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DOE OSTI2024

New insights on the effects of chemistry and temperature on α’ precipitation during aging of FeCrAl alloys

Here, the effect of Al on α' precipitation in FeCrAl alloys was studied through thermal aging of several model binary FeCr and FeCrAl alloys with Cr content of 13 wt.%, 17 wt.%, and 25 wt.% with and without 5.5 wt.% Al. Aging was performed up to 1,000h at varying temperatures from 400-500°C. At 400°C no age hardening was observed due to slow kinetics at this temperature. For both the 17Cr and 25Cr alloys, the addition of Al shows a lowering of the miscibility gap, consistent with other reports in literature. Interestingly, however, for the 25Cr alloys the addition of Al in the FeCrAl ternary alloy accelerated α' precipitation below the miscibility gap. Such enhanced precipitation has also been predicted by our atomistic kinetic Monte Carlo (AKMC) simulations. While previous literature has often focused on Al suppressing α', here we show that while Al can lower the miscibility gap in the Fe-Cr ferritic system thermodynamically, it may also enhance the kinetics of precipitation.

36 MATERIALS SCIENCE↗

DOE OSTI2013

Binder characterisation of mortars used at different ages in the San Lorenzo church in Milan

The paper describes a study on the mortars of the basilica of San Lorenzo in Milan, which was carried out to support an archaeological study aimed at dating and documenting the construction techniques used throughout the centuries. The church, which was founded between the 4th and 5th century, at the end of the period when Milan was the capital of the Roman Empire, was subjected in time to extensions, collapses and reconstructions that lasted until the Renaissance period and even later on. Thanks to the good state of conservation, San Lorenzo church is a collection of materials and construction techniques throughout a period of more than a millennium. Mortars were investigated in order to compare the binders used for structural elements built in different historical ages. From an archaeological study, samples of mortars attributed to the late Roman period, the Middle Ages and the Renaissance were available. The binder of each sample was separated by the aggregates and it was characterised on the basis of X-ray diffraction analysis, thermogravimetric analysis and scanning electron microscopy. Constituents of the binder were identified and their origin is discussed in order to investigate if they could be attributed to the original composition of the binder or to possible alteration in time due to atmospheric pollution. Results show that, even though the binder is mainly based on magnesian lime, there are significant differences in the microstructure of the binding matrix used in mortars ascribed to the different historical periods. In the Roman period, in correspondence of the structural elements that required higher strength, also hydraulic cocciopesto mortars were detected. Gypsum was found in most samples, which was maybe added intentionally. - Highlights: • Binders of mortars of San Lorenzo church in Milan were investigated. • Roman, Middle Ages and Renaissance samples were studied by XRD, TG and SEM. • Magnesian-lime binders containing silico-aluminates were used in all periods. • Cocciopesto hydraulic mortars were used only in the Roman period. • Gypsum was found in most samples, which was maybe added intentionally.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Precipitation behavior of stainless steel weld overlay cladding exposed to a long-term thermal aging

Highlights: • Silicide phase formation with G-phase was first time to be observed. • Precipitation behavior discrepancy existed at different locations of ferrite phase. • G-phase and silicide phase formed along dislocations and within ferrite matrix. • Heterogeneous distribution of elements induced silicide phase formation. - Abstract: Thermal aging behavior of stainless steel weld overlay cladding aged at 400 °C for 10,000 h was investigated. The results showed that the precipitates along the dislocation and within ferrite matrix contained the face-centered cubic structural G-phase and silicide phase. Silicide phase, supposed to be (Fe, Mn){sub 3}Si phase, preferred to form with G-phase along the dislocations and within ferrite matrix. Silicide phase showed a cube-on-cube relationship with ferrite phase and G-phase. Heterogeneous distribution of elements within Ni-Mn-Si clusters was responsible for silicide phase formation during thermal aging process, and the corresponding precipitation behavior discrepancy at different forming sites (dislocations, ferrite matrix and phase boundary) was discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2018

Extended investigation of sol aging effect on TiO2 electron transporting layer and performances of perovskite solar cells

Highlights: • Conditions of deposition of compact sol-gel TiO{sub 2} significantly influence the parameters of perovskite cells. • Sol aging originally considered as beneficial was proved to be adverse due to no repeatability, defects and residual water. • Free from such disadvantages TiO{sub 2} made from fresh sol can support as good cell parameters. • Roughness of transparent conductive oxide influences the optimal thickness of electron transporting layer. - Abstract: Organic−inorganic hybrid perovskites have created significant opportunities for low-cost and high-performance solar cells. The electron transporting layer (ETL) is one of the main components of the solar cell, which selectively transports electrons and at the same time acts as a barrier for holes. This paper focuses on the ETL composed of titanium dioxide deposited by sol-gel method. In particular, perovskite solar cells with ETL from aged titanium sol revealed significant differences of short circuit current which is 8% higher than their counterpart with ETL from fresh sol. Analysis of ETL morphology by atomic force microscopy combined with electrochemical impedance spectroscopy and optical properties measurements enabled to determine the source of this diversity. Additionally, the role of roughness of transparent electrode was indicated. The in-depth material analysis revealed some disadvantages of the ETL material, originally considered as supporting higher photovoltaic performance. The results indicated several problems associated with hardly controlled aging conditions, defects and presence of residual water, strongly advocate for TiO{sub 2} ETL form the fresh sol, which after optimization can guarantee the same good solar cell performance.

14 SOLAR ENERGY↗

DOE OSTI2016

Analysis of governing factors controlling gas transport through fresh and aged triptycene-based polyimide films

In this report the fundamental gas transport properties and physical aging behavior of a series of triptycene-based polyimides with various substitution groups were investigated. Wide-angle x-ray diffraction revealed that the 6FDA-1,4-triptycene polyimides exhibit two chain packing domains with d-spacing values of ~6.7 Å and ~5.3 Å, corresponding to triptycene-induced chain packing disruption and chain segments lacking the triptycene moiety, respectively. Positron annihilation lifetime spectroscopy (PALS) showed a bimodal distribution of microcavity size made up of triptycene cleft cavities that are ~3 Å diameter and larger interchain cavities with an average diameter of ~7 Å. Additionally, PALS confirmed 6FDA-1,4-trip_CH 3 has the lowest fractional free volume, primarily due to smaller contributions from the interchain cavities, and 6FDA-1,4-trip_CF 3 has the largest fractional free volume. It was also found that the addition of substituent groups had a unique and positive effect on the aging properties over nine months, in which the addition of CH 3 and CF 3 groups led to permeability increases of ~20% and ~40%, respectively. This is caused by the combination of the lowered driving force for physical aging, the substituent groups sterically hindering tighter packing with time, and the interconnectivity and/or unblocking of free volume over time through small-scale, local chain motion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

Ultra-selective CANAL Polymers for Hydrogen-based Membrane Separations after Long-Term Aging

Hydrogen is a critically important molecule in the chemicals and energy industries, driving the need for efficient purification technologies such as membrane-based separations. However, polymer membranes often suffer from physical aging, leading to decreased gas permeability over time. This study leverages the unique aging behavior of contorted microporous polymers, synthesized via catalytic arene-norbornene annulation (CANAL) polymerization, to enhance molecular sieving for H 2 separations. While prior studies demonstrated a 1000% increase in H 2 /CH 4 selectivity with minimal permeability loss over 150 days, we extend this investigation to hyperaged (∼1 year) CANAL polymers and evaluate their performance under various conditions of industrial relevance. We report a remarkable 6100% increase in H 2 /CH 4 selectivity and a 2400% improvement in H 2 /N 2 selectivity, with only a 55% decline in H 2 permeability. These membranes exhibit excellent long-term stability in binary and ternary gas mixtures and at elevated temperatures. Additionally, extended aging enhances H 2 /CO 2 selectivity beyond the 2008 upper bound due to improved size-sieving. High-temperature permeation experiments and grand canonical Monte Carlo simulations reveal that H 2 permeability increases from 570 to 3500 barrer as the temperature rises from 35 °C to 190 °C, while H 2 /CO 2 selectivity declines from 14 to 3 due to the higher diffusion activation energy of CO 2 . Despite this tradeoff, hyperaged CANAL membranes maintain performance beyond the 200 °C upper bound, having selectivity–permeability performance comparable to many state-of-the-art membranes for H 2 /CO 2 separations. As a result, this study highlights the robustness and industrial viability of ultra-selective CANAL polymers for hydrogen purification, contributing to advancements in clean energy and sustainable separation technologies.

36 MATERIALS SCIENCE↗

DOE OSTI2016

Precipitation kinetics during aging of an alumina-forming austenitic stainless steel

The microstructural evolution of DAFA26, an alumina-forming austenitic (AFA) stainless steel, was investigated during aging. The effect of aging at 750 °C and 800 °C on the growth of spherical γ’-Ni 3 (Al, Ti) particles present in the as-processed state was studied extensively using X-ray diffraction, microhardness testing, scanning electron microscopy, transmission electron microscopy, and atom probe tomography. The γ’ particles had a cube-on-cube orientation relationship with the matrix (i.e. ((010)(010) m //(010)(010) p , [100][100] m //[100][100] p )). The coarsening kinetics of γ’-Ni 3 Al particles were in agreement with the Lifshitz, Slyozof-Wagner theory. Coarse Laves phase particles were also present in the as-processed state, and during the aging process both smaller Laves phase precipitates and B2-NiAl precipitates formed on both the grain boundaries and in the matrix. As a result, the γ’ precipitates were determined to have the most impact on the room temperature hardness.

36 MATERIALS SCIENCE↗

DOE OSTI2017

Anomalous aging of EPDM and FEPM under combined thermo-oxidative and hydrolytic conditions

Previous observation of EPDM and FEPM materials aged in thermo-oxidative and thermo-oxidative plus hydrolytic environments revealed an unusual trend: the degradation and disintegration of these polymers in the former case but the ability to maintain mechanical performance and shape in the latter [1]. No abnormalities were observed in the chemical (oxidation rates, FTIR spectra, solvent uptake, gel content, and weight loss vs. temperature) or physical (modulus profile) measurements that could explain these empirically observed aging differences. A second controlled aging test was conducted to verify this trend using only EPDM. Once again it was shown that thermo-oxidative conditions appear to cause more degradative damage (enhanced embrittlement) than observed for the combined thermo-oxidative plus hydrolytic environments. From these data we conclude that water may favorably interfere with normal thermo-oxidative degradation processes. This interference may occur via some combination of chemical and physical property changes in the presence of steam such as: oxidation rate and O2 permeability changes, additional sensitivity to hydrolytic damage, and/or mechanistic changes in relation to pH and hydroperoxide formation.

15 GEOTHERMAL ENERGY↗

DOE OSTI2026

Hygrothermal aging effects on polyimide and acrylate-based adhesive materials in high-performance flat-flex cable assemblies

Flat-flex assemblies are widely used across a diverse range of technologies, including consumer electronics, automotive systems, aerospace and defense applications, and medical devices, due to their compact form factor and flexibility. However, environmental stressors like temperature and humidity are known to degrade performance over time, though the main mechanisms for degradation remain unknown. Here, in this work, we examined the aging behavior of copper/polyimide/adhesive laminate systems under varying temperature and humidity conditions, focusing on material degradation and its effects on mechanical and dielectric properties. Results show that peel strength and breakdown voltage decrease with exposure time, temperature, and humidity; spectroscopic characterization revealed that the adhesive, and not the polyimide, is the weak link in the material stack-up. The adhesive, identified as a butyl acrylate-acrylonitrile (BA-AN) copolymer, exhibited age-related spectral changes that correlated with exposure severity and duration. Hydrolysis at BA ester and AN nitrile groups was identified as the primary degradation mechanism, producing amides, acids, and alcohols. We developed a mechanistic model that connects kinetic parameters for BA-AN spectral band decay to peel strength and breakdown voltage, and implicates hydrolysis at the AN moiety, not BA, in performance decrements. Modeling predictions at ambient conditions indicate faster decline in peel strength than dielectric strength at early times, followed by plateauing of both properties at longer times. These findings provide critical insights into laminate aging mechanisms and highlight the importance of addressing BA-AN degradation to improve the long-term reliability of these systems in high-humidity environments.

organic↗

DOE OSTI2015

Examination of the mechanism for the reversible aging behavior at open circuit when changing the operating temperature of (La 0.8 Sr 0.2 ) 0.95 MnO 3 electrodes

The aging behavior of symmetrical cells, consisting of either (La 0.8 Sr 0.2 ) 0.95 MnO 3 (LSM) or La 0.6 Sr 0.4 Co 0.2 Fe 0.8 O 3 (LSCF) electrodes screen printed on either 8 mol% yttria-stabilized zirconia (YSZ) or Ce 0.8 Gd 0.2 O 2 (GDC) electrolyte substrates, is reported as the symmetrical cell is thermally cycled between 700 °C and 800 °C. For LSM, between 700 °C and 850 °C, the polarization resistance exhibits slow increases or decreases with time (on the order of days) after a quick change in temperature. When increasing the temperature, the polarization resistance decreases with time, and when decreasing the temperature, the polarization resistance slowly increases with time. In a previous work, the authors had explained these results with LSM by connecting the testing conditions to literature reports of surface analysis of LSM thin films which demonstrated a change in the amount of surface cation segregation as a function of temperature. In this work, TEM/EDS/XPS analysis of dense LSM pellets thermally cycled under the same conditions as the symmetrical cells does not indicate any significant reversible change in the surface composition of the LSM pellet between 700 °C and 800 °C. An alternative hypothesis is proposed to explain the relationship between polarization resistance and the LSM cation/anion vacancy concentrations controlled by the Schottky reaction. The timescale of aging behavior is related to the time necessary for the cations to move to or from the LSM surface to adjust to the new equilibrium at each temperature. Furthermore, the relevance in understanding the mechanism behind the aging behavior is emphasized with respect to fuel cell sample/stack modeling as well as to proper testing procedures for reaching reliable conclusions when comparing different electrode samples.

42 ENGINEERING↗

DOE OSTI2013

Yes-associated protein homolog, YAP-1, is involved in the thermotolerance and aging in the nematode Caenorhabditis elegans

The mammalian Hippo pathway comprises mammalian Ste20-like kinases (MST1/2) and large tumor suppressor kinases (LATS1/2). LATS1/2, which are activated by MST1/2, phosphorylate a transcriptional co-activator, yes-associated protein (YAP), and induce the recruitment of YAP by 14-3-3 to cytoplasm, so that the TEAD-dependent gene transcriptions are turned off. Although the core components of the Hippo pathway are well conserved in metazoans, it has been discussed that Caenorhabditis elegans lacks YAP ortholog, we found that F13E6.4 gene encodes a protein that shows sequence similarities to YAP in the N-terminal TEAD-binding domain and in the WW domain. We designated this gene as yap-1. YAP-1 is widely expressed in various cells such as epithelial cells, muscles, hypodermal cells, gonadal sheath cells, spermatheca, and hypodermal cells. YAP-1 is distributed in cytoplasm and nuclei. wts-1 (LATS ortholog) and ftt-2 (14-3-3 ortholog) knockdowns cause nuclear accumulation of YAP-1, supporting that the subcellular localization of YAP-1 is regulated in a similar way as that of YAP. Heat shock also causes the nuclear accumulation of YAP-1 but after heat shock, YAP-1 translocates to cytoplasm. Knockdowns of DAF-21 (HSP90 ortholog) and HSF-1block the nuclear export of YAP-1 during this recovery. YAP-1 overexpression is beneficial for thermotolerance, whereas YAP-1 hyperactivity induced by wts-1 and ftt-2 knockdowns is deleterious on thermal response and yap-1 deficiency promotes health aging. In short, YAP-1 partially shares basal characters with mammalian YAP and plays a role in thermal stress response and healthy aging. - Highlights: ► We named Caenorhabditis elegans F13E6.4 gene yap-1 as a putative YAP homolog. ► The localization of YAP-1 is regulated by WTS-1 and FTT-2. ► YAP-1 is involved in healthy aging and thermosensitivity.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2021

Reducing lipofuscin accumulation and cardiomyocytic senescence of aging heart by enhancing autophagy

Highlights: • Lipofuscin accumulation varies in different regions and tissues of the heart. • Lipofuscin accumulation is related to cardiomyocytic senescence. • Enhancement of autophagy alleviates lipofuscin accumulation and myocardial senescence. Cardiomyocytes are particularly prone to lipofuscin accumulation. In the aging heart, lipofuscin accumulation is augmented. This study examined distribution of lipofuscin and senescent cardiomyocytes and evaluated improvement of lipofuscin accumulation and cardiomyocytic senescence of the aging heart after treatment with rapamycin. The results of Schmorl staining, Sudan black staining and autofluorescence detection showed that there was more lipofuscin in the myocardium of the ventricles especially in the left ventricle. The conductive tissue contained less lipofuscin than the myocardium. In the aged hearts, lipofuscin accumulation and senescent cardiomyocytes were increased, and the level of autophagy was reduced. In double staining of Sudan black B and senescence-associated β-galactosidase, 10%–20% lipofuscin-loaded cardiomyocytes became senescent. All senescent cardiomyocytes contained lipofuscin deposits. After enhancing autophagy with feed of rapamycin for six months, lipofuscin accumulation and senescence of cardiomyocytes were improved in old rats. Colocalization of autophagic structure and lipofuscin as well as electron micrographs showed that some lipofuscin-loaded lysosomes were sequestrated by autophagic structures. This study suggests that rapamycin-enhanced autopahgy is effective for reducing lipofuscinogenesis and promoting degradation of lipofuscin. Therefore, enhancing autophagy is a novel therapy for alleviating lipofuscin accumulation and myocardial senescence.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2025

Creation of Self-Semi-Interpenetrating Network Structures in PIM-1 Membranes for Enhanced Physical Aging Resistance

A series of self-semi-interpenetrating network (ssIPN) thin films based on PIM-1 structure were developed by end-cross-linking telechelic PIM-1 oligomers end-capped with curable carboxylic acid groups to form model networks, which are penetrated by linear high-molecular-weight PIM-1 chains. ssIPN films with systematically varied network content ranging from 10 to 30 wt % were comprehensively examined on their microstructure and gas permeation properties. Fresh PIM-1 ssIPN films exhibited gas separation performances close to those of as-cast linear PIM-1, where the films closely followed the upper bound trade-off line, gaining as much selectivity as they lose gas permeability as the network content increases. This indicates that gas permeability is largely preserved despite cross-linking. Wide-angle X-ray scattering supported this observation, with peaks shifting toward lower d-spacing as oligomer content increased, suggesting tighter chain packing with higher cross-linkable oligomer loading. In physical aging studies over two months, all ssIPN films outperform linear PIM-1 for H 2 /CH 4 and O 2 /N 2 separations. Notably, the PIM-1 ssIPN with 10 wt % network content showed the best physical aging resistance, with negligible permeability loss even after one month. Finally, these findings highlight a promising macromolecular strategy for enhancing the physical aging resistance of microporous polymer membranes for gas separation.

PIM-1↗

DOE OSTI2019

Interplay between Swelling Kinetics and Nanostructure in Perfluorosulfonic Acid Thin-Films: Role of Hygrothermal Aging

Impacts of processing, storage, and operation on thin-film perfluorosulfonic acid (PFSA) ionomer coatings used in electrodes of electrochemical devices remains unestablished. In this work, alteration of structure–function relationship in ionomers is achieved via exposure to elevated temperature and humidity (hygrothermal aging). Findings reflect a strong inverse correlation between aging-induced ionomer thin-film domain orientation and water-transport kinetics evaluated from swelling. Finally, impact of aging is shown to be more pronounced on platinum due to interactions with PFSA, as evidenced by greater increase in nanodomain orientation parallel to substrate accompanied by reduced water transport, in contrast to silicon support.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Strong Sensitivity of Simulated Biomass Burning Aerosol Transport and Radiative Effects Over the South Atlantic to Carbonaceous Aerosol Aging and Particle Density

Biomass burning aerosol (BBA) impacts climate through aerosol‐cloud‐radiation interactions, but models disagree on the sign and magnitude of BBA radiative effects. We quantify the sensitivity of BBA radiative effects and transport to three BBA‐relevant processes and properties: parameterized oxidative aging of organic aerosol (OA), a combined change to black carbon (BC) density and the method for calculating aerosol refractive index, and reduction in OA density. We evaluate Unified Model simulations against two aircraft campaigns from summer 2017 over the Southeast Atlantic. The model generally performs well, such that discrepancies between the observational data sets may sometimes limit the precision of the evaluation. Our newly developed aging parameterization reproduces observed OA:BC mass ratios well and allows modeled OA:BC to decrease with smoke age, but increases bias in aerosol extinction and changes the BBA radiative effect little (+0.12 W m -2 ). We calculate aerosol refractive index using either a volume‐weighted component average or the Maxwell‐Garnett (MG) mixing assumption, which represents BC as small inclusions in a host material. Compared to MG mixing, the volume‐weighted average refractive index and reduced BC density increase aerosol absorption, substantially increasing the total BBA radiative effect (+2.66 W m -2 ) and amount of BBA transported across the ocean through BC self‐lofting. Reducing OA density to better match literature values changes the total BBA radiative effect by −1.96 W m -2 . Changes to direct radiative effects exceed changes to cloud radiative effects. Our findings emphasize the sensitivity of aerosol radiative effects and transport to these processes and properties, which we suggest could be improved in climate models.

Southeast Atlantic↗

DOE OSTI2024

Influence of loblolly pine anatomical fractions and tree age on oil yield and composition during fast pyrolysis

Fast pyrolysis of woody materials is a technology pathway for producing renewable fuels and chemicals. This is a presentation of isolating needles, bark, and stemwood from a single tree as well as isolating stemwood and whole tree samples from the same species of tree with different ages and pyrolyzing each individually as well as in mixtures. This gives insight into the role of tree anatomical fractions on the resulting intermediate oil product as well as into interactions between these components. The highest carbon content oil (45.1 wt% as received) was produced from a one-to-one mixture of stemwood and needles, followed by the pure stemwood (43.4–43.8 wt% as received), while the lowest oil carbon content was from a one-to-one blend of bark and needles (26.7 wt% as received). The pyrolysis oil yield (combining oil and aqueous where separation occurred) varied from 54 wt% as received (needles) to 72.3 wt% as received (stemwood). When comparing trees of different ages, we find the change in the ratio of the anatomical fractions is a dominant factor in the product composition and yields, while the product composition and yields vary slightly with tree age when only the stemwood is pyrolyzed. Here, in this study, we present the bench-scale pyrolysis, yields, and product characterization of loblolly pine feedstocks (13- vs. 23 year-old, residues, air-classified residues, whole tree, needles, bark, and stemwood).

09 BIOMASS FUELS↗

DOE OSTI2011

Surface enhanced Raman scattering of aged graphene: Effects of annealing in vacuum

In this paper, we report a simple method to recover the surface enhanced Raman scattering activity of aged graphene. The Raman signals of Rhodamine molecules absorbed on aged graphene are dramatically increased after vacuum annealing and comparable to those on fresh graphene. Atomic force microscopy measurements indicate that residues on aged graphene surface can efficiently be removed by vacuum annealing, which makes target molecule closely contact with graphene. We also find that the hole doping in graphene will facilitate charge transfer between graphene and molecule. These results confirm the strong Raman enhancement of target molecule absorbed on graphene is due to the charge transfer mechanism.

36 MATERIALS SCIENCE↗

DOE OSTI2012

Ageing of a neutron shielding used in transport/storage casks

In radioactive materials transport/storage casks, a mineral-filled vinylester composite is used for neutron shielding which relies on its hydrogen and boron atoms content. During cask service life, this composite is mainly subjected to three types of ageing: hydrothermal ageing, thermal oxidation and neutron irradiation. The aim of this study is to investigate the effect of hydrothermal ageing on the properties and chemical composition of this polymer composite. At high temperature (120 Degree-Sign C and 140 Degree-Sign C), the main consequence is the strong decrease of mechanical properties induced by the filler/matrix debonding.

36 MATERIALS SCIENCE↗