers to microns. This work demonstrates the unique ability of gas adsorption techniques to analyze open pores with sizes between sub-nanometer and sub-micron in bulk nuclear graphite, with supporting microscopy results.

I. Contescu, Cristian

AGC-2 Graphite Preirradiation Data Analysis Report

This report describes the specimen loading order and documents all preirradiation examination material property measurement data for graphite specimens contained within the Second Advanced Graphite Capsule (AGC 2) irradiation capsule. The AGC 2 capsule is the second in six planned irradiation capsules comprising the Advanced Graphite Creep (AGC) test series. The AGC test series is used to irradiate graphite specimens in order to garner quantitative data necessary for predicting the irradiation behavior and operating performance of new nuclear grade graphites. This testing will ascertain the in service behavior of the graphite for pebble bed and prismatic very high temperature reactor designs. Similar to the First Advanced Graphite Capsule (AGC 1) preirradiation examination report, material property tests were conducted on specimens from 18 nuclear grade graphite types. However, AGC 2 tested an increased number of specimens (i.e., 512) prior to loading them into the AGC 2 irradiation assembly. All AGC 2 specimen testing was conducted at Idaho National Laboratory from July 2009 to August 2010. This report also details the specimen loading methodology for graphite specimens inside the AGC 2 irradiation capsule. The AGC 2 capsule design requires “matched pair” creep specimens that have similar dose levels above and below the neutron flux profile mid plane. This provides similar specimens with and without an applied load. Analysis in this document utilizes the neutron flux profile calculated for the AGC 2 capsule design, the capsule dimensions, and the size (i.e., length) of the selected graphite specimens to create a stacking order that produces “matched pairs” of graphite specimens above and below the AGC 2 capsule elevation mid point, thus providing specimens with similar neutron dose levels.

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Nuclear Safety [Vol. 29, No. 1, January-March 1988]

Nuclear Safety is a review journal that covers significant developments in the field of nuclear safety. Its scope includes the analysis and control of hazards associated with nuclear energy, operations involving fissionable materials, and the products of nuclear fission and their effects on the environment. Primary emphasis is on safety in reactor design, construction, and operation; however, the safety aspects of the entire fuel cycle, including fuel fabrication, spent-fuel processing, nuclear waste disposal, handling of radioisotopes, and environmental effects of these operations, are also treated. Table of Contents for this issue follows. THE CHERNOBYL ACCIDENT: 1 Core History and Nuclide Inventory of the Chernobyl Core at the Time of Accident by Gerald Kirchner and Cornelius C. Noack; GENERAL SAFETY CONSIDERATIONS: 6 Nonprescriptive Nuclear Safety Regulation: The Example of Loss of Offsite Power by M. W. Golay, V. P. Manno, and C. Vlahoplus, Jr., 20 Nuclear Power Safety Goals in Light of the Chernobyl Accident by C. Whipple and C. Starr; ACCIDENT ANALYSIS: 29 Containment Loads from Severe Accidents—U.S. Program by W. Kerr and M. K. Dey; PLANT SAFETY FEATURES: 36 Safety Characteristics of Modern High-Temperature Reactors: Focus on German Designs by W. Kröger, H. Nickel, and R. Schulten; ENVIRONMENTAL EFFECTS: 49 Radiation Hormesis and Nuclear Safety by C. C. Congdon; OPERATING EXPERIENCES: 58 Evaluation of Nonradiological Water Chemistry at Power Reactors by Harvey Zibulsky, James J. Kottan, Walter J. Pasciak, Mary Ann Castrogivanni, and Sujit Banerjee, 64 Reactor Shutdown Experience Compiled by J. W. Cletcher, 67 Operating U.S. Power Reactors Compiled by E. G. Silver; RECENT DEVELOPMENTS: 85 General Administrative Activities Compiled by E. G. Silver, 94 Reports, Standards, and Safety Guides by D. S. Queener, 100 Status of Power-Reactor Projects Undergoing Licensing Review Compiled by E. G. Silver, 103 Proposed Rule Changes as of Sept. 30, 1987; ANNOUNCEMENTS: 5 Northwestern University Short Course on Radiation Safety, 28 International Approach to Nuclear Safety (After Three-Mile Island and Chernobyl), 57 RPI Short Course on Modern Developments in Boiling Heat Transfer and Two-Phase Flow, 107 20th DOE/NRC Nuclear Air Cleaning Conference, 110 Third International Topical Meeting on Nuclear Power Plant Thermal Hydraulics and Operations, 108 The Authors, 111 Indexes to Nuclear Safety, Volume 28.

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