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At least 811 records · Page 45

Intact archeological human bones and age at death studied with transmission x–ray diffraction and small angle x–ray scattering

In this work, high-energy, wide-angle x-ray scattering (WAXS, x-ray diffraction) and small-angle x-ray scattering (SAXS) were used to study intact human second metacarpal bones (mc2) from two UK archeological sites. A novel method correcting for irregular mass distribution was applied in these transmission geometry experiments done at beamline 1-ID of the Advanced Photon Source. The authors asked whether there were age-at-death-related changes in carbonated apatite (cAp) lattice parameters and whether SAXS could detect collagen D-period peaks in the archeological mc2. For each of the two sites, Ancaster and Wharram Percy in England, six female mc2s were studied; for each site, two were from each of three age-at-death cohorts (young, 18-29 years; middle, 30-49 years; old >= 50 years) along with a modern control mc2. The Rietveld method was applied to the WAXS patterns to provide precise lattice parameter values. The cAp lattice parameters did not correlate with age-at-death estimated from dental wear. From WAXS and the 00.2 diffraction peak widths, four archeological mc2s possessed coherently scattering domain lengths (crystallite c-axis sizes) that matched that of the modern mc2; SAXS revealed the same four archeological mc2 had D-period peak intensities equivalent to that of the modern mc2. The other eight archeological mc2s had significantly larger crystallite sizes (than the modern mc2) and weak or absent D-period peaks, differences attributed to diagenetic changes. Based on these data, the authors suggest that WAXS 00.2 peak width and SAXS D-period peak intensity can be used with intact bones to select those likely to retain largely unaltered tissue nanostructure, which might be required for other analyses. Taken as a whole, the results suggest detecting age-related deterioration in nanostructural features may be difficult in bone showing significant bioerosion.

59 BASIC BIOLOGICAL SCIENCES↗

Impact of hygrothermal aging on structure/function relationship of perfluorosulfonic-acid membrane

Perfluorosulfonic-acid (PFSA) membranes are widely used as the solid electrolyte in electrochemical devices where their main functionalities are ion (proton) conduction and gas separation in a thermomechanically stable matrix. Due to prolonged operational requirements in these devices, PFSA membranes’ properties change with time due to hygrothermal aging. This paper studies the evolution of PFSA structure/property relationship changes during hygrothermal aging, including chemical changes leading to changes in ion-exchange capacity (IEC), nanostructure, water-uptake behavior, conductivity, and mechanical properties. Our findings demonstrate that with hygrothermal aging, the storage modulus increases, while IEC and water content decrease, consistent with the changes in nanostructure, that is, water- and crystalline-domain spacings inferred from small- and wide-angle X-ray scattering (SAXS/WAXS) experiments. In addition, the impact of aging is found to depend on the membrane's thermal prehistory and post-treatments, although universal correlations exist between nanostructural changes and water uptake. Lastly, the findings have impact on understanding lifetime, durability, and use of these and related polymers in various technologies.

30 DIRECT ENERGY CONVERSION↗

Effect of Hydrothermal Aging on Injection Molded Short Jute Fiber Reinforced Poly(Lactic Acid) (PLA) Composites

This work focused on the durability of short jute fiber reinforced poly(lactic acid) (PLA) composites in distilled water at different temperatures (23, 37.8 and 60 °C). Morphological, thermal and mechanical properties (tensile, flexural, and impact) of jute/PLA composites were investigated before and after aging. Different from traditional synthetic fiber reinforced polymer composites, the stability of jute/PLA composites in water was significantly influenced by hydrothermal temperature. The mechanical properties of the composites and molecular weight of PLA matrix declined quickly at 60 °C, however, this process was quite slower at temperatures of 23 and 37.8 °C. Impact properties of the composites were hardly decreased, but the tensile and flexural properties suffered a drop though to various degrees with three degradation stages at 23 and 37.8 °C. The poor interface of composites and the degradation of PLA matrix were the main damage mechanism induced by hydrothermal aging. Furthermore, considering the hydrolysis of PLA matrix, the cleavage of PLA molecular chain in different aging time was quantitatively investigated for the first time to illustrate hydrolysis degree of PLA matrix at different aging time.

36 MATERIALS SCIENCE↗

The Effect of Melt Ultrasound Treatment on the Microstructure and Age Hardenability of Al-4 Wt Pct Cu/TiC Composite

In the present work, Al-4 wt pct Cu/TiC composite was synthesized by the molten salt route that contains submicron-sized TiC particles in the Al-4 wt pct Cu matrix. The concentration of the TiC particle in the base alloy is 7.5 wt pct. Melt ultrasound treatment was done by remelting the as-cast composite at 1023 K (750 °C) in a view to refine the size of TiC particles to nanoscale and distribute them evenly in the matrix. The microstructure and age hardenability of the untreated and ultrasound-treated composites were investigated. The TiC particles accelerate the precipitation kinetics of CuAl{sub 2} phase in Al-4 wt pct Cu alloy. In the present study, the hardness obtained for untreated Al-4 wt pct Cu/TiC composite is 120 VHN within 5 hours of peak aging time, which is higher than the hardness of the monolithic Al-4 wt pct Cu, which is 104 VHN at 35 hours of peak aging time. Melt ultrasound treatment of Al-4 wt pct Cu/TiC composite shows no significant effect on the distribution and refinement of TiC particles in the matrix. However, it partially disintegrates the TiC into Al{sub 3}Ti and Al{sub 4}C{sub 3} particles. The ultrasound-treated composite showed an improved hardness of about 132 VHN at 5 hours of peak aging, in comparison to that of the untreated composite, by forming denser and homogeneous CuAl{sub 2} precipitates.

36 MATERIALS SCIENCE↗

Electron Beam Welding of Nimonic 80A Superalloy: Microstructure Evolution and EBSD Study After Aging Heat Treatment

The purpose of this research was to evaluate integrity and microstructure changes of the electron beam-welded Nimonic 80A and the base metal after aging heat treatment process, i.e., 700 °C/72 h/air cooling. Here, microstructure, microhardness and tensile were investigated by various tools, i.e., scanning electron microscope with energy-dispersive spectroscopy and electron backscatter diffraction, x-ray diffraction analysis and Vickers hardness. Evaluation of microstructure shows that the weld zone mainly consists of columnar dendrites. The effect of aging heat treatment on the microstructure morphology and phase structure is very limited. Also, it was observed that there are obvious segregation and precipitates in intracrystalline and along the grain boundaries after aging heat treatment. Electron backscatter diffraction results show that the weld zone and base metal have a clear difference in the grain boundary characterization and kernel average misorientation at room temperature and after aging heat treatment, which leads to a difference in microhardness of the weld zone. In addition, the relationship between microhardness and tensile strength is discussed.

36 MATERIALS SCIENCE↗

Mechanical Properties and Corrosion Behavior of Spray-Formed 7075 Alloy with One-Stage Aging

The mechanical properties, corrosion resistance and microstructure of the spray-formed 7075 alloy after one-stage aging treatments were studied by using a tensile tester, hardness tester, slow strain rate test, electrical test, intergranular corrosion test, electrochemical corrosion test, scanning electron microscope and transmission electron microscope. The results show that the strength and hardness of the alloy have double peaks with the one-stage aging treatments. With aging at 120 °C for 24 h (first peak), abundant tiny η′ phases and η phases precipitate in the matrix. The tensile strength of the alloy increases to 760 MPa, and the elongation is 4.8%. After aging at 120 °C for 132 h (second peak), blocky η phases appear. The tensile strength and elongation of the alloy are 757 MPa and 5.9%, respectively. The grain boundary precipitates dissociate, and the precipitate-free zones are widened. The corrosion resistance of the alloy increases.

36 MATERIALS SCIENCE↗

An Investigation on Microstructure Evolution, Mechanical Properties, and Strain Aging of Mg-1.8Zn-0.7Si-0.4Ca Biomedical Alloy Processed by Equal Channel Angular Pressing

The influence of equal channel angular pressing (ECAP) on microstructure and mechanical behavior, as well as, strain aging during ECAP and post-ECAP of Mg-1.8Zn-0.7Si-0.4Ca biomedical alloy was examined. The alloy in solid solution heat-treated condition was processed by ECAP with route B{sub C} at 350 and 400 °C. The specimens ECAPed at 350 °C were aged at 125 and 150 °C for different times. The hardness and shear punch test results indicated that performing ECAP at 350 °C for 4 passes increases the hardness and shear strength of the alloy from 48 HV and 110 MPa to 71 HV and 188 MPa, respectively. It was revealed that the average grain size of the alloy decreases from 78 µm to about 3 µm after 4 passes of ECAP. Three precipitates of CaMgSi, Ca{sub 2}Mg{sub 6}Zn{sub 3}, and Mg{sub 2}Si were detected in the solid solution specimen. After 4 passes of ECAP at 350 °C, Ca{sub 2}Mg{sub 6}Zn{sub 3} was completely dissolved and the morphology of Mg{sub 2}Si changed from Chinese script to fiber-shaped particles. Dynamic strain aging occurred at high-temperature ECAP, and the specimens were overaged during post-ECAP aging. Small MgZn particles were detected in the overaged sample.

36 MATERIALS SCIENCE↗

Universal aging characteristics of macroscopically and microscopically dissimilar metallic glasses

Supercooled liquids and glasses, due to their intrinsically unstable nature, are known to relax continuously until an equilibrium state is reached. By exploring atomic relaxation, aging and microscopic structure of chemically similar but physically dissimilar metallic glasses, we find that neither the relaxation time nor aging correlate with the free volume or density of the glasses. Furthermore, atomic relaxation time in these metallic glasses does not depend on the microscopic structure of the systems. The activation energy for the diffusion process indicates a completely different microscopic mechanism governing the atomic transport process. Nevertheless, the age-dependent relaxation time surprisingly exhibits a universal time-waiting time-temperature superposition. In conclusion, our results provide a convincing proof of the universality in the aging of out-of-equilibrium materials.

36 MATERIALS SCIENCE↗

Soil fertility management for sustainable Miscanthus × giganteus production: Increased tiller weight from nitrogen management explains yield gains in aged miscanthus

Aging-related yield decline in Miscanthus × giganteus (miscanthus) remains a major constraint to sustainable biomass production. This study evaluated how nitrogen (N) management and soil fertility influence yield-component traits and productivity in aging miscanthus. Trials were conducted at two sites established in 2008 at the University of Illinois Energy Farm, Urbana, IL. (i) The Sun Grant trial received 0, 60, and 120 kg N ha −1 annually until 2015. Starting 2021, half of each plot received 60 or 120 kg N ha −1 , resulting in six legacy-contemporary treatments: 0N–0N, 0N–120N, 60N–0N, 60N–60N, 120N–0N, 120N–120N. (ii) The Energy Farm trial remained unfertilized until 2014, when one half of each plot received 56 kg N ha −1 , forming two treatments: 0N–0N, 0N–56N. Sun Grant trial results showed N fertilization increased tiller density (tillers m −2 ) and tiller weight (g tiller −1 ) in juvenile to early-mature miscanthus (2011–2015). After N withdrawal, both traits declined (20 % and 40 %), though legacy effects persisted in tiller weight in the aging stands (2020–2023). Contemporary N had little effect on tiller density but increased tiller weight by 34 %–77 %, resulting in 23 %–106 % higher machine-harvested biomass yield in 0–120N, 60-60N, and 120-120N plots. At the Energy Farm trial, 0N–56N plots yielded 59 %–108 % more biomass than 0N–0N. Soil total N increased (Sun Grant: 47 % by 2020; Energy Farm: 58 % by 2023), while Mehlich-3 P (42 %–44 %) and K (21 %–46 %) declined. These findings identify tiller weight as a key determinant of biomass yield in aging miscanthus and highlight the need for P and K management for long-term productivity.

09 BIOMASS FUELS↗

Quantifying the effects of artificial aging on the ignition and self-propagating reactions of Ni(V)/Al multilayers

Bimetallic, reactive multilayers are uniformly structured materials composed of alternating nanoscale layers that may be ignited to produce self-propagating intermetallic-formation reactions. When reactive multilayers age, there is a change in local composition and loss of stored chemical energy due to mass transport and rearrangement at the interfaces. Here, to quantify the long-term reliability of commercial Ni(V)/Al multilayers, the effects of accelerated aging on both ignition sensitivity and self-propagating reactions have been examined. Thermally aged samples were characterized using transmission electron microscopy, differential scanning calorimetry, and laser ignition combined with high-speed videography. The analytically quantifiable nature of both continuous wave laser ignition and reactive wave propagation enabled calculations of Arrhenius rate constants for as-received and various heat-treated multilayers. With heat treatment, there is a change in the intermixed thickness and interfacial chemistry that decreases the activation energy for point ignition but increases it for self-propagating reactions. This finding implies that with increased thermal aging, the reaction becomes easier to facilitate in the solid state but harder in the liquid phase.

Energetic material↗

Asynchronous aging and turnover of human circulating and tissue-resident memory T cells across sites

Memory T cells are maintained in tissues as circulating effector-memory (T EM ) and tissue-resident (T RM ) populations for protective immunity, though the role of site and subset in memory persistence remains undefined. Here, in this work, we investigated age-associated dynamics of human T cells in lymphoid organs, mucosal sites, and blood over 10 decades of life using retrospective radiocarbon ( 14 C) birth dating, along with cellular, transcriptome, and epigenetic profiling. Memory T cells across peripheral sites exhibited continuous turnover with mean lifespans of 1–2 years, while the spleen contained longer-lived T cells. Over age, T EM cells expressed senescent markers and a GZMK transcriptional signature, while T RM cells maintained site-specific resident phenotypes without exhibiting features of senescence. Both T EM and T RM cells showed age-associated DNA hypomethylation, though T RM cells exhibited more epigenetically regulated genes. Together, our findings reveal asynchronous aging of human memory T cells by subset and site, as well as persistence of T RM cells without immunosenescence.

T cells↗

Two-scale model for the effect of physical aging in elastomers filled with hard nanoparticles

A two-scale model is developed, and solved numerically, to describe the mechanical behavior of elastomers filled with hard nanoparticles. Of particular interest is the slow recovery of the elastic modulus after large-amplitude oscillatory deformation. To account for this effect, the physical aging of the glassy bridges between the filler particles is captured with two thermal degrees of freedom for the matrix material, namely a kinetic and a configurational one. Formulating the two-scale model enriched with aging in a nonequilibrium thermodynamics context, first results in a constitutive relation for the Cauchy stress tensor. Second, the dynamics of physical aging is described, which eventually results in the slow recovery of the elastic modulus with waiting time. The proposed model is investigated numerically under large amplitude oscillatory shear deformation. Of particular interest in this respect is the coupling of the micro-scale dynamics with the physical aging on the macroscopic scale. This coupling is examined in detail, both in an approximate way using a Gaussian approximation, as well as numerically, under specific conditions. It turns out that the CONNFFESSIT approach (Laso and Öttinger 1993 ) can not be employed for the numerical solution of the model under arbitrary loading conditions because of the novel structure of the two-level coupling term. While a procedure for solving the model numerically for the case of strong applied deformation is presented in this paper, other solution methodologies need to be sought for the cases of weak and no applied deformation.

36 MATERIALS SCIENCE↗

Evolution of the role of molybdenum in duplex stainless steels during thermal aging: From enhancing spinodal decomposition to forming heterogeneous precipitates

Thermal aging of ferrite in duplex stainless steels leads to a complex microstructural evolution that can give way to large deleterious changes in mechanical properties. The microstructural evolution mechanisms that happen concurrently are strongly linked to minor changes in composition. By characterizing duplex stainless steels with various compositions over a range of aging conditions, it was revealed that adding a modest amount of Mo to cast austenitic stainless steel (such as changing from grade CF3 to grade CF3M) not only increases the kinetics of spinodal decomposition and Ni-Si-Mn-rich G-phase precipitation, but it also forms a separate Mo-rich phase. At shorter equivalent aging times, Mo segregates from Fe and towards Cr accelerating spinodal decomposition. At longer aging times, Mo enriches in the Ni-Si-Mn clusters before phase separating into an adjoined Mo-rich cluster. We found that these phase changes and precipitation events result in a rather steep drop in fracture and impact toughness. These results will inform the design of similar alloys for use at high temperatures.

36 MATERIALS SCIENCE↗

Pouch cells with 15% silicon calendar-aged for 4 years

Small amounts of high-capacity silicon-based materials are already used in the anode of commercial Li-ion batteries, helping increase their energy density. Despite their remarkable storage capability, silicon continu-ously reacts with the electrolyte, accelerating time-dependent cell performance fade. Nevertheless, very limited information is available on the specific consequences of this reactivity for the calendar aging of Li-ion cells. Here, we analyze aging effects on 450 mAh pouch cells containing 15 wt% of Si (and 73 wt% graphite) after storage at 21 °C for four years. We show that severe losses of Si capacity occurred due to particle isolation when cells were stored at high states of charge (SOC), but not when cells were fully discharged prior to storage. Impedance rise was also significantly higher when cells were kept at high SOCs and was mostly due to phenomena taking place at the cathode; the continuous electrolyte reduction at the anode did not lead to a major increase in bulk electrode resistance. A series of post-test characterization provided additional information on the effects of time and SOC on the calendar aging of Si-containing cells. In conclusion, our study highlights the many challenges posed by Si during calendar aging and can inform future studies in the field.

25 ENERGY STORAGE↗

Precipitation behavior of α phase during aging treatment in a β-quenched Ti-7333

Highlights: • The precipitation behaviors of α precipitate are investigated in the hot-rolled Ti-7333. • The formation of the V-shaped α configuration is closely related to the variant selection of α phase. • The angle between the closely packed direction of α{sub GB} and GB plane plays a key role on the precipitation of α{sub GB}. - Abstract: In this work, the precipitation behavior of α phase during the isothermal aging treatment was investigated in the β-quenched Ti-7333. The results indicate that dislocations contribute to the precipitation of α phase with a dot-like morphology at the beginning of aging treatment, and these dot-like α precipitates holding the same Burgers orientation relationship (BOR) with respect to the β matrix coalesce into the platelet morphology. The platelet-like α precipitates that orientate to different growth directions combine with each other to form the V-shaped configuration. And the formation of this configuration is closely related with the variant selection (VS) of α phase, which is resulted from the perfect accommodation of transformation strain within the β matrix. Meanwhile, it is found that low-angle grain boundaries (LAGBs) and high-angle grain boundaries (HAGBs) can be decorated by α phase during the aging treatment, and its precipitation degree significantly depends on the angle between the closely packed direction of αGB and the GB plane. The volume fraction of α phase increases with increasing aging time, and this increasing volume fraction eventually results in the increase in micro-hardness of the alloy.

36 MATERIALS SCIENCE↗

Intergranular corrosion resistance of Zn modified 5××× series Al alloy during retrogression and re-aging treatment

Highlights: • Increase the strength due to precipitation hardening of T-Mg{sub 32}(AlZn){sub 49} phase in the Zn modified Al-Mg alloy. • Both high corrosion resistance and high strength are achieved by retrogression and re-aging treatment in Al-5Mg-3Zn alloy. • Large Mg and Zn content difference between GBP and PFZ results in relatively high IGC susceptibility. • The intergranular corrosion mechanism of Zn modified Al-Mg alloy during retrogression and re-aging treatment is clarified. - Abstract: The effects of retrogression and re-aging treatment on the intergranular corrosion behavior of Al-5.0Mg-3.0Zn alloys are systematically studied. The alloy's strength increases when retrogression temperature increases from 390 °C to 420 °C. Samples retrogressed at 390 °C then re-aged are very susceptible to intergranular corrosion and those retrogressed at 405 °C and 420 °C express good corrosion resistance. Then the alloy's corrosion susceptibility rises with increasing retrogression temperature. Grain boundary precipitates are coarsened and distributed discontinuously with decreasing retrogression temperature. Higher retrogression temperature results in higher Mg and Zn content difference and intergranular corrosion susceptibility.

36 MATERIALS SCIENCE↗

Effect of isothermal and non-isothermal aging on the low cycle fatigue behavior of an Al–Cu–Mg–Si forging alloy

Highlights: • Non-isothermal aging treatment is performed to improve low cycle fatigue performance of an Al-Cu-Mg-Si forging alloy. • Mixed precipitation characteristic manifested as shearable and non-shearable θ' phases is obtained by non-isothermal aging. • Planar slip associated with particle shearing mechanism contributes to the high fatigue crack propagation resistance. - Abstract: Low cycle fatigue (LCF) behavior of an Al–Cu–Mg–Si forging alloy was investigated at room temperature. Isothermal aging (T6) and non-isothermal aging (NIA) treatments were applied to produce different microstructures. Under the same strain amplitude, the LCF life of NIA specimen exceeded that of T6 specimen. Besides, NIA specimens exhibited cyclic stability behavior in contrast to cyclic hardening behavior of T6 specimens. The different LCF behaviors could be rationalized by different deformation mechanisms under cyclic straining. T6 specimens with non-shearable θ′-phases underwent Orowan bypassing mechanism leading to the cyclic hardening behavior. While NIA specimens with shearable and non-shearable θ′-phases suffered from both particle shearing and Orowan bypassing mechanisms resulting in the cyclic stability behavior. Non-shearable θ′-phases bypassed by dislocations introduced more stress concentration, while shearable θ′-phases cut through by dislocations caused less stress concentration. Therefore, fatigue life of NIA specimen is longer than that of T6 specimen.

36 MATERIALS SCIENCE↗

A brittle fracture mechanism in thermally aged duplex stainless steels revealed by in situ high-energy X-ray diffraction

A direct relationship between the microstructural evolution and macroscopic fracture behaviors of a thermally aged (at 475 °C for 400 h) duplex stainless steel (DSS) has been established with experimental results from atom probe tomography (APT), nanoindentation and in situ synchrotron-based high-energy X-ray diffraction (HE-XRD). Furthermore, the APT experiments demonstrate that ferrite in DSS spinodally decomposes into Cr-enriched and Cr-depleted domains during thermal aging, which leads to a severe hardening effect in ferrite. The lattice strain development during deformation acquired with the in situ HE-XRD measurements confirms the cleavage fracture of α{110} and α{200} ferrite grains aligned perpendicular to loading direction. The thermally aged DSS can be readily fractured by connecting the cleavage cracks in ferrite. Conclusively, the spinodal-decomposition-induced hardening in ferrite and the premature failure of ferrite control the final brittle fracture in the aged DSS.

36 MATERIALS SCIENCE↗