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All sources NASA NTRS DOE OSTI

DOE OSTI2018

Tensile Testing of Generation II FeCrAl Tubing

FeCrAl tubing is being developed as an improved accident tolerant cladding material for light water reactor fuels. A very promising generation FeCrAl alloy, C26M, is not being produced in long tubing for future reactor testing. In this report, the results of two FeCrAl tubes are presented. Tubes from two different heats of C26M are tested. Tensile tests were conducted in air at room temperature, 300 °C, and 600 °C.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2018

Beam current effect as a potential challenge in SEM-EBSD in situ tensile testing

Highlights: • In situ SEM-EBSD tensile tests were conducted using 304L steels with 8 and 10.4% Ni. • KAM and GROD evolution, twinning, and phase instability were investigated. • Phase transformation in 8% Ni-steel was sensitive to the electron beam current. In situ mechanical tensile tests coupled with electron backscatter diffraction (EBSD) analysis were conducted using specimens of two 304L steels with ~8 and 10.4% Ni content, respectively. Twinning was observed in steel with 10.4% Ni content, whereas steel with 8% Ni content demonstrated martensitic transformation. Testing showed that the kinetics of martensitic transformation in steel with 8% Ni content was influenced by the electron beam current used during EBSD scans. Continuous scanning using 32 nA nominal beam current led to suppression of the phase instability in the near-surface layer, but acceptable comparable-to-the-bulk results were obtained using 8 nA beam current. The exact mechanism of the beam current role is unclear, but it appears to be neutral regarding Kernel Average Misorientation behavior and deformation-induced twinning.

36 MATERIALS SCIENCE↗

DOE OSTI2021

A numerical and experimental approach to compare the effect of sample thickness in small in-situ SEM and large ex-situ tensile testing in Alloy 709

ASTM standards for tensile tests define specific sample size requirements regardless of grain size of the material. However, sample size requirements for testing should be considered in conjunction with the number of grains within its reduced cross-sectional area. This is particularly important for in-situ Scanning Electron Microscope (SEM) tensile tests, as they have to be conducted on smaller samples. In this study, a comprehensive experimental and numerical evaluation of the effect of specimen thickness (and the resulting number of grains within the cross-section) were conducted using in-situ SEM tensile test (on submillimeter thick samples) and ex-situ tensile tests (on samples of 0.68–5.9 mm thickness) and the results are compared with FEM simulations outcome. All tests were conducted at room temperature and the results are correlated to the number of grains within the thickness of specimens. The tensile test results indicated that even though the 0.2% proof stress and the tensile strength do not vary for the current range of thicknesses (with number of grains in the cross-section varying from 13 to 118), a difference in necking mechanism exists. Post tensile strength, thinner samples undergo more shear failure and diagonal localized necking whereas thicker samples experience more diffuse necking indicated by decreased area of shear failure at the edges and increased area of dimpled tensile failure at the center of the sample. Further, FEM results complement the experimental findings by showing the formation of conjugated localized shear bands on the upper and lower surface in the 0.68 mm thick sample and shear bands combining to form singular shear bands in thicker samples. These results also confirm the validity of the in-situ SEM tensile tests conducted on thinner samples as long as the required minimum number of grains exist within the cross-section.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Swab Tensile Testing and Procedures

This tensile test is to mimic the worst-case scenario of the swab being caught on an obstruction when being pulled out of the nasopharyngeal space. It is to determine how much tensile force the swab can withstand without breaking. A variety of different swabs (different materials and different geometries) were tested using the protocol outlined in Section 2 (Tensile Testing Procedure). Not all of the swabs were pre-treated using the Autoclave. For those swabs that were pre-treated using the Autoclave, the tensile tests were performed within 6 hours of completion of the Autoclave pre-treatment, unless otherwise noted. The FormLabs-USF and FormLabs-Northwell were printed at LLNL using FormLabs Surgical Grade V1 Resin on a Form 3B Printer. Results Summary: All FormLabs design and treatment variations (e.g. autoclaving and “aging”) had higher tensile strength compared commercial swabs. Autoclaving degraded the tensile strength. “Aging” after autoclaving improved the tensile strength. “Aging” without autoclaving degraded the tensile strength. No differences were observed in tensile strength with different autoclaving protocols. No significant differences were observed in tensile strength for different batches.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2020

Swab Tensile Testing Results and Procedures

36 MATERIALS SCIENCE↗

DOE OSTI2020

Swab Tensile Testing Results and Procedures

This tensile test is to mimic the worst-case scenario of the swab being caught on an obstruction when being pulled out of the nasopharyngeal space. It is to determine how much tensile force the swab can withstand without breaking. A variety of different swabs (different materials and different geometries) were tested using the protocol outlined in Section 2 (Tensile Testing Procedure). Not all of the swabs were pre-treated using the Autoclave. For those swabs that were pre-treated using the Autoclave, the tensile tests were performed within 6 hours of completion of the Autoclave pre-treatment, with the exception of the Injection Molded samples. For the Injection Molded samples, the tensile tests were performed within 24 hours of the completion of the Autoclave pre-treatment. The FormLabs-USF and FormLabs-Northwell were printed at LLNL using FormLabs Surgical Grade V1 Resin on a Form 3B Printer. All other samples were provided by HP.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Mechanical properties of neutron irradiated F82H using micro-tensile testing

Room temperature micro-tensile tests were successfully performed on F82H specimens neutron-irradiated at 573 K up to 5 dpa and unirradiated using a focused ion beam (FIB) device. Dimensions of the gauge section for micro-tensile specimens were about 10 µm (length) × 1 µm2 (area). These specimens were fabricated in a FIB device. The tensile properties obtained on specimens of micrometer size qualitatively agreed with results from millimeter size specimens. Using this micro-tensile testing technique is considered to become very useful data in combining the micro-tensile data on ion irradiated F82H with data on neutron irradiated material. This method overcomes the limitation on obtaining mechanical property on ion irradiated specimens to only micro-indentation testing.

Ando, Masami↗

DOE OSTI2018

Size Effect Studies on Tensile Tests for Hot Stamping Steel

Tensile tests have been widely used to determine basic mechanical properties of materials. However, the properties measured may be related to geometrical factors of the tested samples especially for high-strength steels; this makes the properties’ definitions and comparisons difficult. In this study, a series of tensile tests of ultra-high-strength hot-stamped steel were performed; the geometric shapes and sizes as well as the cutting direction were modified. The results demonstrate that the hot-stamped parts were isotropic and the cutting direction had no effect; the measured strengths were practically unrelated to the specimen geometries, including both size and shape. The elongations were slightly related to sample sizes within the studied range but highly depended on the sample shape, represented by the coefficient K. Such phenomena were analyzed and discussed based on microstructural observations and fracture morphologies. Moreover, two widely used elongation conversion equations, the Oliver formula and Barba’s law, were introduced to verify their applicability, and a new interpolating function was developed and compared.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Nanomechanical testing of freestanding polymer films: in situ tensile testing and Tg measurement

Abstract A method for small-scale testing and imaging of freestanding, microtomed polymer films using a push-to-pull device is presented. Central to this method was the development of a sample preparation technique which utilized solvents at cryogenic temperatures to transfer and deposit delicate thin films onto the microfabricated push-to-pull devices. The preparation of focused ion beam (FIB)-milled tensile specimens enabled quantitative in situ TEM tensile testing, but artifacts associated with ion and electron beam irradiation motivated the development of a FIB-free specimen preparation method. The FIB-free method was enabled by the design and fabrication of oversized strain-locking push-to-pull devices. An adaptation for push-to-pull devices to be compatible with an instrumented nanoindenter expanded the testing capabilities to include in situ heating. These innovations provided quantitative mechanical testing, postmortem TEM imaging, and the ability to measure the glass transition temperature, via dynamic mechanical analysis, of freestanding polymer films. Results for each of these mentioned characterization methods are presented and discussed in terms of polymer nanomechanics. Graphic Abstract

36 MATERIALS SCIENCE↗

DOE OSTI2024

Facile Tensile Testing Platform for In Situ Transmission Electron Microscopy of Nanomaterials

In situ tensile testing using transmission electron microscopy (TEM) is a powerful technique to probe structure-property relationships of materials at the atomic scale. In this work, a facile tensile testing platform for in situ characterization of materials inside a transmission electron microscope is demonstrated. The platform consists of: 1) a commercially available, flexible, electron-transparent substrate (e.g., TEM grid) integrated with a conventional tensile testing holder, and 2) a finite element simulation providing quantification of specimen-applied strain. The flexible substrate (carbon support film of the TEM grid) mitigates strain concentrations usually found in free-standing films and enables in situ straining experiments to be performed on materials that cannot undergo localized thinning or focused ion beam lift-out. The finite element simulation enables direct correlation of holder displacement with sample strain, providing upper and lower bounds of expected strain across the substrate. The tensile testing platform is validated for three disparate material systems: sputtered gold-palladium, few-layer transferred tungsten disulfide, and electrodeposited lithium, by measuring lattice strain from experimentally recorded electron diffraction data. The results show good agreement between experiment and simulation, providing confidence in the ability to transfer strain from holder to sample and relate TEM crystal structural observations with material mechanical properties.

2D materials↗

DOE OSTI2020

Swab Tensile Testing Results and Procedures - PA11 Rev. 10 Swabs

This tensile test is to mimic the worst-case scenario of the swab being caught on an obstruction when being pulled out of the nasopharyngeal space. It is to determine how much tensile force the swab can withstand without breaking. All swabs were provided by HP and were the PA11 material and Rev 10 design. All of the swabs were tested using the protocol outlined in Section 2 (Tensile Testing Procedure). Not all of the swabs were pre-treated using the Autoclave. For those swabs that were pre-treated using the Autoclave, the tensile tests were performed within 6 hours of completion of the Autoclave pre-treatment, with the exception of the “Aged” swabs. For the “Aged” swabs, the tensile tests were performed 7 days after the Autoclave pre -treatment. The “Aged” swabs that were not pre-treated using the Autoclave, were tested 7 days after those that were not “Aged.”

36 MATERIALS SCIENCE↗

DOE OSTI2025

Understanding the limitations and potential of micro tensile testing of tungsten and needs for crystal plasticity modelling

Tungsten is the leading plasma facing material candidate due to its exceptional properties. Understanding the response to neutron irradiation is crucial for the lifetime evaluation of tungsten. The limited space in nuclear reactors and the high levels of radioactivity of the specimens after irradiation are significant barriers to accurately measuring the mechanical properties after neutron irradiation. Testing of micro tensile specimens is one approach to reduce the total amount of irradiated material needed for a set of mechanical testing experiments. However, micro samples are not necessarily measuring the bulk material properties, as size effects produce higher measured mechanical properties than is observed in engineering size counterparts. Determining the minimal sample size for reliable bulk property measurement, combined with modeling efforts, is essential. We conducted room temperature tensile tests on tungsten micro tensile specimens fabricated with focused ion beam, plasma focused ion beam and femto-second laser ablation system to dimension of 2×2×7?µm³, 7×7×18?µm³, and 80×100×233?µm³ (width×thickness×gauge-length), respectively. Elevated tensile testing was performed up to 475°C on 5×5×18?µm³ specimens fabricated with focused ion beam. The smallest specimens exhibited a high degree of ductility and strength, whereas the largest specimens demonstrated behavior akin to bulk tungsten. To investigate the effects introduced by the micro specimen fabrication processes and to obtain the necessary bulk dislocation density for the crystal plasticity model, we employed X-ray diffraction depth profiling. This measurement was performed using different X-ray sources with varying penetration depths. Finally, the potential and limitations of micro mechanical tests for tungsten will be discussed.

36 - MATERIALS SCIENCE↗

DOE OSTI2021

Analyzing the effect of misalignment on single-filament carbon fiber tensile testing via stereoscopic computer vision imaging

An understanding of the constitutive properties of carbon fibers (CF) is critical to the accuracy of high-resolution composite simulations and to the development of CF derived from low-cost alternative precursor materials. Single-fiber tensile testing is a capable tool to measure CF properties and is well suited to research efforts where only a small number of fibers may be available. However, single-fiber tensile tests are challenging to conduct due to the difficulty in handling small diameter fibers (5-15 μm), the brittleness of single fibers, and the required nanoscale/microscale resolution of testing equipment. The accuracy of the measured properties depends on several factors, but a critical factor is fiber misalignment, especially at short gauge lengths. Current standards do not address the effect of tensile specimen misalignment on measured properties. Furthermore, this work presents a robust method of fiber alignment using stereoscopic computer vision that enables users to align fibers vertically for tensile testing to improve the accuracy of resulting mechanical properties. Additionally, an analytical relationship between fiber misalignment angle and measured properties is developed and validated against the experimental results. As a result, new best practices for single-fiber tensile testing of CF are recommended.

47 OTHER INSTRUMENTATION↗

DOE OSTI2023

Investigating the failure behavior of cast Al-11Ce-0.4Mg alloys using in-situ scanning electron microscopy tensile testing

Within the last decade, research on Al-Ce-Mg alloys has reported promising results for use in cast part applications. In this paper, the failure behavior of cast Al-11Ce-0.4Mg (wt%) was investigated experimentally with focus on the effect the matrix and intermetallic phases have on the fracture propagation behavior at failure. For the first time, in-situ SEM tensile testing was used to study the failure behavior of cast Al-Ce alloys, reporting results for uniaxial, DIC, and single edge notch tensile tests. The results of the in-situ SEM tensile testing were compared with the materials characterization experiments, which included serial sectioning, EBSD, EDS, and fractography. Analysis of EBSD and EDS mapping of cast Al-11Ce-0.4Mg showed that the cast microstructure was a hypereutectic two phase Al-Ce alloy with grains encompassing large complex colonies of laminar eutectic Al 11 Ce 3 intermetallic. The uniaxial tensile results reported the effect casting defects have on the strength and ductility of the alloy, and DIC in-situ testing showed that the eutectic colonies plastically deform less than the matrix phase. In-situ SEM single edge notch tensile testing displayed how the strength of an individual phase affected the crack propagation direction in the alloy. The results of both the materials characterization and in-situ tensile testing experiments on the failure of this alloy revealed further directions for future alloy development that can improve both the strength and fracture toughness of Al-Ce-Mg alloys.

36 MATERIALS SCIENCE↗

DOE OSTI2020

Swab Tensile Testing - HP Rev 10 Summary

42 ENGINEERING↗

DOE OSTI2022

Measurement of grain boundary strength of Inconel X-750 superalloy using in-situ micro-tensile testing techniques in FIB/SEM system

Grain boundaries (GBs), known as two-dimensional defects, are omnipresent in polycrystalline metallic alloys and thus influence a wide range of mechanical properties under different environmental conditions like irradiation and corrosion. Therefore, quantifying the strength of individual GBs is critical for understanding the degradation of mechanical properties of materials under different conditions. In this study we developed an efficient approach for the fabrication of micro-tensile specimens with a GB almost perpendicular to the tensile direction, which is expected to advance the development of individual GB tensile testing at micro or nanoscale in a wide scope of materials. Further, an in-situ cantilever micro-tensile testing method was developed and used to quantify the strength of a Σ3 GB in Inconel X-750 with the combination of finite element modeling. The average ultimate tensile strength (UTS) of a non-irradiated Σ3 GB is estimated at around 1.4 GPa, comparable to that of a neutron-irradiated Σ3 GB with a dose of ~1.5 dpa (1.3 GPa). Moreover, the in-situ push-to-pull micro-tensile testing technique developed in this work provides valuable insights into the high-angle GB deformation and fracture behavior. This method generates qualitatively similar ductility behavior before and after neutron irradiation as the bulk material testing. However, the ductility and UTS values obtained from this method are different from bulk measurements due to vastly different specimen dimensions.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Length scale effects of micro- and meso-scale tensile tests of unirradiated and irradiated Zircaloy-4 cladding

Zircaloy-4 is an essential material for cladding structures within fission-based reactors. To explore the changes in properties measured on differing length scales, FIB-machined micro-scale tensile tests were performed on both irradiated and control groups of Zircaloy-4. This was correlated with tensile testing on femtosecond laser-machined meso-scale specimens. Pronounced size effects were found when varying specimen geometry. Increases in tensile geometry size were associated with a reduction in measured yield stress for both irradiated and unirradiated samples. Here, meso-scale testing found strength and strain values similar to that of bulk-scale testing.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Toward Standardized Microscale Tensile Testing for Two‐Photon Polymerization‐Fabricated Materials in Liquid

Two-photon polymerization (TPP) enables the fabrication of intricate 3D microstructures with submicron precision, offering significant potential in biomedical applications like tissue engineering. In such applications, to print materials and structures with defined mechanics, it is crucial to understand how TPP printing parameters impact the material properties in a physiologically relevant liquid environment. Herein, an experimental approach utilizing microscale tensile testing (μTT) for the systematic measurement of TPP-fabricated microfibers submerged in liquid as a function of printing parameters is introduced. Using a diurethane dimethacrylate-based resin, the influence of printing parameters on microfiber geometry is first explored, demonstrating cross-sectional areas ranging from 1 to 36 μm 2 . Tensile testing reveals Young's moduli between 0.5 and 1.5 GPa and yield strengths from 10 to 60 MPa. The experimental data show an excellent fit with the Ogden hyperelastic polymer model, which enables a detailed analysis of how variations in writing speed, laser power, and printing path influence the mechanical properties of TPP microfibers. The μTT method is also showcased for evaluating multiple commercial resins and for performing cyclic loading experiments. Collectively, this study builds a foundation toward a standardized microscale tensile testing framework to characterize the mechanical properties of TPP printed structures.

mechanical characterization↗