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At least 397 records · Page 22

In Situ Radiography During Tensile Tests

Laboratory system for testing specimens of metal-, ceramic-, and intermetallic-matrix composite materials incorporates both electromechanical tensile-testing subsystem and either of two imaging subsystems that take x-ray photographs of specimens before, during, and after tensile tests. Used to test specimens of reaction-bonded silicon nitride reinforced with silicon carbide fibers (SiC/RBSN) considered for high-temperature service in advanced aircraft turbine engines. Provides data on effects of preexisting flaws (e.g., high-density impurities and local variations of density) on fracture behavior. Accumulated internal damage monitored during loading. X-ray source illuminates specimen in load frame while specimen is pulled. X-ray images on film correlated with stress-vs.-strain data from tensile test.

Baaklini, George Y.↗

Hoop Tensile Characterization Of SiC/SiC Cylinders Fabricated From 2D Fabric

Tensile stress-strain properties in the hoop direction were obtained for 100-mm diameter SiC/SiC cylinders using ring specimens machined from the cylinder ends. The cylinders were fabricated from 2D balanced fabric with several material variants, including wall thickness (6, 8, and 12 plies), Sic fiber type (Sylramic, Sylramic-iBN, Hi-Nicalon, and Hi-Nicalon S), fiber sizing type, and matrix type (full CVI Sic, and partial CVI plus melt-infiltrated SiC-Si). Fiber ply splices existed in the all the hoops. Tensile hoop measurements were made at room temperature and 1200 C using hydrostatic ring test facilities. The hoop results are compared with in-plane data measured on flat panels using same material variants, but containing no splices.

Verrilli, Michael J.↗

Report on Evolution of Inconel 718 Following HFIR Irradiation

The report presents the microstructure and mechanical properties of 3D printed Inconel 718 after irradiation in the High Flux Isotope Reactor (HFIR) at Oak Ridge National Laboratory (ORNL) to assess its potential use as a structural material. The structural components near the outlets of several proposed reactor cores will experience significant neutron fluxes and outlet coolant temperatures ranging from the hot standby temperature of 300 °C to nearly 550 °C at the center of the part. These components must support the core in appropriate loading conditions and require structural analysis at relevant temperatures. In FY21, three heat treatments were designed and conducted to simplify the microstructure and to determine how each precipitating phase contributed to the overall strength. In FY21, baseline mechanical properties were measured from uniaxial tensile tests on subsize SS-J2 specimens at room temperature and at elevated temperatures of 300, 450, and 600 °C to serve a comparison to the irradiated properties. Four capsules containing 3D printed Inconel 718 were inserted into HFIR in FY21 for a matrix of two temperatures and two doses. The lower of the two doses was available for characterization in FY22. Multiple heat treatments of Inconel 718 irradiated to nominal conditions of 2 displacements per atom (dpa) at either 300 or 600 °C were strained with uniaxial tensile tests at the Irradiated Material Examination and Testing (IMET) Facility to discern the mechanical properties. Transmission electron microscopy was performed to correlate the observed mechanical properties with nanoscale features. The initially homogenous AM718-HM increased in strength at both irradiation temperatures based on a high density of nanometer-scale radiation-induced cavities at lower temperature and nucleation and growth of γ" precipitates at higher temperatures. The precipitate-hardened AM718-HT2 showed very small differences in strength before and after irradiation: the contribution to strength from γ" precipitates was replaced with dislocation loops. Because the radioactivity of the nickel superalloys from neutron activation limited the scope of the analysis, a feasibility study examined the possibility of an ultra-miniature specimen geometry, colloquially SS-Tiny (SS-T), for mechanical property determination using the nonirradiated Inconel 718. This study found an overestimation of ductility from the SS-T geometry with yield strength and ultimate tensile strength slightly above the SS-J2 geometry: this could be contributed to a reduction in specimen thickness.

36 MATERIALS SCIENCE↗

A Study of Influencing Factors on the Tensile Response of a Titanium Matrix Composite With Weak Interfacial Bonding

The generalized method of cells micromechanics model is utilized to analyze the tensile stress-strain response of a representative titanium matrix composite with weak interfacial bonding. The fiber/matrix interface is modeled through application of a displacement discontinuity between the fiber and matrix once a critical debonding stress has been exceeded. Unidirectional composites with loading parallel and perpendicular to the fibers are examined, as well as a cross-ply laminate. For each of the laminates studied, analytically obtained results are compared to experimental data. The application of residual stresses through a cool-down process was found to have a significant effect on the tensile response. For the unidirectional laminate with loading applied perpendicular to the fibers, fiber packing and fiber shape were shown to have a significant effect on the predicted tensile response. Furthermore, the interface was characterized through the use of semi-emperical parameters including an interfacial compliance and a "debond stress;" defined as the stress level across the interface which activates fiber/matrix debonding. The results in this paper demonstrate that if architectural factors are correctly accounted for and the interface is appropriately characterized, the macro-level composite behavior can be correctly predicted without modifying any of the fiber or matrix constituent properties.

Goldberg, Robert K.↗

Hoop Tensile Properties of Ceramic Matrix Composite Cylinders

Tensile stress-strain properties in the hoop direction were obtained for 100-mm diameter SiC/SiC ceramic matrix composite cylinders using ring specimens machined form the cylinder ends. The cylinders were fabricated from 2D balanced SiC fabric with several material variants, including wall thickness (6,8, and 12 plies), SiC fiber type (Sylramic, Sylramic-iBN, Hi-Nicalon, and Hi-Nicalon S), fiber sizing type, and matrix type (full CVI SiC, and partial CVI SiC plus slurry cast + melt-infiltrated SiC-Si). Fiber ply splices existed in all the hoops. Tensile hoop measurements are made at room temperature and 1200 C using hydrostatic ring test facilities. The failure mode of the hoops, determined through microstructural examination, is presented. The hoop properties are compared with in-plane data measured on flat panels using same material variants, but containing no splices.

Verrilli, Michael J.↗

Unraveling the Highly Plastic Behavior of ALD-Aluminum Oxide Encapsulations by Small-Scale Tensile Testing

We present a study directly measuring the electron-beam-induced plasticity of amorphous Al 2 O 3 coatings. Core–shell nanostructures are employed as small-scale model systems for two-dimensional coatings made by atomic layer deposition (ALD). Copper nanowires (NWs) are used as substrates for ALD deposition, representing a model system for interconnects commonly found in integrated circuits. Experiments are performed in situ in a transmission electron microscope (TEM) and further analyzed with electron energy loss spectroscopy (EELS). Our in situ TEM tensile experiments reveal the highly plastic behavior of the ALD shell, which withstands a maximum strain of 188%. Comparable samples under beam-off conditions show a brittle fracture, which underlines the effect of electron irradiation. The electron-beam-activated bond switching within the amorphous network enables compensation of the applied tensile strain, leading to viscous flow. By incorporating an intermediate nanocrystalline layer within the Al 2 O 3 shell, the plasticity is suppressed and brittle fracture occurs. This work directly demonstrates the tuning of mechanical properties in amorphous ALD structures through electron irradiation.

36 MATERIALS SCIENCE↗

Atomic faulting induced exceptional cryogenic strain hardening in gradient cell–structured alloy

Coarse-grained materials are widely accepted to display the highest strain hardening and the best tensile ductility. We experimentally report an attractive strain hardening rate throughout the deformation stage at 77 kelvin in a stable single-phase alloy with gradient dislocation cells that even surpasses its coarse-grained counterparts. Contrary to conventional understanding, the exceptional strain hardening arises from a distinctive dynamic structural refinement mechanism facilitated by the emission and motion of massive multiorientational tiny stacking faults (planar defects), which are fundamentally distinct from the traditional linear dislocation–mediated deformation. In conclusion, the dominance of atomic-scale planar deformation faulting in plastic deformation introduces a different approach for strengthening and hardening metallic materials, offering promising properties and potential applications.

Gradient dislocation structure↗

Optical fiber sensors for damage analysis in aerospace materials

Under this grant, fiber optic sensors were investigated for use in the nondestructive evaluation of aging aircraft. Specifically, optical fiber sensors for detection and location of impacts on a surface, and for detection of corrosion in metals were developed. The use of neural networks was investigated for determining impact location by processing the output of a network of fiberoptic strain sensors distributed on a surface. This approach employs triangulation to determine location by comparing the arrival times at several sensors, of the acoustic signal generated by the impact. For this study, a neural network simulator running on a personal computer was used to train a network using a back-propagation algorithm. Fiber optic extrinsic Fabry-Perot interferometer (EFPI) strain sensors are attached to or embedded in the surface, so that stress waves emanating from an impact can be detected. The ability of the network to determine impact location by time-or-arrival of acoustic signals was assessed by comparing network outputs with actual experimental results using impacts on a panel instrumented with optical fiber sensors. Using the neural network to process the sensor outputs, the impact location can be inferred to centimeter range accuracy directly from the arrival time data. In addition, the network can be trained to determine impact location, regardless of material anisotropy. Results demonstrate that a back-propagation network identifies impact location for an anisotropic graphite/bismaleimide plate with the same accuracy as that for an isotropic aluminum plate. Two different approaches were investigated for the development of fiber optic sensors for corrosion detection in metals, both utilizing optical fiber sensors with metal coatings. In the first approach, an extrinsic Fabry-Perot interferometric fiber optic strain sensor was placed under tensile stress, and while in the resulting strained position, a thick coating of metal was applied. Due to an increase in the quantity of material, the sensor does not return to its original position upon removal of the applied stress, and some residual strain is maintained within the sensor element. As the metal thickness decreases due to corrosion, this strain is released, providing the sensing mechanism for corrosion detection. In the second approach, photosensitive optical fibers with long period Bragg gratings in the core were coated with metal. The Bragg gratings serve to couple core modes at discrete wavelengths to cladding modes. Since cladding modes interact with the metal coating surrounding the fiber cladding, the specific wavelengths coupled from core to cladding depend on the refractive index of the metal coating. Therefore, as the metal corrodes, the resulting change in index of the coating may be measured by measuring the change in wavelength of the coupled mode. Results demonstrate that both approaches can be successfully used to track the loss in metal coating on the optical fiber sensors due to corrosion.

Schindler, Paul↗

Application of Powder Diffraction Methods to the Analysis of the Atomic Structure of Nanocrystals: The Concept of the Apparent Lattice Parameter (ALP)

The applicability of standard methods of elaboration of powder diffraction data for determination of the structure of nano-size crystallites is analysed. Based on our theoretical calculations of powder diffraction data we show, that the assumption of the infinite crystal lattice for nanocrystals smaller than 20 nm in size is not justified. Application of conventional tools developed for elaboration of powder diffraction data, like the Rietveld method, may lead to erroneous interpretation of the experimental results. An alternate evaluation of diffraction data of nanoparticles, based on the so-called 'apparent lattice parameter' (alp) is introduced. We assume a model of nanocrystal having a grain core with well-defined crystal structure, surrounded by a surface shell with the atomic structure similar to that of the core but being under a strain (compressive or tensile). The two structural components, the core and the shell, form essentially a composite crystal with interfering, inseparable diffraction properties. Because the structure of such a nanocrystal is not uniform, it defies the basic definitions of an unambiguous crystallographic phase. Consequently, a set of lattice parameters used for characterization of simple crystal phases is insufficient for a proper description of the complex structure of nanocrystals. We developed a method of evaluation of powder diffraction data of nanocrystals, which refers to a core-shell model and is based on the 'apparent lattice parameter' methodology. For a given diffraction pattem, the alp values are calculated for every individual Bragg reflection. For nanocrystals the alp values depend on the diffraction vector Q. By modeling different a0tomic structures of nanocrystals and calculating theoretically corresponding diffraction patterns using the Debye functions we showed, that alp-Q plots show characteristic shapes which can be used for evaluation of the atomic structure of the core-shell system. We show, that using a simple model of a nanocrystal with spherical shape and centro-symmetric strain at the surface shell we obtain theoretical alp-Q values which match very well the alp-Q plots determined experimentally for Sic, GaN, and diamond nanopowders. The theoretical models are defined by the lattice parameter of the grain core, thickness of the surface shell, and the magnitude and distribution of the strain field in the surface shell. According to our calculations, the part of the diffraction pattern measured at relatively low diffraction vectors Q (below 10/angstrom) provides information on the surface strain, whle determination of the lattice parameters in the grain core requires measurements at large Q-values (above 15 - 20/angstrom).

Palosz, B.↗

Processing and characterization of the homologous Zr x Ta 2 O 2x+5 series

In this study, Zr x Ta 2 O 2x+5 (ZTOx) was systematically studied to determine ideal solid-state synthesis and pressureless sintering conditions. For Zr 6 Ta 2 O 17 (ZTO6) and other compositions with values of x in ZTOx the optimal synthesis temperature of 1100 °C with 1 h dwell time was optimal. XRD phase analysis of the homologous series indicated that for ZTOx, x = 5, 6, 7, and 8 were within the phase stability field while x = 4 and x = 9 were outside the phase stability field. Unit cell lattice parameters changed anisotropically with Zr:Ta ratio with an overall <0.1% change in unit cell volume across the solid solution. Some Raman modes red shifted while others blue shifted, indicating competing tensile and compressive strains. Sintering of ZTOx required a progressively higher temperature as Zr-content increased despite the same starting powder grain sizes and synthesis temperature. Higher Vickers hardness for Zr-rich (12.7–12.8 GPa) than Ta-rich Zr x Ta 2 O 2x+5 (11.6–11.7 GPa) disappeared when accounting for different sintering temperatures. Indentation toughness was similar for all compositions (1.2–1.4 MPa m 1/2 ). Properties of Zr x Ta 2 O 2x+5 series indicate tunability of Zr:Ta composition ratio while maintaining the structure and room temperature mechanical properties comparable to Hf 6 Ta 2 O 17 and 8 mol% yttria stabilized zirconia ceramics.

36 MATERIALS SCIENCE↗

Bio-treatment of poplar via amino acid for interface control in biocomposites

Advanced biocomposites reinforced by abundant biomass-derived fillers can add a revenue stream to enhance the economic viability of biofuel production chains and the energy efficiency of the composite industry. However, the low stiffness of biopolymers limits their use in structural applications. Poplar fibers (mesh size: <180 μm, Populus spp.), an abundant waste from the wood industry, were used as bio-filler to fabricate high-performance biocomposites based on polylactic acid (PLA), in which the poplar fibers were modified by an amino acid (l-lysine). As a benefit of the amino acid treatment, the tensile Young's moduli of the lysine/poplar/PLA composites increased by up to 68% with the addition of a small amount of lysine, compared with neat PLA. At the same time, the tensile strength, failure strain, and Young's modulus of the poplar/PLA composites all increased after adding only 0.1 wt % of lysine. It has been observed that the lysine content has a significant effect on the decomposition temperature, complex viscosity, storage modulus, crystallization temperature, and crystallinity of composites. The fracture surfaces of the composites with an optimum lysine content had fewer voids and were more compact compared with composites without any lysine. The pores on the surfaces of poplar fibers became more available for the penetration of PLA molecules as a result of lysine addition. Finally, this study presents a facile method for reinforcing biocomposites with extremely low-cost and environmentally friendly biofillers.

59 BASIC BIOLOGICAL SCIENCES↗

Digital image correlation and infrared thermography data for seven unique geometries of 304L stainless steel

Material Testing 2.0 (MT2.0) is a paradigm that advocates for the use of rich, full-field data, such as from digital image correlation and infrared thermography, for material identification. By employing heterogeneous, multi-axial data in conjunction with sophisticated inverse calibration techniques such as finite element model updating and the virtual fields method, MT2.0 aims to reduce the number of specimens needed for material identification and to increase confidence in the calibration results. To support continued development, improvement, and validation of such inverse methods—specifically for rate-dependent, temperature-dependent, and anisotropic metal plasticity models—we provide here a thorough experimental data set for 304L stainless steel sheet metal. The data set includes full-field displacement, strain, and temperature data for seven unique specimen geometries tested at different strain rates and in different material orientations. Commensurate extensometer strain data from tensile dog bones is provided as well for comparison. We believe this complete data set will be a valuable contribution to the experimental and computational mechanics communities, supporting continued advances in material identification methods.

36 MATERIALS SCIENCE↗

First-principles study of hydrogen behavior near W/WC interfaces

Hydrogen (H) solution, migration, and binding to vacancies near the tungsten/tungsten carbide (W/WC) interfaces based on hcp WC or bcc W (W/WCb and Wb/WC) have been studied by first-principles simulations to provide insights into the effect of C on H behavior in W exposed to C deposition in fusion reactors. The H behavior near the W/WC interfaces is related to the tensile or compressive strain due to the lattice match and interfacial effects. Near the W/WCb interface, the H solution energy in hcp WC increases approaching the interface, while it decreases from the W side to the interface. The configuration change of the W slab significantly decreases the H solution energy but has only a modest effect on the H migration energy barrier in comparison with the values in bcc W. The interface enhances the H binding to vacancies in WC layers. Both the interface and configuration adjustment of the W slab reduce the H binding to vacancies on the W side of the interface. Near the Wb/WC interface, H solution energies in both WC and W slabs weakly decrease approaching the interface. The configuration change of the WC slab significantly increases the H solution energy and binding energy to vacancies but decreases the H migration energy barrier in comparison with the values in hcp WC. The H energetics near the W/WC interfaces indicate the likelihood of H localization and diffusion in the W side of the interface, rather than diffusing through the interface into WC layers.

Yang, L. (ORCID:0000000322166071)↗

Evaluation of 304L stainless steel deformation and failure under cyclic loading

The motivation for this work came from the simulation of components subjected to impact. In these problems, repeated loading can be generated by vibrational motion between internal parts of the component or by the occurrence of multiple impacts. Graphs of tensile equivalent plastic strain $(\overline{\varepsilon}_T^\rho)$ versus time from such cases had the character shown in Fig. 1. The equivalent plastic strain grew by alternating periods of accumulation and hold. The periods of hold indicate times when $d\overline{\varepsilon}_T^\rho$ did not accumulate. This can be due to the material unloading into the elastic range, or actually plastically reverse loading with hydrostatic stress σ h < 0 as was demonstrated for an impact simulation. Similar observations were made from the simulation of a 2-degree-of-freedom mass-elastic-plastic-spring system subjected to impact.

36 MATERIALS SCIENCE↗

Coal to Carbon Fiber (C2CF) Continuous Processing for High Value Composites (Final Report)

Coal tar is a condensed and recovered by-product of the coking of metallurgical coal for steel production. The heaviest fraction of distilled coal tar is an isotropic pitch largely used as a binder in the manufacturing of carbonaceous electrodes for primary aluminum smelting and in electric arc furnaces. Coal tar pitch offers high carbon yield upon carbonization. In this project, a process to convert the domestically sourced isotropic coal tar pitch, containing very low particulates (QI = 0.32 wt.%), to form flow-domain mesophase pitch amenable for melt spinning into precursor (green) fibers for carbon fiber, was developed and optimized. The final reproducible processing developed is reviewed in this report, along with several characterizations of the mesophase pitch. A final definition of the characteristics of a ‘spinnable’ mesophase pitch is presented. With this mesophase pitch, reproducible and stable multifilament melt spinning was developed, producing green fiber tows with filament diameters of approximately 20 m. The multifilament melt spinning was the most challenging aspect of the project and required the most effort. The best practices learned from this project for melt spinning are reviewed in this report. Once spun, the green fibers were oxidatively stabilized, carbonized and graphitized under inert gas atmosphere to form the final carbon fibers. Given the relatively high softening point of the mesophase pitch, no issues of interfilament fusion were observed during batch oxidation, and subsequent batch carbonization and graphitization went smoothly in all cases. An ~ 80 wt.% conversion of the green fiber mass to final carbon fiber was achieved. After graphitization, the carbon fibers showed high tensile moduli (most were ~ 600 GPa, or 87 Msi) consistent with commercially-available high-performance pitch-based carbon fiber. However, tensile strength and strain to failure were comparatively low. Further work to reduce defects in and on the fiber surfaces would increase these properties. SEM imaging of the graphitic fiber textures is presented herein. Rudimentary composites were fabricated from the carbon fibers and characterized showing similar modulus to baseline composites fabricated with commercial carbon fiber. Finally, a basic economic analysis was done showing the potential to increase the value of the isotropic coal tar pitch by up to 13.6 to 136 times based on a carbon fiber value of $\$$5/lb to $\$$50/lb, respectively. Moreover, the site case study suggests that the coal tar from the single integrated steel mill could supply production of up to 16 kt/yr of carbon fiber. Finally, a technological gap analysis was done which shed light on remaining technical challenges. These challenges included: recovery and utilization of condensates from the mesophase pitch processing, further advancing and increasing stability of the multifilament melt spinning processing, optimization of the oxidation processing, defect reduction for increased carbon fiber strength, and the development of a weaving process towards carbon fiber fabrics. To maximize the coal value chain, the primary objectives of this project were to (a) develop and scale efficient processing technology for producing melt-spinnable mesophase pitch from isotropic coal tar pitch, (b) clarify and simplify tedious continuous fiber processing technologies (particularly multifilament melt spinning of mesophase pitch) towards the efficient production of high performance carbon fiber, and (c) demonstrate and characterize representative composite parts derived from the final carbon fiber. Immense progress was made on all 3 objectives and is detailed in this report.

01 COAL, LIGNITE, AND PEAT↗

STRAIN CONCENTRATION AND DUCTILITY

Birefringent technique to observe plastic strain concentration during tensile tests of copper strip specimens containing arrays of discontinuities

STRESS CONCENTRATION↗