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DOE OSTI2023

Nuclear Testing and the Joint Task Force System

During the 1940s, 50s, and early 60s, the United States conducted eight nuclear test operations in the far reaches of the Pacific Ocean. These operations were possible only because of a military command and control organization, the joint task force. Commanded by the Army Navy, and Air Force on a rotating basis, each of the seven JTFs provided the means by which the thousands of ships, planes, material, and personnel were moved over thousands of miles of ocean. The first task force, JTF-1, was created to test the destructive effects of the Fat Man bomb on Naval vessels at Bikini Atoll in the summer of 1946. Commanded by Vice Admiral William “Spike” Blandy, JTF-1 was a purely military operation supported by the MED. Never meant to be a permanent organization, JTF-1 was dissolved soon after completing its mission.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2024

Robustness and printed sensor qualification

A limiting factor of additive manufactured (AM) sensors for in-pile applications is the development of appropriate interconnection and packaging strategies that can maintain reliable performance in extreme environments. Failure mechanisms in these harsh conditions could include, but not limited to, materials interaction (i.e., intermetallic formation) and coefficient of thermal expansion (CTE) mismatch between the individual components of the sensors. To mitigate premature failure and enable the successful sustained operation of AM sensors, non-destructive qualification tests are used as an intermediate process control step used for verifying robustness and reliability of the sensor before they are deployed. A materials system of interest is the use of barium strontium titanium oxide (BST) films on stainless steel 316L (SS316L) substrate. Due to BST’s high dielectric constant and tunable dielectric properties, there is an interest for its application as an insulation/encapsulation layer for capacitive strain gauges when printed on structural materials. Previous work on the BST/SS316L material system, however, showed that the BST cracks when exposed to temperatures up to 600 °C due to CTE mismatch between the printed BST film and the metallic substrate. When comparing different fabrication techniques, less surface cracking was observed in the samples that deposited thinner (i.e., 2-20 μm) than samples that were thicker (i.e., 135 µm – 300 µm). The objective of this report is to establish a qualification process that will determine and address any challenges (i.e., mechanical failure of thick prints) of the AM sensor prior to its application in experimental tests. To demonstrate the qualification process in this report, laser spallation and uniaxial tensile tests using dynamic and quasi-static loading, respectively, will be discussed.

36 - MATERIALS SCIENCE↗

DOE OSTI2022

Development of a Laser Ultrasonics-based Approach for Rapid Screening of High Entropy Alloys

This project utilized a laser ultrasonic technique to systematically study temperature-induced evolution of material properties in a set of interrelated binary alloys and a high entropy alloy (HEA) fabricated using arc-melting and spark plasma sintering processes. This technique involved the use of a nanosecond duration, high-intensity pulsed laser to thermo-elastically generate ultrasonic waves that propagate in the bulk of the metal alloy. Sub-nanometer-scale displacements associated with the propagating bulk ultrasonic waves were detected along the epicenter on the opposite surface of the sample using a 1 GHz bandwidth photorefractive interferometer. Phase transformations and microstructural changes were inferred from the temperature-dependent trends in the bulk acoustic velocities and features in the ultrasonic epicentral waveforms measured in the binary alloys. These inferences were then correlated with electron/optical microscopy observations and predictions using calculations of phase diagrams (CALPHAD). The results showed that the laser-generated ultrasonic pulses were strongly influenced by changes in material microstructure and could accurately track thermally driven phase transformations and detect the presence of microscale heterogeneities (grain boundaries, dendritic structures, etc.) in the set of binary alloy samples. The measurement approach was then applied to a quinary HEA sample for estimating phase transition temperature and determining microstructural heterogeneity. The rapid, non-contact and non-destructive ultrasonic testing approach demonstrated here is amenable to high throughput combinatorial investigations that can be applied to graded composition HEAs produced using advanced manufacturing methods. When paired with atomistic simulations and CALPHAD modeling, this approach can overcome the bottlenecks faced by current material characterization methods in efficiently screening the vast discovery space of HEAs that spans over a hundred million unique quinary alloy compositions.

36 MATERIALS SCIENCE↗

DOE OSTI2022

A laser ultrasonics-based approach for rapid screening of high entropy alloys

This project demonstrates a laser ultrasonics-based characterization methodology for rapid metallic materials design and discovery via in situ determination of phases, microstructures and elastic properties with respect to temperature. Ultrasonic waves are strongly affected by material microstructure, and therefore serve as a facile means to probe elastic properties, phase content and their size distributions and volume fractions. In this study, a laser ultrasonic technique is used to systematically study the evolution of properties in a set of interrelated simple binary alloys and high entropy alloys (HEA). Phase transformations and microstructural changes inferred from the ultrasonic signals will be correlated with electron microscopy data and predictions using calculations of phase diagrams (CALPHAD). The non-contact and non-destructive ultrasonic testing approach developed in this study could overcome several limitations associated with current material characterization methods for materials discovery. It is expected that laser ultrasonics-based methodology developed in this work will be utilized to evaluate novel graded composition HEAs currently being developed at the Idaho National Laboratory (INL) using advanced manufacturing methods based on direct energy deposition and spark plasma sintering processes, and contribute to accelerate the discovery of HEAs.

36 MATERIALS SCIENCE↗

DOE OSTI2022

A laser ultrasonics-based approach for rapid screening of high entropy alloys

The primary objective of this seed project is to develop a laser ultrasonics-based characterization methodology for rapid metallic materials design and discovery via in situ determination of phases, microstructures and elastic properties with respect to temperature. Ultrasonic waves are strongly affected by material microstructure, and therefore, serve as a facile means to probe elastic properties, phase content and their size distributions and volume fractions. In this study, a laser ultrasonic technique will be used to systematically study the evolution of properties in a set of interrelated simple binary alloys and high entropy alloys (HEA). Phase transformations and microstructural changes inferred from the ultrasonic signals will be correlated with electron microscopy data and predictions using calculations of phase diagrams (CALPHAD). The non-contact and non-destructive ultrasonic testing approach developed in this study could overcome several limitations associated with current material characterization methods for materials discovery. It is expected that the products of the proposed work will be utilized to evaluate novel graded composition HEAs currently being developed at the Idaho National Laboratory (INL) using advanced manufacturing methods based on direct energy deposition and spark plasma sintering processes, and contribute to accelerate the discovery of HEAs.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Sister Rod Destructive Examinations (FY2021) Appendix E Mechanical Testing

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Sister Rod Destructive Examinations (FY22) Appendix E: Mechanical Testing

As a part of the DOE NE High Burnup Spent Fuel Data Project, Oak Ridge National Laboratory (ORNL) is performing destructive examinations (DEs) of high burnup (HBU) (>45 GWd/MTU) spent nuclear fuel (SNF) rods from the North Anna Nuclear Power Station operated by Dominion Energy. The SNF rods, called sister rods or sibling rods, are all HBU and include four different kinds of fuel rod cladding: standard Zircaloy-4 (Zirc-4), low-tin Zirc-4, ZIRLO, and M5. The DEs are being conducted to obtain a baseline of the HBU rod’s condition before dry storage and are focused on understanding overall SNF rod strength and durability. Composite fuel and defueled cladding will be tested to derive material properties. Although the data generated can be used for multiple purposes, one primary goal for obtaining the post-irradiation examination data and the associated measured mechanical properties is to support SNF dry storage licensing and relicensing activities by (1) addressing identified knowledge gaps and (2) enhancing the technical basis for post-storage transportation, handling, and subsequent disposition.This appendix documents the status of the ORNL Phase 1 DE activities related to the mechanical testing of selected sister rods in Phase 1 of the sister rod test program.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Sister Rod Destructive Examinations (FY22) Appendix E: Mechanical Testing - Spent Fuel and Waste Disposition

As a part of the DOE NE High Burnup Spent Fuel Data Project, Oak Ridge National Laboratory (ORNL) is performing destructive examinations (DEs) of high burnup (HBU) (>45 GWd/MTU) spent nuclear fuel (SNF) rods from the North Anna Nuclear Power Station operated by Dominion Energy. The SNF rods, called sister rods or sibling rods, are all HBU and include four different kinds of fuel rod cladding: standard Zircaloy-4 (Zirc-4), low-tin Zirc-4, ZIRLO, and M5. The DEs are being conducted to obtain a baseline of the HBU rod’s condition before dry storage and are focused on understanding overall SNF rod strength and durability. Composite fuel and defueled cladding will be tested to derive material properties. Although the data generated can be used for multiple purposes, one primary goal for obtaining the post-irradiation examination data and the associated measured mechanical properties is to support SNF dry storage licensing and relicensing activities by (1) addressing identified knowledge gaps and (2) enhancing the technical basis for post-storage transportation, handling, and subsequent disposition. This report documents the status of the ORNL Phase 1 DE activities related to the mechanical testing of selected sister rods in Phase 1 of the sister rod test program.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2026

Identifying the Accuracy of Surface Roughness for Metal Additive Manufacturing Parts Captured with Computed Tomography Scanning

Conventional surface roughness measurement techniques require direct access to internal surfaces, often necessitating destructive sectioning of test articles. Computed tomography (CT) offers a non-destructive alternative for internal surface characterization, but its application in metrology remains unstandardized and sensitive to machine resolution and operator technique. This study investigates the feasibility of using CT scanning to quantify areal surface roughness in metal AM heat exchanger tubes with three distinct internal geometries: ribbed, discrete W, and featureless. CT-derived surface parameters were extracted using custom Python scripts and compared to measurements obtained from a focus variation microscope calibrated against a known standard. Results show that CT-based roughness measurements closely matched microscope values for the discrete W specimen, deviations between CT and microscope measurements were minimal—less than 1 µm—indicating reliable reconstruction. In contrast, the ribbed and featureless specimens, with lower roughness values showed greater discrepancies. The findings suggest that CT scanning can be a viable non-destructive metrology tool for AM parts with surface roughness above approximately 8 µm. For smoother surfaces, current CT capabilities may not provide sufficient accuracy, highlighting the need for resolution-aware workflows and further standardization in CT-based surface metrology.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Sister Rod Destructive Examinations (FY20) Appendix E: Mechanical Testing

This report documents work performed under the Spent Fuel and Waste Disposition’s Spent Fuel and Waste Science and Technology program for the US Department of Energy (DOE) Office of Nuclear Energy (NE). This work was performed to fulfill Level 2 Milestone M2SF-21OR010201032, “ORNL High Burnup Confirmatory Demo Sibling Rod Testing Results,” within work package SF-21OR01020103 and is an update to the work reported in M2SF-19ORO010201026 and M2SF-19OR010201028.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Slides on AFC-4C-R5 MNT20E destructive PIE :SEM, Micro-tensile testing, Post-test TEM Characterization

Slides containing updated PIE results for AFC-4C-R5 (MNT20E)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Quantitative Non-Destructive Evaluation of Fatigue Damage Based on Multi-Sensor Fusion

Based on sensor fusion and machine learning, this project developed a novel non-destructive evaluation (NDE) methodology, which consists of a remaining useful life (RUL) prediction framework and regression models for predicting residual stress and full width at half maximum (FWHM). A series of fatigue testing experiments were conducted using 5052-H32 aluminum alloy specimens. All specimens were measured using linear ultrasonic (LU) and nonlinear ultrasonic (NLU) testing methods non-destructively. Machine learning models were developed to use LU and NLU measurements to predict loading condition, fatigue level, residual stress, and FWHM. It was demonstrated that the developed methodology could distinguish new and fatigue specimens with an accuracy of 97.53%. Also, the prediction errors for residual stress and FWHM were as low as 4.73% and 1.62%, respectively. An interactive database was created to publicly share the data generated from the project. It is envisioned that the developed NDE technology will equip manufacturers with a responsive screening system for incoming used metallic components, and potentially lead to a significant increase in using used metallic components for remanufacturing.

42 ENGINEERING↗

DOE OSTI2021

UV-Fluorescence Imaging of Silicon PV Modules After Outdoor Aging and Accelerated Stress Testing

Fast, non-destructive, outdoor-compatible methods for photovoltaic module characterization are essential for monitoring module quality without disrupting energy production. UV-fluorescence (UVF) imaging of the encapsulant layer can be used for crack detection in the field. We show that UVF patterns vary widely between modules and types of applied stress. We propose that combining accelerated stress testing (e.g. thermal cycling and damp heat) with field investigations can help build understanding of different types of UVF, which are formed and subsequently quenched at varying rates. Ultimately, such understanding could enable estimating when cracks were formed.

41 EE - Solar Energy Technologies Office (EE-4S)↗

DOE OSTI2020

Testing of UV Oxidation Process for Acetonitrile Destruction

The Hanford Site Effluent Treatment Facility (ETF) currently treats aqueous waste streams that include condensates from the 242-A evaporator, leachate from the Environmental Restoration Disposal Facility (ERDF), as well as laboratory wastes and, in the future, will treat liquid effluents from the Hanford Waste Treatment and Immobilization Plant (WTP) and Integrated Disposal Facility (IDF) leachate. Liquid effluents from the WTP will have significant concentrations of acetonitrile. Acetonitrile is formed by reaction of nitrates and sugar in the WTP low activity waste (LAW) melters and is prevalent in the submerged bed scrubber (SBS) and wet electrostatic precipitator (WESP) liquid effluents from WTP off-gas treatment. When these liquids are concentrated in the WTP Effluent Management Facility (EMF) evaporator in the direct feed low activity waste (DFLAW) flow-sheet, testing has shown that the majority of the acetonitrile partitions to the evaporator condensate. Since the evaporator condensate is directed to the ETF, this creates a potential issue with the ETF waste acceptance criteria and, specifically, the ETF Delisting Modification treatability envelope limits. Consequently, there is a need to assess possible mitigation approaches, one of which involves identification and assessment of potential treatment processes to destroy the acetonitrile, which is the subject of the present report.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Anomaly Detection in Materials Digital Twins with Multiscale ICME for Additive Manufacturing

Detecting anomaly in fatigue and fracture experimental materials science is an interesting yet challenging topic. The reasons are threefold. First, the anomalous microstructure feature that gives rise to structural failure is small, sometimes in the order of 10 -7 of the interrogated volume. This, in turn, results in a highly imbalanced classification problem in machine learning (ML). Second, the consequence is high, in the sense that the test specimen is destructed in such case. Third, the convolution between microstructure stochasticity and the small probability of void nucleation, growth, and coalescence makes failure and fracture a hard-to-predict and challenging problem in materials science due to its irreproducibility, even experimentally. In this paper, we developed a materials digital twin and applied anomaly detection methods to detect voids and anomaly in additive manufacturing (AM). The materials digital twin is driven by two integrated computational materials engineering (ICME) models, which are kinetic Monte Carlo (kMC) and crystal plasticity finite element method (CPFEM). In conclusion, we demonstrated that by using anomaly detection, it is possible to detect voids and other defects in materials digital twin, which paves way for future research in integrating materials digital twin with its physical counterpart.

ICME↗

DOE OSTI2020

Cyclic deformation and lattice strain distribution of high Nb containing TiAl alloy

Low cycle fatigue of lamellar TiAl with 8.5 at.-%Nb was studied with a total strain amplitude of 0.28% at three temperatures: room temperature, 750°C and 900°C. At room temperature, the material exhibited cyclic hardening and the fracture mode was mainly interlamellar. At 750°C and 900°C, the material showed cyclic softening and the fracture mode was translamellar. The lattice strain in γ phase was almost tensile and larger tensile lattice strain in γ phase seems detrimental. Besides, the opposite direction of {201} γ and {100} α2 lead to crack propagation along α 2 /γ interfaces. B2/β o phase always suffered compressive lattice strain in the tests. Finally, the destruction of lamellar microstructure was the reason for colony refinement at 750°C and 900°C.

phase transformation↗

DOE OSTI2022

Non-destructive analysis of swelling in the EMPIrE fuel test

The European Mini-Plate Irradiation Experiment (EMPIrE) was designed to support the development and testing of a coated uranium-molybdenum (U-Mo) dispersion fuel for the conversion of select high-performance research reactors (HPRRs) to utilize low-enriched uranium (LEU). To aid in the development of the coated fuel form, the EMPIrE test included several plate designs and irradiated them in the Idaho National Laboratory (INL) Advanced Test Reactor (ATR) at a high meat power density (~21 kW/cm 3 ) and to high fuel particle fission densities (~6.4 × 10 21 fissions/cm 3 ). These conditions mimic the bounding conditions of the BR-2 reactor in Belgium, where a concurrent irradiation experiment was performed, and exceed those previously explored in dispersion U-Mo fuel plates. A local fuel swelling analysis, as determined through high-fidelity, post-irradiation mini-plate profilometry, was used along with statistical methods to non-destructively evaluate the overall performance and separate the effects of convoluted fabrication variables. While some effects observed with this non-destructive analysis were subtle, others had more significant, and possibly competing, effects on the fuel swelling behavior. In closing, these observations will be examined further with destructive examinations to more fully assess them as the fuel design is developed and qualified.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Multi-Scale Characterization of Porosity and Cracks in Silicon Carbide Cladding after Transient Reactor Test Facility Irradiation

Silicon carbide (SiC) ceramic matrix composite (CMC) cladding is currently being pursued as one of the leading candidates for accident-tolerant fuel (ATF) cladding for light water reactor applications. The morphology of fabrication defects, including the size and shape of voids, is one of the key challenges that impacts cladding performance and guarantees reactor safety. Therefore, quantification of defects’ size, location, distribution, and leak paths is critical to determining SiC CMC in-core performance. This research aims to provide quantitative insight into the defect’s distribution under multi-scale characterization at different length scales before and after different Transient Reactor Test Facility (TREAT) irradiation tests. A non-destructive multi-scale evaluation of irradiated SiC will help to assess critical microstructural defects from production and/or experimental testing to better understand and predict overall cladding performance. X-ray computed tomography (XCT), a non-destructive, data-rich characterization technique, is combined with lower length scale electronic microscopic characterization, which provides microscale morphology and structural characterization. This paper discusses a fully automatic workflow to detect and analyze SiC-SiC defects using image processing techniques on 3D X-ray images. Following the XCT data analysis, advanced characterizations from focused ion beam (FIB) and transmission electron microscopy (TEM) were conducted to verify the findings from the XCT data, especially quantitative results from local nano-scale TEM 3D tomography data, which were utilized to complement the 3D XCT results. In this work, three SiC samples (two irradiated and one unirradiated) provided by General Atomics are investigated. The irradiated samples were irradiated in a way that was expected to induce cracking, and indeed, the automated workflow developed in this work was able to successfully identify and characterize the defects formation in the irradiated samples while detecting no observed cracking in the unirradiated sample. These results demonstrate the value of automated XCT tools to better understand the damage and damage propagation in SiC-SiC structures for nuclear applications.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗