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INSTRUMENTATION FOR IN-CORE REAL-TIME MECHANICAL TESTING OF STRUCTURAL MATERIALS (INCREASE) PROJECT

Idaho National Laboratory (INL), in collaboration with the Electric Power Research Institute (EPRI), Nuclear Regulatory Commission, French Atomic and Alternative Energies Commission (CEA), Joint Research Centre, Nuclear Research and Consultancy Group, and Research Center Rez, is the operating agent of the In-Core Real-Time Mechanical Testing of Structural Materials (INCREASE) joint experimental program (JEEP) project that operates within the Nuclear Energy Agency (NEA)’s Framework for Irradiation Experiments (FIDES-II) program. The first objective of the INCREASE project is to design a shared capsule that can house a variety of in-core mechanical testing instrumentation for enabling smart irradiation experiments. The second objective is to collect in core stress relaxation data pertaining to high priority stainless steel (SS) materials under light water reactor conditions with target temperature of 340°C +/-20°C and a minimum neutron damage of 2 displacement per atom (dpa). The INCREASE project will be demonstrated in the Massachusetts Institute of Technology Nuclear Research Reactor (MITR).

36 MATERIALS SCIENCE↗

FY24 Integrated Results for High-Temperature Mechanical Testing of LPBF 316H Stainless Steel

This report provides the mechanical test data of laser powder bed fusion (LPBF) 316H stainless steel (SS) collected during Fiscal Year 2024 (FY 24) under the US Department of Energy, Office of Nuclear Energy’s Advanced Materials and Manufacturing Technologies program, along with the current state of microstructural-based understandings of the behaviors. Materials with variabilities in manufacturing site, machine, laser parameters, powder chemistry, porosity, specimen geometry and heat treatment were tested in high-temperature tension, creep, fatigue and creep-fatigue. Electron microscopy and optical microscopy were performed on selected materials before and after the tests to provide microstructural-based understandings to the mechanical behavior. It was discovered that the as-built (AB) and stress-relieved (SR) materials exhibit similar behaviors in tension and creep, as do the solution-annealed (SA) and hot-isostatic pressed (HIP) materials. The AB and SR materials are softer but more ductile than the SA and HIP materials in tension. In creep, the LPBF materials have comparable rupture times but lower rupture strains compared to the wrought materials. The AB and SR materials have low creep rupture strains (<10%) when tested at 720°C and 800°C, while the SA and HIP materials are much more ductile. The LPBF materials exhibit large scatter in fatigue and creep-fatigue lives. The cyclic lives of creep-fatigue tests are lower than those of fatigue tests. In fatigue and creep-fatigue, SR materials outperform SA materials. A common observation from the cyclic tests is that, given the same post-build heat treatment, a lower initial peak stress generally results in a longer cyclic life regardless of hold time. It was also discovered that the batch variation can be more impactful than heat treatment, as demonstrated by the overall better performance of one batch of material than another, regardless of the heat treatment. The results provided insights into how different factors impact the behaviors of LPBF 316H SS. An outlook to FY 25 work scope is provided.

36 MATERIALS SCIENCE↗

Mechanism test bed. Flexible body model report

The Space Station Mechanism Test Bed is a six degree-of-freedom motion simulation facility used to evaluate docking and berthing hardware mechanisms. A generalized rigid body math model was developed which allowed the computation of vehicle relative motion in six DOF due to forces and moments from mechanism contact, attitude control systems, and gravity. No vehicle size limitations were imposed in the model. The equations of motion were based on Hill's equations for translational motion with respect to a nominal circular earth orbit and Newton-Euler equations for rotational motion. This rigid body model and supporting software were being refined.

Compton, Jimmy↗

Experimental Evaluation of Interfacial Bonding Strength Between 304 Stainless Steel Substrate and Electrodeposited Nickel Coating Using Mesoscale Mechanical Testing Methods

Electrodeposition is a commonly used method for depositing a metal layer on a metallic substrate, to provide a decorative finish or for functional purposes including wear and corrosion resistance. The interfacial bonding strength is a critical factor in determining the quality of electrodeposition, as it ensures the adhesion of the deposited layer to the substrate. Despite its importance, there has not previously been a suitable mechanical testing method to quantitatively characterize the bonding strength between the electrodeposited layers and the substrate, due to the high strength of the materials and to restrictions imposed by the geometry (due to the small thickness of the plating layer) to manufacture tensile bars. In this study, we introduce a novel mesoscale mechanical testing method to overcome these limitations. This technique was applied to assess the bonding strength between a 304 stainless steel (SS) substrate and electrodeposited nickel with three different plating formulae (nickel sulfamate, Watts bath, and hard nickel). The thickness of the pure nickel coatings achieved for each of the three electrolyte solutions was approximately 1 mm on each side of the substrate. Mesoscale tensile bars of 1 mm length were manufactured by a femtosecond laser, with the material interface at the center of the gauge section, and then tensile-tested with digital image correlation. Further, the results proved that the electrodeposition technique is able to produce a very high bonding strength that is close to the yield strength of both the substrate material and the electrodeposited nickel layer. Additionally, in the case of the Watts bath formula, the interfacial bonding strength between the SS 304 and electrodeposited nickel can exceed that of the nickel layer. This method is expected to be useful for quantifying the interfacial bonding strength in numerous applications.

36 MATERIALS SCIENCE↗

Initial Mechanical Testing of Superalloy Lattice Block Structures Conducted

The first mechanical tests of superalloy lattice block structures produced promising results for this exciting new lightweight material system. The testing was performed in-house at NASA Glenn Research Center's Structural Benchmark Test Facility, where small subelement-sized compression and beam specimens were loaded to observe elastic and plastic behavior, component strength levels, and fatigue resistance for hundreds of thousands of load cycles. Current lattice block construction produces a flat panel composed of thin ligaments arranged in a three-dimensional triangulated trusslike structure. Investment casting of lattice block panels has been developed and greatly expands opportunities for using this unique architecture in today's high-performance structures. In addition, advances made in NASA's Ultra-Efficient Engine Technology Program have extended the lattice block concept to superalloy materials. After a series of casting iterations, the nickel-based superalloy Inconel 718 (IN 718, Inco Alloys International, Inc., Huntington, WV) was successfully cast into lattice block panels; this combination offers light weight combined with high strength, high stiffness, and elevated-temperature durability. For tests to evaluate casting quality and configuration merit, small structural compression and bend test specimens were machined from the 5- by 12- by 0.5-in. panels. Linear elastic finite element analyses were completed for several specimen layouts to predict material stresses and deflections under proposed test conditions. The structural specimens were then subjected to room-temperature static and cyclic loads in Glenn's Life Prediction Branch's material test machine. Surprisingly, the test results exceeded analytical predictions: plastic strains greater than 5 percent were obtained, and fatigue lives did not depreciate relative to the base material. These assets were due to the formation of plastic hinges and the redundancies inherent in lattice block construction, which were not considered in the simplified computer models. The fatigue testing proved the value of redundancies since specimen strength was maintained even after the fracture of one or two ligaments. This ongoing test program is planned to continue through high-temperature testing. Also scheduled for testing are IN 718 lattice block panels with integral face sheets, as well as specimens cast from a higher temperature alloy. The initial testing suggests the value of this technology for large panels under low and moderate pressure loadings and for high-risk, damage-tolerant structures. Potential aeropropulsion uses for lattice blocks include turbine-engine actuated panels, exhaust nozzle flaps, and side panel structures.

Krause, David L.↗

Hydraulic Apparatus for Mechanical Testing of Nuts

The figure depicts an apparatus for mechanical testing of nuts. In the original application for which the apparatus was developed, the nuts are of a frangible type designed for use with pyrotechnic devices in spacecraft applications in which there are requirements for rapid, one-time separations of structures that are bolted together. The apparatus can also be used to test nonfrangible nuts engaged without pyrotechnic devices. This apparatus was developed to replace prior testing systems that were extremely heavy and immobile and characterized by long setup times (of the order of an hour for each nut to be tested). This apparatus is mobile, and the setup for each test can now be completed in about five minutes. The apparatus can load a nut under test with a static axial force of as much as 6.8 x 10(exp 5) lb (3.0 MN) and a static moment of as much as 8.5 x 10(exp 4) lb in. (9.6 x 10(exp 3) N(raised dot)m) for a predetermined amount of time. In the case of a test of a frangible nut, the pyrotechnic devices can be exploded to break the nut while the load is applied, in which case the breakage of the nut relieves the load. The apparatus can be operated remotely for safety during an explosive test. The load-generating portion of the apparatus is driven by low-pressure compressed air; the remainder of the apparatus is driven by 110-Vac electricity. From its source, the compressed air is fed to the apparatus through a regulator and a manually operated valve. The regulated compressed air is fed to a pneumatically driven hydraulic pump, which pressurizes oil in a hydraulic cylinder, thereby causing a load to be applied via a hydraulic nut (not to be confused with the nut under test). During operation, the hydraulic pressure is correlated with the applied axial load, which is verified by use of a load cell. Prior to operation, one end of a test stud (which could be an ordinary threaded rod or bolt) is installed in the hydraulic nut. The other end of the test stud passes through a bearing plate; a load cell is slid onto that end, and then the nut to be tested is threaded onto that end and tightened until the nut and load cell press gently against the bearing plate.

Hinkel, Todd J.↗

Small-scale mechanical testing and characterization of fuel cladding chemical interaction between HT9 cladding and advanced U-based metallic fuel alloy

Fuel cladding chemical interactions (FCCI) occurred on the interface between the nuclear metal fuel and cladding is the primary cause of cladding wastage, weakening cladding mechanical integrity, and placing fuel and cladding at risk. Although the microstructural and phase information of FCCI has been fairly understood, mechanical properties remain less studied due to limited reaction volume. Here, through a combining of advanced electron microscopy characterizations and small-scale mechanical testing techniques, including indentation and micro-tensile testing, this study investigated the microscale mechanical properties of FCCI between the ferritic/martensitic (F/M) HT9 cladding and an advanced Uranium (U)-based metallic fuel irradiated at the Advanced Test Reactor to 2.2% FIMA with peak inner cladding temperature reached to 650 °C. Mechanical testing results show significant hardening and embrittlement in the FCCI region. The brittle fracture of FCCI specimen is mainly attributed to the formation of nano-crystallized intermetallic σ-FeCr phase. Whereas mechanical softening was revealed in the unreacted HT9 matrix due to irradiation-induced microstructural and microchemical evolution, specifically, the disappearance of martensitic lath structure and the formation of Fe 2 Mo Laves phase precipitation which consumed the solid solution strengthening Mo from the F/M HT9 matrix. Due to the achieved high cladding temperature, this fuel pin is of particular significance for revealing the high-temperature irradiation effect on the mechanical properties of HT9 cladding. Therefore, the outcomes of this study are expected to contribute to the development of multi-scale mechanical behavior modeling of HT9 cladding for Generation IV reactors which requires cladding to run at higher temperature (above 600 ?).

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Micro-Scale Mechanical Testing of Non-Woven Carbon Nanotube Sheets and Yarns

Non-woven carbon nanotube (CNT) sheets and yarns were tested using a novel micro-scale mechanical testing system. CNT sheets were observed to delaminate during uniaxial testing using an adbesive gripping method, resulting from a higher proportion of load bearing in the outer sheets versus internal sheets and an apparently low interlaminar shear strength. In response to this, a new spool-grip method was used to alleviate non-uniform through-thickness stresses, circumvent premature delamination, and allow the sheet material to sustain a 72% increase in measured tensile strength. Furthermore, tension tests of CNT yarns showed that the yarn-structure was approximaiely 7 times stronger than the sheet structure, owing to a higher degree of CNT alignment in the test direction.

Magargee, J.↗

Thermal-Mechanical Testing of Hypersonic Vehicle Structures

A viewgraph presentation describing thermal-mechanical tests on the structures of hypersonic vehicles is shown. The topics include: 1) U.S. Laboratories for Hot Structures Testing; 2) NASA Dryden Flight Loads Laboratory; 3) Hot Structures Test Programs; 4) Typical Sequence for Hot Structures Testing; 5) Current Hot Structures Testing; and 6) Concluding Remarks.

Hudson, Larry↗

Manufacturing and Mechanical Testing of TC1225/LM-PAEK and TC1200/PEEK Thermoplastic Composite Panels

Development of thermoplastic composites (TPCs) for aerospace structures is experiencing renewed enthusiasm attributed to the availability of rapid manufacturing technology, ease of joining through fusion welding processes, and the successful utilization of the material in flight critical structures. Semicrystalline thermoplastics such as polyether ether ketone (PEEK), polyether ketone ketone (PEKK), and polyphenylene sulfide (PPS) have been successfully demonstrated as thermoplastic skins, keel beams, and angle brackets for commercial aircraft. Composite specimens were fabricated from the Toray TC1225 and TC1200 unidirectional prepreg systems and tested to gain confidence with NASA in-house TPC processing as part of the Thermoplastics Development for Exploration Application (TDEA) project. TC1225 is a relatively new material system that uses T700GC fibers and low-melt polyaryl ether ketone (LM-PAEK) resin. TC1200 is the latest version of a material system that has been available for several decades with AS4 fibers and PEEK resin. Results for ultrasonic inspection, optical microscopy, acid digestion, and differential scanning calorimetry establish the quality of the panels. Mechanical test data for unnotched and notched laminate tension and compression as well as compression after impact provide data for equivalency assessment and support material selection in TDEA. Satisfactory equivalence of the TC1225 results and the National Center for Advanced Materials Performance (NCAMP) database was found. The results indicate high-quality manufacturing was achieved, and the resulting mechanical test data are in agreement with that in the literature.

Thermoplastic Composites↗

Mechanical Testing of MLCCs

Cracking of multilayer ceramic capacitors, MLCCs, remains a serious problem for space systems. This problem increases substantially for large size capacitors and in cases when manual soldering is involved or the system experiences mechanical shock or vibration. In any case, a fracture occurs when the sum of external and internal mechanical stresses exceeds the strength of the part. To reduce the probability of cracking, the level of stress should be reduced, e.g. by optimizing the assembly workmanship and rules for board design, and the strength of the parts increased by selecting the most mechanically robust capacitors. The latter might possibly be achieved by selecting MLCCs based on the in-situ measurements of mechanical characteristics using four types of tests: flexural strength, hardness, fracture toughness, and flex bend testing. Note that military specifications MIL-PRF-123 and MIL-PRF-55681 do not have requirements for mechanical testing of the parts. However, specifications for automotive industry components employ two types of mechanical tests: beam load (break strength) test per AEC-Q200-003 and board flex test per AEC-Q200-005. A recent military specification for thin dielectric capacitors, MIL-PRF-32535, has one mechanical test, board flex testing, that is similar to AEC-Q200-005. The purpose of this report was assessment of the efficiency of different mechanical tests for selection robust capacitors and comparison of mechanical characteristics of Base Metal Electrode (BME) and Precious Metal Electrode (PME) capacitors. The report has three parts related to the first three mechanical tests mentioned above.

Precious Metal Electrode (PME) capacitors↗

Mechanical testing of large thallium doped sodium iodide single crystals

The findings of mechanical tests performed on five thallium-doped sodium iodide NaI(Tl) crystals are presented. These crystals are all in the shape of circular flat plates, 20.0 in. in diameter an d0.5 in. thick. The test setup, testing procedure, and the test data are presented. Large crystals exhibit a high degree of material plasticity, as well as a much higher strength than previously anticipated, on the order of 500 psi. Also revealed from the testing is the fact that crystal with a large number of grain boundaries developed less plasticity, and therefore less permanent deformation, than those with fewer grain boundaries.

Lee, H. M.↗

Fracturing process of micro-concrete under uniaxial and triaxial compression: Insights from in-situ X-ray mechanical tests

This paper presents an experimental study of concrete at meso-scale (aggregates, macro-pores and mortar matrix) in order to get a better understanding of the local failure mechanisms known to drive the macroscopic mechanical behaviour of the material. The main originality comes from conducting in-situ X-ray mechanical tests on micro-concrete samples of realistic composition (including cement, sand, aggregates and water), under uniaxial compression and, for the first time, under triaxial compression at 5 MPa, 10 MPa and 15 MPa confining pressures. A timeseries analysis of the set of 3D images coming from each test allows for the measurement of the 3D kinematic fields (displacement and strain fields) throughout the experiments. The different failure patterns observed for each loading path are discussed, along with a quantification of the 3D fracturing processes at the scale of the largest heterogeneities (aggregates and macro-pores). With an increasing level of confinement, the transition from brittle to ductile response is observed, as well as an increase of the strength of the material. The pronounced impact of the meso-scale heterogeneities of concrete on their local failure mechanisms is highlighted. It is shown that strain localisation mainly originates between aggregates and mortar matrix, with the shape and location of the largest aggregates and macro-pores essentially driving the propagation of the cracking network.

36 MATERIALS SCIENCE↗

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↗

In-Situ Scanning Electron Microscope Experiments for Microscale Mechanical Testing and Validated Modeling of Fiber Reinforced Thermoplastics

A novel, in-situ, scanning electron microscope (SEM) mechanical testing capability for materials at the microscale which provides experimental validation to a machine learning (ML) toolset for full-field validation of physics-based micromechanics models is being developed by researchers at NASA Glenn Research Center. These are enabling technologies for the integration of multiscale digital twins for materials into system level models which will result in the improved performance, material discovery, reduced production cost and time, rapid characterization, and prognostic structural health monitoring (SHM) for materials and structures for extreme environments in support of NASA space exploration missions. In order to bridge the material structure-to-system gap for digital twins, physics-based models must be experimentally validated at multiple length scales. Seminal microscale experiments, conducted at the Air Force Research Laboratory (AFRL), were limited to transverse compression of single-layer, unidirectional thermoset polymer matrix composite (PMC) micropillar specimens [1]. The early phases of the current project followed those initial results and setup to reproduce the compression testing of PMC material on the custom-built piezoelectric actuated micromechanical testing rig built by MicroTesting Solutions LLC. In this work, samples of thermoplastic PMC material were first machined into 3 mm cubes, and then further machining and final milling was done using a Focused Ion Beam (FIB). The initial experiment was done on a pillar roughly 20 µm x 20 µm x 40 µm tall. Additional pillars were milled with final sizes ranging from 20 µm x 20 µm x 40 µm tall to 40 µm x 40 µm x 65 µm tall. A speckle pattern for in-situ full-field measurements using Digital Image Correlation (DIC) was applied with platinum, which was coated on the surface, and then the FIB was used to mill away some of the coating to produce an irregular pattern of Pt on the pillar surface. The samples were loaded into the custom testing rig and placed into the SEM and loaded under compression until failure. Images were collected in the SEM during testing. Post-processing of the images was conducted using DIC to obtain full-field displacement and strain measurements elucidating the role of the matrix as well as fiber-fiber interaction at the microscale within the composite subjected to compression loading well into the non-linear regime of the material. Moreover, the evolution of fiber-matrix debonding and matrix cracking is observed in-situ at the microscale. This data, along with images segmented with a newly developed ML toolset [2], was used to create and validate physics-based micromechanics models. An image of the failed micropillar is shown in Figure 1. The techniques developed in the initial compression experiment was tailored to the validation needs of the models and expanded to include different sized samples as well as possibly tension and fatigue.

Laura Wilson↗

Final Status Report Confirming Completion of Mechanical Testing of HFIR Irradiated Nanocomposite Materials

This report provides a final status report on the in-cell mechanical testing of High Flux Isotope Reactor (HFIR)-irradiated nanodispersion-strengthened materials at the Irradiated Materials Examination and Testing (IMET) facility. All tension tests were performed at room temperature with a nominal strain rate of 0.018 mm/mm/min using shoulder-loading grip sets by following the standard testing procedure in ASTM E8/E8M. Round 1 (unirradiated) and round 2 (0.7 dpa) testing was completed in FY 2021. This report confirms completion of round 3 (1.4 dpa) and round 4 (2.1 dpa) tensile testing in FY 2022 with examples of test data collected on select sample conditions. Additionally, the report includes IDs of samples selected for shipment to Idaho National Laboratory (INL) for additional characterization.

36 MATERIALS SCIENCE↗

Mechanical testing of PH13-8Mo H950 Steel for Xue-Wierzbicki Fracture Criterion Determination at 20° C and -40° C

Mechanical testing was conducted to collect the data needed to build a Xue-Wierzbicki (XW) fracture model for PH13-8 Mo H950 stainless steel (PH 13-8 SS). This model is intended for use in structural analysis of this material between room temperature and -40° C. Tests were performed on four different specimen geometries such that a range of stress states were characterized at room temperature and -40° C. Tensile tests on R5 tensile specimens were also performed to assess material anisotropy. Fracture toughness test were also conducted. The fracture toughness of this material at -40° C was 68% of the room-temperature value. Material strength generally increased with decreasing temperature while the opposite trend was observed for ductility. These trends were most pronounced for specimens with the largest stress triaxialities.

36 MATERIALS SCIENCE↗

ISS SGANT Group Level Offloading Test Mechanism

The International Space Station (ISS) Space-to-Ground Antenna (SGANT) is used for ISS communication with earth through the Tracking and Data Relay Satellite (TDRSS). Due to the different speeds of travel between earth, ISS and TDRSS, a steerable SGANT was required on the ISS. The mechanical design of SGANT is an unbalanced mechanism with insufficient strength and driving torque to support and drive itself in a 1G environment. For ground testing, a specially designed offloading mechanism is required. Basically, the test mechanism must offload the SGANT in a two-axis operation, allowing the SGANT to move within a specific range, speed and acceleration; therefore the SGANT can move from elevation 0 to 90 deg and be tested at both the 0 and 90 deg positions. The load introduced by the test equipment should be less than 10.17 N-m (7.5 ft-lbf). The on-ground group level tracking test is quite challenging due to the unbalanced antenna mechanical design and tough specification requirements. This paper describes the detailed design, fabrication, and calibration of the test mechanism, and how the above requirements are met. The overall antenna is simplified to a mass model in order to facilitate the offloading mechanism design and analysis. An actual SGANT mass dummy was made to calibrate the system. This paper brings together the theoretical analysis and the industrial experience that were relied upon to meet the above-mentioned requirements for the ground test. The lessons learned during the calibration phase are extremely important for future double or multiple offloading system designs. The ISS SGANT QM and FM units passed their ground test and the SGANT/Boom fit check successfully, and the Flight Model (FM) was delivered to SSPF in April 1998. It is now installed on ISS and functioning well.

Zhang, Xi-Lin↗