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DOE OSTI2021

Serrated Flow in Alloy Systems

This chapter presents the problem of the complexity of plastic flow in alloys, which is manifested by serrated deformation curves and transient plastic strain localizations. This phenomenon, which uncovers an inherently collective nature of the dynamics of crystal defects, is well known for conventional alloys. Surprisingly, despite the particular microstructure of HEAs, which strongly impacts the microscopic dynamics of defects, not only the HEAs are prone to the macroscopically jerky flow, but the serration patterns display many similar features, thus bearing evidence to similar laws for the collective dynamics. To provide a comprehensive approach to this problem, the chapter is subdivided into two parts. The first part presents the state-of-the art of this research under the angle of distinct regimes of collective dislocation dynamics found in conventional alloys, e.g., self-organized criticality, deterministic chaos, or synchronization. The second part summarizes recent investigations into serrated flows in HEAs, uncovering common and specific types of behaviors. Both parts conclude with the formulation of diverse open questions concerning these strongly coupled fields of research.

Lebyodkin, Mikhail↗

NASA NTRS1985

Permafrost and Subsurface Ice in the Solar System

The properties and behavior of planetary permafrost are discussed with reference to the ability of such surfaces to sustain loads characteristics of spacecraft landing and planetary bases. In most occurrences, water ice is in close proximity to, or in contact with, finely divided silicate mineral matter. When ice contacts silicate mineral surfaces, a liquid-like, transition zone is created. Its thickness ranges from several hundred Angstron units at temperatures near 0 degrees C to about three Angstrom units at -150 degrees C. When soluble substances are present, the resulting brine enlarges the interfacial zone. When clays are involved, although the interfacial zone may be small, its extent is large. The unfrozen, interfacial water may amount to 100% or more weight at a temperature of -5 degrees C. The presence of this interfacial unfrozen water acts to confer plasticity to permafrost, enabling it to exhibit creep at all imposed levels of stress. Nucleation processes and load-bearing capacity are examined.

Anderson, D. M.↗

NASA NTRS1988

A viscoplastic constitutive theory for metal matrix composites at high temperature

A viscoplastic constitutive theory is presented for representing the high temperature deformation behavior of metal matrix composites. The point of view taken is a continuum one where the composite is considered a material in its own right, with its own properties that can be determined for the composite as a whole. It is assumed that a single preferential (fiber) direction is identifiable at each material point (continuum element) admitting the idealization of local transverse isotropy. A key ingredient is the specification of an experimental program for the complete determination of the material functions and parameters for characterizing a particular metal matrix composite. The parameters relating to the strength of anisotropy can be determined through tension/torsion tests on longitudinally and circumferentially reinforced thin walled tubes. Fundamental aspects of the theory are explored through a geometric interpretation of some basic features analogous to those of the classical theory of plasticity.

Robinson, David N.↗

DOE OSTI2025

Effects of chemical composition and physicochemical properties of poplar biomass on the performance of 3D printed poplar-reinforced PLA materials

Lignocellulosic biomass has been well-acknowledged as a filler for making 3D printed composites. The technical performances of composites were influenced by the characteristics of the components. The correlations between poplar biomass properties and the mechanical and thermal performances of the 3D printed poplar-plastic composites were investigated. The characteristics of poplar were modified by different pretreatment methods, including using hot water, dilute acid, and organic solvent (organosolv), and each treated poplar biomass was applied as a filler in a polylactic acid (PLA) polymer matrix to produce eco-friendly materials. These solvent pretreatments increased the hydrophobicity and surface area of poplar. Organosolv treated poplar showed the highest cellulose content and significantly increased Young's modulus of its biocomposites. Principal component analysis revealed that the specific surface area and water contact angle of biomass contributed to the thermal stability of biocomposites. Additionally, the degree of polymerization of cellulose and xylan content within the biomass correlated with the biocomposites' break stress. Notably, the crystallinity of biocomposites impacted the modulus of these materials. The reported relationships between biomass characteristics and 3D printed composite behaviors provide guidance for optimizing biomass processing in biocomposite applications.

Ji, Anqi [State Univ. of New York (SUNY), Syracuse↗

DOE OSTI2024

New dynamic diamond anvil cell for time-resolved radial x-ray diffraction

The dynamic diamond anvil cell (dDAC) is a recently developed experimental platform that has shown promise for studying the behavior of materials at strain rates ranging from intermediate to quasi-static and shock compression regimes. Combining dDAC with time-resolved x-ray diffraction (XRD) in the radial geometry (i.e., with incident x-rays perpendicular to the axis of compression) enables the study of material properties such as strength, texture evolution, and deformation mechanisms. This work describes a radial XRD dDAC setup at beamline P02.2 (Extreme Conditions Beamline) at DESY’s PETRA III synchrotron. Time-resolved radial XRD data are collected for titanium, zirconium, and zircon samples, demonstrating the ability to study the strength and texture of materials at compression rates above 300 GPa/s. In addition, the simultaneous optical imaging of the DAC sample chamber is demonstrated. The ability to conduct simultaneous radial XRD and optical imaging provides the opportunity to characterize plastic strain and deviatoric strain rates in the DAC at intermediate rates, exploring the strength and deformation mechanisms of materials in this regime.

47 OTHER INSTRUMENTATION↗

DOE OSTI2024

New dynamic diamond anvil cell for time-resolved radial x-ray diffraction

47 OTHER INSTRUMENTATION↗

NASA NTRS2002

Deformation During Friction Stir Welding

Friction Stir Welding (FSW) is a solid state welding process that exhibits characteristics similar to traditional metal cutting processes. The plastic deformation that occurs during friction stir welding is due to the superposition of three flow fields: a primary rotation of a radially symmetric solid plug of metal surrounding the pin tool, a secondary uniform translation, and a tertiary ring vortex flow (smoke rings) surrounding the tool. If the metal sticks to the tool, the plug surface extends down into the metal from the outer edge of the tool shoulder, decreases in diameter like a funnel, and closes up beneath the pin. Since its invention, ten years have gone by and still very little is known about the physics of the friction stir welding process. In this experiment, an H13 steel weld tool (shoulder diameter, 0.797 in; pin diameter, 0.312 in; and pin length, 0.2506 in) was used to weld three 0.255 in thick plates. The deformation behavior during friction stir welding was investigated by metallographically preparing a plan view sections of the weldment and taking Vickers hardness test in the key-hole region.

Henry J. White↗

NASA NTRS2004

Tensile Creep Fracture of Polycrystalline Near-Stoichiometric NiAl

Tensile creep fracture behavior of polycrystalline near-stoichiometric NiAl has been studied between 700 and 1200 K under initial applied stresses varying between 10 and 200 MPa. The stress exponent for fracture varied between 5.0 and 10.7 while the activation energy for fracture was 250 +/- 22 kJ/mol. The fracture life was inversely proportional to the secondary creep rate in accordance with the Monkman-Grant relation although there was extensive scatter in the data. This observation suggests that the fracture life for near-stoichiometric NiAl was influenced by creep under these stress and temperature conditions. Several different fracture morphologies were observed. Transgranular ductile cleavage fracture occurs at 700 K and at the higher stresses at 800 K. The fracture mode transitions to transgranular creep fracture at 900 and 1000 K and at lower stresses at 800 K, while plastic rupture and grain boundary cavitation occur at 1100 and 1200 K. An experimental fracture mechanism map is constructed for near-stoichiometric NiAl.

Raj, Sai V.↗

DOE OSTI2026

Counterintuitive Compatibilization of Poly(-Valerolactone) and Poly(L-Lactic Acid) by Statistical Copolymers toward Compostable and Recyclable Packaging

Poly(δ-valerolactone) (PVL) and poly(l-lactic acid) (PLLA) are bioderivable, compostable, and chemically recyclable plastics with synergistic properties for addressing plastic waste accumulation in receiving environments. Though recyclable-by-design polymers often fall short of competing with incumbent materials, blending affords a means to leverage individual component strengths toward ideal tunable properties. Polymer blends are often immiscible, but a range of methodologies are available to promote mixing. Here, we report on the compatibilization of 9 immiscible PVL and PLLA blends with three different compatibilization agents: thermoplastic starch, synthesized PVL-co-PLLA statistical copolymers (SCPs), and synthesized PVL-b-PLLA block-type copolymers. Resulting degrees of compatibilization are observed through scanning electron microscopy, corroborated by thermal and mechanical analyses monitoring performance as a function of microdomain size. Small-angle and wide-angle X-ray scattering experiments are conducted to observe the influence of compatibilizers on individual crystalline phases to further elucidate material behavior. Molecular dynamics simulations provide key insights into the interfacial interactions between homopolymers and compatibilizers. Finally, a suite of end-of-life avenues is established by biodegradation in industrial composting conditions, chemical recycling by deconstruction to hydroxymethyl esters, and direct chemical depolymerization to lactone precursors in mixed feed. Overall, we highlight several promising blends and the counterintuitive SCP compatibilization phenomenon toward high-performance, sustainable materials.

Compatibilization, copolymer compatibilizer, bio-b↗

DOE OSTI2024

In-Situ and Ex-Situ Studies on the Morphology Changes of Polymer Pipeline Materials for Use in Hydrogen Gas Environments

The US natural gas infrastructure is a national asset that could be used to deliver hydrogen and hydrogen blends of natural gas as a pathway to reduce carbon emissions. The distribution system comprises nearly 50% plastic pipe composed of medium- and high-density polyethylene materials (MDPE and HDPE). While these materials perform adequately for natural gas, research on their hydrogen compatibility is essential to understand if any immediate and long-term risks are associated with hydrogen addition. The Blended Gas CRADA, a HyBlend project, has established a comprehensive test method for evaluating MDPE and HDPE of various plastic resin compositions of pipeline material in pure hydrogen and 20% hydrogen/80% methane blends. Both in-situ and ex-situ measurements were performed to capture hydrogen-induced changes in the polyethylene material's crystalline, amorphous and their interphase regions. We investigated MDPE and HDPE pipeline materials made from different polymer resin systems to evaluate the effects of hydrogen gas. The materials were characterized by their density, diffusion coefficient, free volume ratio, and degree of crystallinity. Various advanced characterization methods, including in situ NMR, ex situ XRD, ex situ DSC, and ex situ TDA, were used to analyze the effects of changes in crystalline, amorphous, and interphase regions due to gas exposure. Time-dependent post-decompression quasi-static tensile tests were conducted to explore the effects of gas exposure time on the mechanical behavior of the pipe materials. This work will highlight the time sensitivities during and after gas exposure. The correlation between gas-induced polyethylene morphology changes and the associated material performance will be addressed for the intended applications. These studies will show that polyethylene resin composition and material exposure are important factors when considering whether hydrogen gas affects pipeline materials positively or negatively.

Simmons, Kevin L.↗

NASA NTRS1985

Influence of the resin on interlaminar mixed-mode fracture

Both literature review data and new data on toughness behavior of seven matrix and adhesive systems in four types of tests were studied in order to assess the influence of the resin on interlaminar fracture. Mixed mode (i.e., various combinations of opening mode 1, G sub 1, and shearing mode 2; G sub 2) fracture toughness data showed that the mixed mode relationship for failure appears to be linear in terms of G sub 1 and G sub 2. The study further indicates that fracture of brittle resins is controlled by the G sub 1 component, and that fracture of many tough resins is controlled by total strain-energy release rate, G sub T. Regarding the relation of polymer structure and the mixed mode fracture: high mode 1 toughness requires resin dilatation; dilatation is low in unmodified epoxies at room temperature/dry conditions; dilatation is higher in plasticized epoxies, heated epoxies, and in modified epoxies; modification improves mode 2 toughness only slightly compared with mode 1 improvements. Analytical aspects of the cracked lap shear test specimen were explored.

Johnson, W. S.↗

NASA NTRS1987

Influence of the resin on interlaminar mixed-mode fracture

Johnson, W. S.↗

DOE OSTI2022

Mechanics of the Ring Tension Test (RTT): A Finite Element-based Investigation

The ring tension test (RTT) is an experimental method for determining mechanical behavior in a material’s circumferential or hoop direction. It is a crucial test for testing anisotropic materials with tube geometry, such as nuclear fuel cladding or irradiated pipes. Several RTT configurations exist, each with their own advantages and disadvantages. However, this test is significantly more complex than traditional tensile testing and can be especially sensitive to small differences and inconsistencies in the test setup and geometry, ultimately affecting the derived mechanical properties. Previous research has focused on method development, and little work has been done on understanding the subtle differences between an ideal test and experiments, specifically when the tests are performed on highly irradiated materials in hot cells. In this work, a finite element-based investigation of the RTT is conducted. Two promising test configurations are investigated, comparing their ability to determine accurate material strengths through plastic deformation. Several non-ideal conditions and uncontrollable effects which are likely to occur during experimental testing such as machining tolerances, variations of specimen geometry from nominal dimensions, rotation of specimens and fixturing, and other test setup discrepancies are studied. The sensitivity of measured strengths to these conditions is presented. A mechanics-based approach to describing and correcting raw data to determine actual strengths is also included for one of the configurations, resulting in a robust correction method with highly accurate material strength measurements. Based on these analyses, the hemicylindrical mandrel configuration is recommended with a gauge region oriented at a 45° angle.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

NASA NTRS1986

A viscoplastic constitutive theory for metal matrix composites at high temperature

A viscoplastic constitutive theory is presented for representing the high-temperature deformation behavior of metal matrix composites. The point of view taken is a continuum one where the composite is considered a material in its own right, with its own properties that can be determined for the composite as a whole. It is assumed that a single preferential (fiber) direction is identifiable at each material point (continuum element) admitting the idealization of local transverse isotropy. A key ingredient in this work is the specification of an experimental program for the complete determination of the material functions and parameters for characterizing a particular metal matrix composite. The parameters relating to the strength of anisotropy can be determined through tension/torsion tests on longitudinally and circumferentially reinforced thin-walled tubes. Fundamental aspects of the theory are explored through a geometric interpretation of some basic features analogous to those of the classical theory of plasticity.

Robinson, D. N.↗

NASA NTRS1987

A viscoplastic constitutive theory for metal matrix composites at high temperature

A viscoplastic theory is presented for representing the high-temperature deformation behavior of metal matrix composites. The point of view taken is a continuum one where the composite is considered a material in its own right, with its own properties that can be determined for the composite as a whole. It is presumed that a single preferential (fiber) direction is identifiable at each material point (continuum element) admitting the idealization of local transverse isotropy. A key ingredient in this work is the specification of an experimental program for the complete determination of the material functions and parameters for characterizing a particular metal matrix composite. The parameters relating to the strength of anisotropy can be determined through tension/torsion tests on longitudinally and circumferentially reinforced thin-walled tubes. Fundamental aspects of the theory are explored through a geometric interpretation of some basic features analogous to those of the classical theory of plasticity.

Robinson, D. N.↗

DOE OSTI2021

Influence of polycarboxylate superplasticizer, citric acid and their combination on the hydration and workability of calcium sulfoaluminate cement

Highlights: • The dispersion efficiency of polycarboxylate superplasticizers drops quickly over time. • Citric acid maintains the dispersion efficiency of PCE over time. • Competitive adsorption between citric acid and PCE occurs. • The combination of citric acid with PCE decreases the initial dispersion efficiency of PCE. PCEs are well known to improve the initial fluidity of CSA. However, their dispersion efficiency drops quickly over time. This issue can be solved by incorporating retarders. In this context, this paper deals with the influence of citric acid, used as a retarder, PCE and their combination on the hydration and workability of CSA. Isothermal calorimetry, XRD and TG analysis were used to describe the hydration process, while workability was characterized with the mini-cone test. Adsorption behavior was investigated using total organic carbon analyzer coupled with ion chromatography. Results show that the introduction of citric acid retained the dispersion efficiency of PCE over time. However, the initial dispersion efficiency of PCE was decreased by citric acid as the latter tend to adsorb first on the surface of cement grains, inhibiting the adsorption of PCE. A dispersion model was proposed to describe the acting mechanism of these admixtures on CSA.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Tuning the spin dynamics and magnetic phase transitions of the Cantor alloy via composition and sample processing protocols: A muon spin relaxation study

CrMnFeCoNi, also called the Cantor alloy, is a well-known high-entropy alloy whose magnetic properties have recently become a focus of attention. Here, we present a detailed muon spin relaxation study of the influence of chemical composition and sample processing protocols on the magnetic phase transitions and spin dynamics of several different Cantor alloy samples. Specific samples studied include a pristine equiatomic sample, samples with deficient and excess Mn content, and equiatomic samples magnetized in a field of 9 T or plastically deformed in pressures up to 0.5 GPa. The results confirm the sensitive dependence of the transition temperature on composition and demonstrate that post-synthesis pressure treatments cause the transition to become significantly less homogeneous throughout the sample volume. In addition, we observe critical spin dynamics in the vicinity of the transition in all samples, reminiscent of canonical spin glasses and magnetic materials with ideal continuous phase transitions. Application of an external magnetic field suppresses the critical dynamics in the Mn-deficient sample, while the equiatomic and Mn-rich samples show more robust critical dynamics. The spin-flip thermal activation energy in the paramagnetic phase increases with Mn content, ranging from 3.1⁢(3) × 10 -21 J for 0% Mn to 1.2⁢(2) × 10 -20 J for 30% Mn content. These results shed light on critical magnetic behavior in environments of extreme chemical disorder and demonstrate the tunability of spin dynamics in the Cantor alloy via chemical composition and sample processing.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Upcycling of Polystyrene Waste to Poly(ionic liquid) Materials

The C–H functionalization of commodity polymers could be a promising approach for upcycling plastic waste into advanced materials, which can alter the properties of the original materials through the introduction of different functionalities onto the existing backbone structures. In this study, waste polystyrene (PS) was modified by Friedel–Crafts acylation using 4-chlorobutyryl chloride (4-CBC) followed by reaction with N-alkylimidazoles to form cationic polyelectrolytes. These methods provide access to what are essentially poly(ionic liquid) (poly(IL)) materials with properties that are distinctly different from those of the PS from which they were formed. In one notable example, the glass transition temperature (T g ) of imidazolium-functionalized PS was ∼16 °C, which is a nearly 90 °C reduction from PS. This is also evidenced by macroscopic mechanical properties where the poly(IL) product is highly elastic in stark contrast to brittle PS. Moreover, the resulting ionomers showed self-healing behaviors in the presence of a “free” IL further contributing to the utility of the materials. Here, the methods in this work can open opportunities to utilize waste PS to obtain a vast array of poly(IL) materials with highly tailored structures and properties.

36 MATERIALS SCIENCE↗