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Research study for gel precursors as glass and ceramic starting materials for space processing applications research

The development of techniques for the preparation of glass and ceramic starting materials that will result in homogeneous glasses or ceramic products when melted and cooled in a containerless environment is described. Metal-organic starting materials were used to make compounds or mixtures which were then decomposed by hydrolysis reactions to the corresponding oxides. The sodium tungstate system was chosen as a model for a glass with a relatively low melting temperature. The alkoxide tungstates also have interesting optical properties. For all the compositions studied, comparison samples were prepared from inorganic starting materials and submitted to the same analyses.

Downs, R. L.↗

Microstructural Study of Micron-Sized Craters Simulating Stardust Impacts in Aluminum 1100 Targets

Various microscopic techniques were used to characterize experimental micro- craters in aluminium foils to prepare for the comprehensive analysis of the cometary and interstellar particle impacts in aluminium foils to be returned by the Stardust mission. First, SEM (Scanning Electron Microscopy) and EDS (Energy Dispersive X-ray Spectroscopy) were used to study the morphology of the impact craters and the bulk composition of the residues left by soda-lime glass impactors. A more detailed structural and compositional study of impactor remnants was then performed using TEM (Transmission Electron Microscopy), EDS, and electron diffraction methods. The TEM samples were prepared by Focused Ion Beam (FIB) methods. This technique proved to be especially valuable in studying impact crater residues and impact crater morphology. Finally, we also showed that InfraRed microscopy (IR) can be a quick and reliable tool for such investigations. The combination of all of these tools enables a complete microscopic characterization of the craters.

Leroux, Hugues↗

Do Minor Interactions Trigger Star Formation in Galaxy Pairs?

Abstract We analyze the galaxy pairs in a set of volume limited samples from the Sloan Digital Sky Survey to study the effects of minor interactions on the star formation rate (SFR) and color of galaxies. We carefully design control samples of isolated galaxies by matching the stellar mass and redshift of the minor pairs. The SFR distributions and color distributions in the minor pairs differ from their controls at >99% significance level. We also simultaneously match the control galaxies in stellar mass, redshift and local density to assess the role of the environment. The null hypothesis can be rejected at >99% confidence level even after matching the environment. Our analysis shows a quenching in the minor pairs where the degree of quenching decreases with the increasing pair separation and plateaus beyond 50 kpc. We also prepare a sample of minor pairs with H α line information. We calculate the SFR of these galaxies using the H α line and repeat our analysis. We observe a quenching in the H α sample too. We find that the majority of the minor pairs are quiescent systems that could be quenched due to minor interactions. Combining data from the Galaxy Zoo and Galaxy Zoo 2, we find that only ∼1% galaxies have a dominant bulge, 4%–7% galaxies host a bar and 5%–10% of galaxies show active galactic nucleus (AGN) activity in minor pairs. This indicates that the presence of bulge, bar or AGN activity plays an insignificant role in quenching the galaxies in minor pairs. The more massive companion satisfies the criteria for mass quenching in most of the minor pairs. We propose that the stripping and starvation likely caused the quenching in the less massive companion at a later stage of evolution.

Astronomy & Astrophysics↗

Data on Cu- and Ni-Si-Mn-rich solute clustering in a neutron irradiated austenitic stainless steel

The data presented in this article is supplementary to the research article “Phase instabilities in austenitic steels during particle bombardment at high and low dose rates” (Levine et al.). Needle-shaped samples were prepared with focused ion beam milling from a 304L stainless steel that was irradiated with fast neutrons (E 0.1 MeV) in the BOR-60 reactor at 318 °C to 47.5 dpa. Atom probe tomography (APT) experiments in voltage mode were then conducted on a Cameca LEAP 5000X HR. Atom position, range, and mass spectrum files after reconstruction with Cameca’s IVAS software are included. Cu- and Ni-Si-Mn-rich solute nanoclusters were identified and analyzed using the Open Source Characterization of APT Reconstructions (OSCAR) program. Python code for OSCAR, information on the program’s underlying algorithm, and sample output files are provided. A proximity histogram of a Ni-Si-Mn-rich cluster and a 1D density/solute concentration profile of a Cu-rich cluster are given to demonstrate OSCAR’s analytical functionalities. The provided APT dataset is valuable for benchmarking phase instabilities in neutron-irradiated austenitic stainless steels that occur at high doses. The OSCAR program can be reused to process other APT data sets where solute nanoclustering is of interest.

42 ENGINEERING↗

Synthesis and characterization of magnetic ionic liquids containing multiple paramagnetic lanthanide and transition metal centers and functionalized diglycolamide ligands

Magnetic ionic liquids (MILs) containing paramagnetic centers have gained widespread recognition as sustainable solvents due to their ability to respond to an external magnetic field. The physico-chemical properties of MILs are dependent on the choice of anion/cation ligands and metal centers; the search for highly tunable ligands and precursors that can confer favorable characteristics, such as low viscosity, is ongoing. Diglycolamides employed as cationic ligands have been previously shown to form hydrophobic MILs that can simultaneously incorporate multiple lanthanide metal centers in both the anion/cation. Despite their enhanced magnetic susceptibility, the effect of diglycolamide chemical structure modifications on the physico-chemical properties of MILs has not been thoroughly studied. Additionally, the possibility of forming diglycolamide-based MILs with popularly employed transition metals has not been investigated and combinations that can simultaneously embed two different types of metal centers in both the anion/cation have not been explored. In this study, thirty (30) MILs comprised of lanthanide and transition metals were synthesized by examining their chelation to both straight-chained and branched diglycolamides. Here, transition metal-based MILs were found to possess high thermal stabilities up to 235 °C compared to 192 °C for those comprised of lanthanides. While MILs comprised of rare-earth metal centers exhibited the lowest viscosities, substituting lanthanides with transition metals in just the anion or cation resulted in enhanced thermal stability and reduced viscosity. The effective magnetic moment for these MILs varied between 4.71 and 21.08 µ B and was much higher compared to all previous classes of MILs prepared using the same metals. Results from this study explore all possible modifications that can be made to these MILs in an effort to demonstrate their structural tunability, which is often highly desirable in various applications, including organic synthesis and chemical separations.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Application of Raman Spectroscopy to Determine Uranium Content in ADUN Solution

The work presented in this report is part of the ongoing efforts to address the nuclear material control and accounting needs for advanced reactor fuel fabrication facilities. This work was supported by the Materials Protection, Accounting, and Control Technologies (MPACT) program under the US Department of Energy Office of Nuclear Energy‘s Nuclear Fuel Cycle and Supply Chain program. The activities and engagements under the MPACT program are designed to support a robust US civilian nuclear energy enterprise. In the work described in this report, we supported MPACT objectives by developing measurement techniques that could be used for material accounting and process monitoring and by working with industry partners to identify existing gaps and areas for improvement. Oak Ridge National Laboratory has been working with commercial tristructural isotropic (TRISO) fuel fabricators such as Standard Nuclear to develop technology for rapid and cost-effective uranium content assessment. This work has focused on demonstrating advanced measurement techniques (e.g., Raman spectroscopy) that can be used for rapid, reliable, and cost-effective routine measurements of uranium content in feed solutions and liquid waste streams as well as for monitoring in-line process measurements and product streams. Specifically, this report explores techniques for accurately determining uranium content in acid-deficient uranyl nitrate (ADUN) solutions and detecting low uranium concentrations in ammonia solutions. Developing such measurement techniques will benefit TRISO fuel fabrication facilities, facilities involved in other parts of the fuel cycle that require online monitoring of aqueous solutions, and potentially molten salt fuel reactors. This work supports developing Raman spectroscopy procedures to determine uranium concentrations in ADUN solutions, which are used as feedstock in the sol–gel process for creating TRISO fuel. Some additional benefits of using Raman spectroscopy for uranium quantification in fabrication facilities include enabling online monitoring of the chemical process, which would provide near real-time feedback; eliminating the need for sample transfers, preparation, or dilution; providing nondestructive measurements; and user friendliness. In this fiscal year, FY25, we determined the identity of the unknown Raman band at approximately 853 cm−1 that was discovered in ADUN Raman spectra in FY24, created calibration curves and determined uranium concentrations of two ADUN solutions, and compared the Raman results to results obtained from inductively coupled plasma mass spectrometry and Davies–Gray titration. Furthermore, we have identified focus areas for experimentation in future fiscal years. A key result is that the accuracy of using Raman can provide accuracy comparable to destructive analysist techniques, With a well-developed calibration curve, using standards and a large number of samples (more than five samples), uncertainty on the order of 1%–3% is achievable. Given that the uncertainties achieved by Raman spectroscopy were on the order of the uncertainties achieved using ICP-MS, we conclude that with a well-developed procedure Raman spectroscopy can be used to determine uranium concentrations in ADUN solutions for NMC&A applications. The benefits of such an approach are that the time and effort will be less than that of comparable destructive analysis techniques, with approximately the same level of technical expertise. This will be attractive to operators of fuel fabrication facilities as it will lower costs and improve efficiencies.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Mercury Speciation via Diffusive Gradients Thin-Films Technology

Objectives: Develop and test various diffusive gradient in thin films (DGT) samplers for mercury - SRNL is developing reactive DGTS (rDGTs). Test chemistry to differentiate methylmercury from total and/or inorganic mercury in environmental samples. Fabricate and test rDGT samplers for deployment. Deploy the rDGTs in variable settings. Mercury is a persistent-bioaccumulative-toxic environmental pollutant. Mercury exists in different species such as elemental, inorganic, and methyl. Mercury speciation determine mercury behavior and toxicity. For example, methylmercury strongly accumulates in biota such as fish resulting in potential human health impacts. DGTs are innovative samplers to measure water concentration by diffusion and capture. Types of Hg DGTs used: Total Hg, Inorganic Hg, and Methyl Hg. Deployment Sites: Upper Three Runs, Lower Three Runs, Steele Creek, East Fork Poplar Creek (SRNL Sites), Horizons Creek, NOA Creek, Bruners Creek (ORNL Sites). DGT concentration estimates closely matched alternative measurements for soluble mercury at each Oak Ridge site - DGTs did not respond to particulate mercury. DGTs provide a representative measure for biota uptake since they are left out longer which allows for an average exposure concentration. DMA-80 provided an efficient and quick analysis. Variability in site location made a difference in Hg species. DGT preparations and sampling wasn't as quick and simple as microcolumn technology. Copper reagent degraded agarose gel - more work and cleaner data are needed to assess speciation in rDGTs. Future Work: Use cross-linked polyacrylamide for the collection layer for a stronger plastic. Make a copper diffusion layer without agarose. Test copper separation in lab using realistic stream conditions such as high organic carbon.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Solar wind-induced secondary ions and their relation to lunar surface composition

Based on previous laboratory experiments simulating solar wind sputtering of lunar surface materials, it appears that solar wind ions sputter secondary ions in sufficient numbers to be measured from low-altitude lunar orbit. Solar wind protons are hundreds of times less efficient than those used in standard secondary ion mass spectrometry; nevertheless secondary ions of Na, Mg, Al, Si, K, Ca, Mn, Ti and Fe were observed sputtered from sample simulants of mare and highland soils. These secondary ion fluxes depend both on concentration in the soil and on probability of ionization; yields of easily ionized elements such as K and Na are relatively much greater than those for the more electronegative elements and compounds. The principal geochemical indicator elements Na, Mg, Al, Si, K, Ca, Ti, Mn and Fe are nevertheless detectable. However, it has not been shown that the observed secondary ions vary strictly one-to-one with their concentrations in the geochemically distinct soil simulants used here. While we have a first order understanding of secondary ion sputtering, it is not clear that the observed ion yields can be linked with great accuracy to the simulant's composition. The simulants were analyzed by electron microprobe to establish their detailed composition. The observed secondary ion fluxes can then be compared with the microprobe results. For example Ti(+) fluxes from the three simulants correspond to the true composition with accuracies of better than 10 percent for the high-Ti basalt, and about 20 percent for the low-Ti simulant. The highlands simulant produced a statistically insignificant Ti(+) count rate. Here we discuss the results of further SIMS experiments using the ASU/Center for Solid State Science facility. With careful isolation and preparation of samples, we avoid the problems of the previous experiments. In particular, we will make use of ground-up sample to mimic the sputtering behavior of regolith, and will avoid charging by placing the soil on a conducting indium substrate. We report the results of a blind test of the SIMS technique using a sample of unknown composition.

Elphic, R. C.↗

Quantifying the cooperative evolution of microphase segregation and nanostructural order in annealed polyurethanes of MDI-BDO-PTHF

Here, we quantify the relationship between microphase segregation and local structure development in thermoplastic polyurethanes. Samples were prepared with varying ratios of 4,40 -methylene diphenyl diisocyanate (MDI) and 1,4-butanediol (BDO) to polytetrahydrofuran (PTHF) and annealed at temperatures T a between RT–140 °C for 20 h each. Distinct populations of smaller and larger ordered domains are distinguished by pair distribution func tion analysis. The intermediate-range order of nanoscale hard domains in the paracrystalline state (form I) is directly extracted and characterized. The results suggest that form I of the MDI-BDO:PTHF system presents a conformational and packing order similar to the form III structure, typically obtained from stretching/annealing, but with limited spatial coherence of 3–7 nm. Heating above T g of the hard segments is necessary to achieve a substantial structural response from the annealing treatment. Increasing T a promotes purification of the soft phase via microphase segregation, coalescence of the hard blocks, and growth of paracrystalline phase, while a minority fraction of longer-range ordered domains left over from production remains relatively constant. We observe a composition-dependent decrease in the average nearest-neighbor dis tance that can be correlated with the greater number of C C, C N, and C O bonds with increased hard segment content. A non-linear deviation in the trend is observed to correlate with sample densification. The mechanical and thermal behavior of the samples is intimately tied to the segregation state.

processing-structure-properties↗

NanoSIP: NanoSIMS Applications for Microbial Biology

High-resolution imaging with secondary ion mass spectrometry (nanoSIMS) has become a standard method in systems biology and environmental biogeochemistry and is broadly used to decipher ecophysiological traits of environmental microorganisms, metabolic processes in plant and animal tissues, and cross-kingdom symbioses. When combined with stable isotope-labeling—an approach we refer to as nanoSIP—nanoSIMS imaging offers a distinctive means to quantify net assimilation rates and stoichiometry of individual cell-sized particles in both low- and high-complexity environments. While the majority of nanoSIP studies in environmental and microbial biology have focused on nitrogen and carbon metabolism (using 15 N and 13 C tracers), multiple advances have pushed the capabilities of this approach in the past decade. The development of a high-brightness oxygen ion source has enabled high-resolution metal analyses that are easier to perform, allowing quantification of metal distribution in cells and environmental particles. New preparation methods, tools for automated data extraction from large data sets, and analytical approaches that push the limits of sensitivity and spatial resolution have allowed for more robust characterization of populations ranging from marine archaea to fungi and viruses. Further, NanoSIMS studies continue to be enhanced by correlation with orthogonal imaging and ‘omics approaches; when linked to molecular visualization methods, such as in situ hybridization and antibody labeling, these techniques enable in situ function to be linked to microbial identity and gene expression. Here we present an updated description of the primary materials, methods, and calculations used for nanoSIP, with an emphasis on recent advances in nanoSIMS applications, key methodological steps, and potential pitfalls.

07 ISOTOPE AND RADIATION SOURCES↗

Flash electropolishing for TEM: Reducing FIB‐induced defects in tungsten with protocols for new materials

Focused ion beam (FIB) milling has become the dominant approach for site-specific transmission electron microscopy (TEM) specimen preparation; however, FIB damage remains a critical limitation for reliable microstructural characterisation, particularly in radiation effects studies. Tungsten is especially susceptible to FIB damage due to its high nuclear stopping power, which promotes the formation and strong diffraction contrast of FIB-induced ‘black spot’ defects that are indistinguishable from very fine irradiation-induced loops/defects resulting from low to intermediate temperature neutron irradiation. In this work, flash electropolishing is systematically evaluated as a post-FIB treatment for minimising preparation-induced artefacts for TEM analysis of tungsten-based alloys. Using a range of non-, ion-, and neutron-irradiated tungsten materials, the effectiveness of flash electropolishing has been assessed through direct comparison with conventional FIB and plasma-FIB preparation including low-energy Ga, Ar, Xe ion cleaning. The results demonstrate that flash electropolishing effectively removes FIB-damaged layers and ‘black spot’ defects, thereby enabling reliable observation of irradiation-induced dislocation structures. Key processing parameters governing flash electropolishing quality – including lamella thickness, applied voltage, polishing duration, electrolyte chemistry, and cathode geometry – have been systematically evaluated, and clear criteria were established for determining when flash electropolishing is required to ensure reliable microstructural analysis. This work also provides practical guidance for implementing flash electropolishing as an artefact-controlled specimen-preparation approach for TEM characterisation of FIB-produced specimens. The systematic protocol can be extended to other, non-tungsten materials.

TEM sample preparation↗

Soil Sampling Results for Closure of a Portion of Solid Waste Management Unit #16

The U.S. Department of Energy/National Nuclear Security Administration (DOE/ NNSA) and National Technology & Engineering Solutions of Sandia, LLC (NTESS), the management and operating contractor for Sandia National Laboratories/California (SNL/CA), has prepared this soil sampling results report for closure of a portion of Solid Waste Management Unit (SWMU) #16. The entire network of SNL/CA sanitary sewer lines, including building laterals, was identified as SWMU #16 under a Resource Conservation and Recovery Act (RCRA) Facility Assessment conducted for SNL/CA in April 1991 (DOE 1992). Along with the previous SWMU #16 investigation results (SNL/CA 2019), the results of this investigation are intended to support closure decisions by the San Francisco Bay Regional Water Quality Control Board (RWQCB), as discussed below. SNL/CA personnel completed upgrading its sanitary sewer discharge network in 2019. These upgrades included installing new sections of underground lines and decommissioning certain sections of the old piping system by capping in place. To date, several sections of the sewer line have been abandoned-in-place by capping as new sewer lines were installed or flow was rerouted to other existing lines. To formally close these abandoned sections of the sewer line, the RWQCB required that SNL/CA personnel collect soil samples to be analyzed for contaminants potentially released from the sewer lines. SNL/CA personnel hired Weiss Associates (Weiss) of Emeryville, California to prepare a sampling and analysis plan, implement the sampling plan and report the results of the investigation under Purchase Order #2166257. The Sampling and Analysis Plan for Partial Closure of Solid Waste Management Unit #16 (SAP) was submitted to the RWQCB on August 14, 2020 by Weiss on behalf of SNL/CA. The RWQCB approved the SAP on September 30, 2020 after Weiss updated the method detection limit and reporting limits for total polychlorinated biphenyls (PCBs) and individual aroclors. Soil sampling was conducted in accordance with the SAP except that fewer locations were sampled due to site constraints, as discussed below. This report presents the results of the sampling effort and documents all associated field activities including borehole clearing, soil sample collection, storage and transportation to the analytical laboratories, borehole backfilling and surface restoration, and storage of investigation-derived waste (IDW) for future profiling and disposal by SNL/CA waste management personnel.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

TEM Analyses of Itokawa Regolith Grains and Lunar Soil Grains to Directly Determine Space Weathering Rates on Airless Bodies

Samples returned from the moon and Asteroid Itokawa by NASA's Apollo Missions and JAXA's Hayabusa Mission, respectively, provide a unique record of their interaction with the space environment. Space weathering effects result from micrometeorite impact activity and interactions with the solar wind. While the effects of solar wind interactions, ion implantation and solar flare particle track accumulation, have been studied extensively, the rate at which these effects accumulate in samples on airless bodies has not been conclusively determined. Results of numerical modeling and experimental simulations do not converge with observations from natural samples. We measured track densities and rim thicknesses of three olivine grains from Itokawa and multiple olivine and anorthite grains from lunar soils of varying exposure ages. Samples were prepared for analysis using a Leica EM UC6 ultramicrotome and an FEI Quanta 3D dual beam focused ion beam scanning electron microscope (FIB-SEM). Transmission electron microscope (TEM) analyses were performed on the JEOL 2500SE 200kV field emission STEM. The solar wind damaged rims on lunar anorthite grains are amorphous, lack inclusions, and are compositionally similar to the host grain. The rim width increases as a smooth function of exposure age until it levels off at approximately 180 nm after approximately 20 My (Fig. 1). While solar wind ion damage can only accumulate while the grain is in a direct line of sight to the Sun, solar flare particles can penetrate to mm-depths. To assess whether the track density accurately predicts surface exposure, we measured the rim width and track density in olivine and anorthite from the surface of rock 64455, which was never buried and has a surface exposure age of 2 My based on isotopic measurements. The rim width from 64455 (60-70nm) plots within error of the well-defined trend for solar wind amorphized rims in Fig. 1. Measured solar flare track densities are accurately reflecting the surface exposure of the grains. Track densities correlate with the amorphous rim thicknesses. While the space-weathered rims of anorthite grains are amorphous, the space-weathered rims on both Itokawa and lunar olivine grains show solar wind damaged rims that are not amorphous. Instead, the rims are nanocrystalline with high dislocation densities and sparse inclusions of nanophase Fe metal. The rim thicknesses on the olivine grains also correlate with track density. The Itokawa olivine grains have track densities that indicate surface exposures of approximately 10(exp 5) years. Longer exposures (up to approximately 10(exp 7) years) do not amorphize the rims, as evidenced by lunar soil olivines with high track densities (approximately 10(exp 11) cm(exp -2)). From the combined data, shown in Fig. 1, it is clear that olivine is damaged (but not amorphized) more rapidly by the solar wind compared to anorthite. The olivine damaged rim forms quickly (in approximately 10(exp 6) y) and saturates at approximately 120nm with longer exposure time. The anorthite damaged rims form more slowly, amorphize, and grow thicker than the olivine rims. This is in agreement with numerical modeling data which predicts that solar wind damaged rims on anorthite will be thicker than olivine. However, the models predict that both olivine and anorthite rims will amorphize and reach equilibrium widths in less than 10(exp 3) y, in contrast to what is observed for natural samples. Laboratory irradiation experiments, which show rapid formation of fully amorphous and blistered surfaces from simulated solar wind exposures are also in contrast to observations of natural samples. These results suggest that there is a flux dependence on the type and extent of irradiation damage that develops in olivine. This flux dependence suggests that great caution be used in extrapolating between high-flux laboratory experiments and the natural case, as demonstrated by. We constrain the space weathering rate through analysis of returned samples. Provided that the track densities and the solar wind damaged rim widths exhibited by the Itokawa grains are typical of the fine-grained regions of Itokawa, then the space weathering rate is on the order of 10(exp 5) y. Space weathering effects in lunar soils saturate within a few My of exposure while those in Itokawa regolith grains formed in approximately 10(exp 5) y. Olivine and anorthite respond differently to solar wind irradiation. The space weathering effects in olivine are particularly difficult to reconcile with laboratory irradiation studies and numerical models. Additional measurements, experiments, and modeling are required to resolve the discrepancies among the observations and calculations involving solar wind amorphization of different minerals on airless bodies.

Berger, Eve L.↗

Preparing to Receive and Handle Martian Samples When They Arrive on Earth

The Astromaterials Acquisition and Curation Office at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10F+ derivative NPR 'Curation of Extraterrestrial Materials', JSC is charged with 'The curation of all extraterrestrial material under NASA control, including future NASA missions. 'The Directive goes on to define Curation as including'...documentation, preservation, preparation, and distribution of samples for research, education, and public outreach."

McCubbin, Francis M.↗

Preparation of a 73 As source sample for application in an offline ion source

For the generation of beams with the offline ion source at the Facility for Rare Isotope Beams (FRIB), suitable source samples are required. Arsenic-73 is a frequently requested user beam due to its significance in nuclear structure studies and astrophysics. In this work, we outline the process of preparing a 73 As source sample, containing (5.76 ± 0.37)∗10 14 atoms of 73 As, which was successfully used to generate a 73 As beam for a multi-day user experiment. Silver arsenate was chosen as the chemical form, due to its favorable volatility within the designated operating temperature range. We refined the precipitation method using stable arsenic prior to its application with the 73 As sample, resulting in precipitation yields of (99.4 ± 4.5)%.

As-73↗

Ultra-selective membrane composed of charge-stabilized fixed carrier and amino acid-based ionic liquid mobile carrier for highly efficient carbon capture

Membrane technology has been extensively studied for CO 2 capture applications, especially for flue gas sources. In the past decades, facilitated transport membranes (FTMs) have made breakthroughs overcoming the permeance-selectivity trade-off upper bound restricting traditional CO 2 separation membranes, but are still facing challenges towards practical applications, including limited performance, such as insufficient CO 2 /N 2 selectivity to achieve 95 % CO 2 dry-base purity by one step separation, and long-term stability. Herein, we designed and fabricated a novel FTM structure containing an ionic liquid (1-ethyl-3-methylimidazolium aminoacetate, [Emim][Gly]) as mobile CO 2 -carrier and a polymeric amine (polyethyleneimine, PEI) as fixed CO 2 -carrier. In this study, the fixed carrier is confined within a carbon nanotube (CNT) framework of 230 nm thickness via electrostatic forces adjusted by a polyelectrolyte (polystyrene sulfonate, PSS), while the mobile carrier diffuses freely within the CNT framework. After optimization of the membrane recipe and spray-coating fabrication procedure, following our previous work, the resulting CNT-PSS-PEI ~ IL membranes demonstrated an ultra-high CO 2 /N 2 selectivity up to 1,000 with CO 2 permeance up to 2,400 GPU (Gas Permeation Unit, 1 GPU = 3.348 × 10 -10 mol·s -1 ·m -2 ·Pa -1 ) under vacuum operation condition. Furthermore, one 100-cm 2 flat sheet membrane sample was prepared and exhibited one-stage CO 2 enrichment from 15 % to 95 % purity (dry-base) for the first time amongst all reported CO 2 separation membranes. The membrane retained a stable performance over 50-h operation period under vacuum condition. The extraordinary CO 2 separation performance illustrates the great potential of the CNT-PSS-PEI ~ IL membranes for flue gas carbon capture application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Cation uptake by fine aggregate in hardened cement mortar and its effect on electrical properties

Electrical resistivity tests can be used to evaluate the transport properties of concrete and provide a durability assessment. However, the electrical resistivity is largely dependent on the pore solution composition and recent work suggests that some aggregates have the capacity for cation uptake. This study first aims to provide further evidence for adsorption of cations on aggregate surfaces, without formation of reaction products (e.g. alkali-silica reaction). Secondly, hardened mortar samples were prepared using a fine aggregate with a high alkali affinity and a non-reactive fine aggregate as a control. The electrical resistivity of mortars was measured, and the pore solution of these mortars was obtained through high-pressure extraction. The effect of aggregate moisture dilution on the pore solution was decoupled by using a pore partitioning model. The results indicate that aggregate minerology can influence the pore solution composition through cation uptake. Specific minerals of minor quantity, like biotite, may be responsible for cation exchange. While adsorbed cations strongly affected pore solution and formation factor measurement, the bulk resistivity measurements on hardened mortar were only marginally influenced. Research on other implications of similar aggregate interactions with pore solutions are an intriguing area for future research.

Alkali-aggregate reaction↗

Internal arcing and lightning strike damage in short carbon fiber reinforced thermoplastic composites

Short carbon fiber reinforced thermoplastic composites (S-CFRTP) are currently used in interior parts of aircraft such as electronic circuitry and assemblies, and their usage in aircraft's exterior is also being studied. In this paper, we present a lightning strike study on S-CFRTPs. High performance thermoplastics such as a polyphenylene sulfide (PPS) reinforced with 50% weight (wt.) short carbon fiber (CF), a polyphenyl sulfone (PPSU) reinforced with 25 % wt. Short CF and a acrylonitrile butadiene styrene (ABS) with 20 % wt. short CF were tested against artificial lightning strikes. All samples were prepared using an extrusion compression molding (ECM) technique. A modified component A (100 kA) of lightning waveform, as defined by SAE ARP 5412-B, was applied. High speed imaging, thermography, scanning electron microscopy (SEM) and ultrasonic non-destructive evaluation were performed to understand the effect of lightning strikes on the thermoplastic panels. The results show that electrical conductivity of the composite, thermal stability of the polymers, and CF orientation significantly affected the damage from artificial lightning strikes. PPS composite had the highest resilience against lightning strike damage, retaining 95% and 89% residual flexural strength and modulus, respectively. CF exfoliation due to internal arcing was observed in the carbon fiber-reinforced ABS polymer (CF-ABS) composite. CF exfoliation damage has been reported for the first time.

36 MATERIALS SCIENCE↗