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At least 811 records · Page 45

Totally chlorine-free peracetic acid pulping for nanocellulose isolation from hemp and poplar

Nanocellulose is a promising and sustainable feedstock for developing advanced and functional materials. However, the characteristics of nanocellulose, such as crystallinity, surface energy, and aspect ratio, can vary depending on biomass source and pretreatment methods, leading to variable performance of the nanocellu-lose-based materials. In this study, cellulose nanocrystals (CNCs) were isolated from hemp and poplar using totally chlorine free (TCF) peracetic acid and sodium chlorite delignification and bleaching pretreatments to probe the influences of biomass source and treatment methods on the isolation and characteristics of CNCs. Our results showed that hemp and poplar were almost completely delignified by peracetic acid treatment, whereas sodium chlorite treatment left 5%–6% lignin in the pulp. The yields of CNCs from raw hemp and poplar biomass ranged from 9.8% to 21.9% and 10.9% to 28.3%, respectively, depending on the treatment methods. The dimensions of CNCs from TCF-treated biomass generally maintained a larger width and aspect ratio than those from sodium chlorite-treated biomass. The poplar-derived CNCs exhibited slightly higher crystallinity of 53%–58% than hemp-derived CNCs of 49%–54%. The zeta potential of the CNCs, ranging from -20.1 mV to -31.1 mV, ensured a well-dispersed aqueous solution. The surface energy (dispersive energy of 40–80 mJ/m2 and specific energy of 2–10 mJ/m2), water interaction, and thermal stability of the CNCs were comparable, regardless of the biomass source and pretreatment methods. Our finding suggests that the TCF technique with peracetic acid treatment is a promising delignification and bleaching approach to obtain cellulose-rich pulps from herbaceous and hardwood biomass for nanocellulose isolation.

09 BIOMASS FUELS↗

Learning neural representations for X-ray ptychography reconstruction with unknown probes

X-ray ptychography provides exceptional nanoscale resolution and is widely applied in materials science, biology, and nanotechnology. However, its full potential is constrained by the critical challenge of accurately reconstructing images when the illuminating probe is unknown. Conventional iterative methods and deep learning approaches are often suboptimal, particularly under the low-signal conditions inherent to low-dose and high-speed experiments. These limitations compromise reconstruction fidelity and restrict the broader adoption of the technique. In this work, we introduce the Ptychographic Implicit Neural Representation (PtyINR), a self-supervised framework that simultaneously addresses the object- and probe-recovery problem. By parameterizing both as continuous neural representations, PtyINR performs end-to-end reconstruction directly from raw diffraction patterns without requiring any pre-characterization of the probe. Extensive evaluations demonstrate that PtyINR achieves superior reconstruction quality on both simulated and experimental data, with remarkable robustness under challenging low-signal conditions. Furthermore, PtyINR offers a generalizable, physics-informed framework for addressing probe-dependent inverse problems, making it applicable to a wide range of computational microscopy problems.

36 MATERIALS SCIENCE↗

TEAMER: Biofouling Analysis for Wave Energy Piston Design - Load Cell Data

Biofouling and corrosion are a major concern for all ocean-deployed components, especially when mechanical motion is involved. Triton has developed the concept of a biofouling mitigation seal as part of the piston sealing assembly for the Triton Wave Energy Converter (TSI-WEC). This mitigation seal has the purpose of preventing the formation of a biofilm on the inside of the piston cylinder. It is hypothesized that the prevention of a biofilm will reduce the amount of macro-biofouling that can occur in the piston assembly. The mitigation seal can also reduce the wear on the main dynamic seal, helping to maintain smooth operation and water-tightness. The cylinder is made from a thermoset composite epoxy, which is resistant to corrosion. However, no studies have researched the material's performance with biofouling. Triton placed two prototype Power Take-Off (PTO) assemblies in a PNNL biofouling tank, one with a biofouling mitigation seal and one without, allowing for an evaluation of seal effectiveness at the prevention of biofouling. In actual WEC operation, wave action would react against the piston, which would drive the linear actuator and electric generator, providing electrical power. In the test setup, this was reversed; a linear actuator was powered to drive the piston in a consistent motion within the cylinder. There are two assemblies: one has a biofouling mitigation seal, the other (control) does not. The following data encompasses a 4 month test period, with load cells being used to monitor piston friction force. Results from this testing will be used to improve seal design and material selection, mitigating risk of premature failure during open water testing and evaluation. This project is part of the TEAMER RFTS 3 (request for technical support) program.

16 TIDAL AND WAVE POWER↗

Production of levulinic acid and biocarbon electrode material from corn stover through an integrated biorefinery process

To overcome the inefficient biomass conversion, waste generation, and lack of co-production in biorefineries, an integrated process was proposed for the conversion of corn stover into levulinic acid and biocarbon electrode material. Corn stover was pretreated through hydrothermal process using 0.45 wt% K 2 CO 3 which removed 76 wt% lignin and 85 wt% xylan while preserving 83 wt% glucan. This was followed by acid hydrolysis to produce levulinic acid at varying H 2 SO 4 concentrations and reaction time in a batch reactor at 190 °C. At a reaction time of 5 min in 2 wt% H 2 SO 4 , 35.8 wt% and 30 wt% glucan in raw and pretreated corn stover was converted to levulinic acid, respectively. The residue from acid hydrolysis was converted into biocarbon for supercapacitor electrodes via a two-step thermal activation process which showed a specific capacitance of 120 F g -1 . The proposed integrated biorefinery concept provides multiple value-added products for a greater financial and environmental sustainability.

09 BIOMASS FUELS↗

Effects of 9.5 Years of Whole-Soil Warming on the Fatty Acid and n-Alkanes Composition in Bulk Soil and Density Fractions at Blodgett Experimental Forest, California, USA

Original data of molecular data (fatty acids and n-alkanes) including concentrations and calculated molecular proxies in a whole-soil warming experiment at the Blodgett Forest Research Station after 9.5 years of warming. The study site has a Mediterranean climate with annual average temperature of 12.5 ℃ and annual average precipitation of 1774 mm. The study site is characterized by a mesic Ultic Alfisol formed from granitic parent material, corresponding to a Dystric Cambisol under the World Reference Base for Soil Resources (WRB) classification system. Experimental warming is applied throughout the soil profile to a depth of 1 m using vertically embedded heating cables that raise soil temperature by 4 °C relative to ambient conditions. Soil samples were collected on 1 May 2023, after the experiment had been operating continuously for about 9.5 years since its initiation in January 2014.The data has been processed from raw data and cross-validated by other peers. The dataset includes: - Bulk_Fattyacid_9.5-year_Soil_Warming_Blodgett, California, USA: fatty acid concentrations and proxies including Carbon Preference Index (CPI) and Average Chain Length (ACL) of bulk soil organic carbon; - Fractions_Fattyacid_9.5-year_Soil_Warming_Blodgett, California, USA: fatty acid concentrations and proxies including CPI and ACL of free particulate organic matter (fPOM) and mineral-associated organic matter (MAOM); - Bulk_Alkanes_9.5-year_Soil_Warming_Blodgett, California, USA: n-alkanes concentrations and proxies including CPI and ACL of bulk soil organic carbon; - Fractions_Alkanes_9.5-year_Soil_Warming_Blodgett, California, USA: n-alkanes concentrations and proxies including CPI and ACL of fPOM and MAOM; - n-Alkanes_All_Monomer_Concentration_9.5-year_Soil_Warming_Blodgett, California, USA: concentration of all the n-alkane monomers identified and integrated for bulk soil, fPOM and MAOM; - Fattyacid_All_Monomer_Concentration_9.5-year_Soil_Warming_Blodgett, California, USA: concentration of all the fatty acid monomers including diacids identified and integrated for bulk soil, fPOM, and MAOM. All data are provided in CSV format and can be viewed using Microsoft Excel. We specifically look at fatty acids (FA) and n-alkanes in bulk soil, fPOM and MAOM and calculated molecular proxies such as CPI and ACL to understand the source of oragnic carbon (with ACL) and degree of decomposition (CPI) of each soil fraction. Due to lack of long-chain fatty acids (carbon number ⩾ 20), microorganism-derived organic carbon is characterized by shorter ACL in comparison to plant-derived organic carbon. Fresh SOC is characterized by even-over-odd dominance for fatty acids and odd-over-even dominance for n-alkanes. Therefore, CPI indicates whether soil organic carbon (SOC) represents fresh input (CPI > 10) or is strongly decomposed (close to 1). The research questions should be then, after 9.5-year warming: 1. whether the relative contribution between microorganism-derived and plant-derived SOC in each soil fraction? 2. whether fPOM became more decomposed whereas MAOM remained relatively persistent in each soil fraction across the soil depth?

Carbon↗

Selective sulfur removal from semi-dry flue gas desulfurization coal fly ash for concrete and carbon dioxide capture applications

High-sulfur mixed fly ash residues from semi-dry flue gas desulfurization units in coal-fired power plants are unsuitable for use as supplementary cementitious material (SCM) for concrete production or carbon dioxide utilization. In this work, we explore the potential for upcycling a representative spray dry absorber ash (10.44 wt% SO 3 ) into concrete-SCM by selective sulfur removal via weak acid dissolution while simultaneously exploring the possibility for CO 2 capture. Towards this effort, parametric studies varying liquid-to-solid ratio, acidity, and CO 2 pressure were conducted in a batch reactor to establish the sulfur removal characteristics in de-ionized water, nitric acid, and carbonic acid, respectively. The dissolution studies show that the leaching of sulfur from calcium sulfite hemihydrate, which is the predominant S phase, is rapid and achieves a concentration plateau within 5 min, and subsequently, appears to be controlled by the primary mineral solubility. Here, preferential S removal was sufficient to meet SCM standards (e.g., 5.0 wt% as per ASTM C618) using all three washing solutions with 0.62–0.72 selectivity (S^), defined as the molar ratio of S to Ca in the leachate, for a raw fly ash with bulk S^ = 0.3. Acid dissolution with 1.43 meq/g of ash or under 5 atm CO 2 retained > 18 wt% CaO and other Si-, Al-rich phases in the fly ash. Based on the experimental findings, two sulfur removal schemes were suggested for either integration with CO 2 capture and utilization processes using flue gas or to produce fly ash for use as a SCM.

01 COAL, LIGNITE, AND PEAT↗

White Beam Normalization

Raw data used to normalize detector performance on the ARCS instrument For the run cycle starting in June 2023. This is a V cylinder and the T0 chopper is set to 150 Hz and phased for 300 meV. All Fermi Choppers are out of the Beam.

MATERIALS SCIENCE↗

Corrosion-resistant polyurethane coatings from structure-homogenized biorefinery lignin through fractionation and oxypropylation

Using lignin for polyurethane (PU) synthesis is challenging because of its heterogeneous structure, i.e., broad molecule weight (MW) distribution and diverse hydroxyl (OH) functionality. This complexity influences the crosslinking reaction between lignin and isocyanate and affects the quality of PU products. Here, we propose a two-step strategy for lignin structure homogenization by lowering its MW and uniforming OH functionality (step 2). Step 1 involves a bioethanol fractionation process, yielding fractionated lignin with one order lower MW than the raw lignin while exhibiting better processability for the subsequent process. Step 2 is performed by an oxyalkylation process using fractionated lignin that converts phenolic and carboxylic OHs to aliphatic OHs. As a result, we obtained structure-homogenized lignin with good compatibility and crosslinking with hexamethylene diisocyanate for PU coating synthesis. Moreover, PU coatings prepared from structure-homogenized lignin display a defect-free microscopic structure and show better corrosion resistance than coatings fabricated from its raw lignin alternative. Overall, the structure homogenization process is a beneficial way of using lignin as biopolyol in PU synthesis toward the application-oriented design of corrosion-resistant lignin-based PU coatings.

36 MATERIALS SCIENCE↗

Microbiological and corrosion analysis of three urine pretreatment regimes with titanium 6A1-4V

One objective of the water recovery test (WRT) performed at NASA's Marshall Space Flight Center (MSFC) for the environmental control and life support systems (ECLSS) of Space Station Freedom is to determine the ability of the water recovery system to reclaim urine for crew reuse. In the process, raw urine is pretreated using a commercially available oxidant, Oxone (Dupont), and sulfuric acid (to reduce ammonia), and pumped into a urine processing subsystem. A combination of sodium hypochlorite and sulfuric acid were also considered as an alternative pretreatment. The ability of these pretreatments, plus a third pretreatment of ozone, to reduce microbial levels in urine generated during testing of the water recovery system at MSFC was examined. In addition, the corrosion rate of weld and base metal specimens of titanium 6A1-4V, a candidate material for the water system of Space Station Freedom, was monitored in the presence of these pretreatments. Specimen surfaces were examined at completion of the 21-day test using scanning electron microscopy. Change in pH, color, turbidity, and odor were recorded over the course of the test.

Huff, Timothy L.↗

Big Hill Geomechanical Analysis Using M-D Viscoplastic Material Model

The integrity of wellbores at the interbed between the caprock and salt is a serious concern in the Big Hill site. For the remediation and life extension of wellbores, more accurate predictions from the global model are needed. The Big Hill global model is improved using the M-D viscoplastic contact surface model and the mesh containing the interbed layer with contact surfaces between the salt and caprock layers, and fault blocks in overburden and caprock layers. The model calibration has been performed based on the cavern volumetric closures obtained from the Caveman calculations. The results agree well from 1991 to the early 2000s. The difference starts to widen after that, it might be because of frequent fluid movement and raw water injection. Therefore, the predictions from this improved model could be used to examine the structural integrity of caverns in Big Hill salt dome.

42 ENGINEERING↗

Software for Testing Electroactive Structural Components

A computer program generates a graphical user interface that, in combination with its other features, facilitates the acquisition and preprocessing of experimental data on the strain response, hysteresis, and power consumption of a multilayer composite-material structural component containing one or more built-in sensor(s) and/or actuator(s) based on piezoelectric materials. This program runs in conjunction with Lab-VIEW software in a computer-controlled instrumentation system. For a test, a specimen is instrumented with appliedvoltage and current sensors and with strain gauges. Once the computational connection to the test setup has been made via the LabVIEW software, this program causes the test instrumentation to step through specified configurations. If the user is satisfied with the test results as displayed by the software, the user activates an icon on a front-panel display, causing the raw current, voltage, and strain data to be digitized and saved. The data are also put into a spreadsheet and can be plotted on a graph. Graphical displays are saved in an image file for future reference. The program also computes and displays the power and the phase angle between voltage and current.

Moses, Robert W.↗

A Module Experimental Process System Development Unit (MEPSDU)

Design work for a photovoltaic module, fabricated using single crystal silicon dendritic web sheet material, resulted in the identification of surface treatment to the module glass superstrate which improved module efficiencies. A final solar module environmental test, a simulated hailstone impact test, was conducted on full size module superstrates to verify that the module's tempered glass superstrate can withstand specified hailstone impacts near the corners and edges of the module. Process sequence design work on the metallization process selective, liquid dopant investigation, dry processing, and antireflective/photoresist application technique tasks, and optimum thickness for Ti/Pd are discussed. A noncontact cleaning method for raw web cleaning was identified and antireflective and photoresist coatings for the dendritic webs were selected. The design of a cell string conveyor, an interconnect feed system, rolling ultrasonic spot bonding heat, and the identification of the optimal commercially available programmable control system are also discussed. An economic analysis to assess cost goals of the process sequence is also given.

Source record↗

Mars Mission Optimization Based on Collocation of Resources

This paper presents a powerful approach for analyzing Martian data and for optimizing mission site selection based on resource collocation. This approach is implemented in a program called PROMT (Planetary Resource Optimization and Mapping Tool), which provides a wide range of analysis and display functions that can be applied to raw data or imagery. Thresholds, contours, custom algorithms, and graphical editing are some of the various methods that can be used to process data. Output maps can be created to identify surface regions on Mars that meet any specific criteria. The use of this tool for analyzing data, generating maps, and collocating features is demonstrated using data from the Mars Global Surveyor and the Odyssey spacecraft. The overall mission design objective is to maximize a combination of scientific return and self-sufficiency based on utilization of local materials. Landing site optimization involves maximizing accessibility to collocated science and resource features within a given mission radius. Mission types are categorized according to duration, energy resources, and in-situ resource utilization. Optimization results are shown for a number of mission scenarios.

G E Chamitoff↗

Effect of Molding and Machining on Neoflon CTFE M400H Polychlorotrifluoroethylene Rod Stock and Valve Seat Properties

Since 1997 numerous fires have been reported to the Food and Drug Administration involving cylinder valves installed on medical use oxygen cylinders sold and operated within the United States. All of the cylinder valves in question had polychlorotrifluoroethylene (PCTFE) valve seats. Subsequent failure analysis showed that the main seat was the primary source of ignition. A review of the incidents involving cylinder valve fires indicated three possible ignition mechanisms: contaminant promotion, flow friction, and resonance. However, gas purity analysis showed that uncombusted, residual oxygen was within specification. Infrared and energy dispersive spectroscopy further showed that no contaminants or organic compounds were present in the remaining, uncombusted valve seat material or on seat plug surfaces. Therefore, contaminant-promoted ignition did not appear to be responsible for the failures. Observations of extruded material along the outer edge of the coined or loaded seat area produced by cylinder overuse or poppet overload led to concerns that accelerated gas flow across a deformed seat surface could generate enough localized heating to ignite the polymeric seat. Low molecular weight or highly amorphous quick-quenched PCTFE grades might be expected to be especially prone to this type of deformation. Such a failure mechanism has been described as flow friction; however, the corresponding mechanistic parameters are poorly understood. Subsequent revelation of low-temperature dimensional instability by thermomechanical analysis (TMA) in a variety of PCTFE sheet and rod stock samples led to new concerns that PCTFE valve seats could undergo excessive expansion or contraction during service. During expansion, additional extrusion and accompanying flow friction could occur. During contraction, a gap between the seal and adjacent metal surfaces could form. Gas flowing past the gap could, in turn, lead to resonance heating and subsequent ignition as described in ASTM Guide for Evaluation Nonmetallic Materials for Oxygen Service (G 63). Attempts to uncover the origins of the observed dimensional instability were hindered by uncertainties about resin grade, process history, and post-process heat history introduced by machining, annealing, and sample preparation. An approach was therefore taken to monitor property changes before and after processing and machining using a single, well-characterized lot of Neoflon CTFE.1 M400H resin. A task group consisting of the current PCTFE resin supplier, two molders, and four valve seat manufacturers was formed, and phased testing on raw resin, intermediate rod stock, and finished valve seats initiated. The effect of processing and machining on the properties of PCTFE rod stock and oxygen gas cylinder valve seats was then determined. Testing focused on two types of extruded rod stock and one type of compression-molded rod stock. To accommodate valve seat manufacturer preferences for certain rod stock diameters, two representative diameters were used (4.8 mm (0.1875 in.) and 19.1 mm (0.75 in.)). To encompass a variety of possible sealing configurations, seven different valve seat types with unique geometries or machining histories were tested. The properties investigated were dimensional stability as determined by TMA, specific gravity, differential scanning calorimetry (DSC), compressive strength, zero strength time, and intrinsic viscosity. Findings are discussed in the context of polymer structure-process-property relationships whenever possible.

Waller, Jess M.↗

Some aspects of space propulsion with extraterrestrial resources

Extraterrestrial resources for space processing of chemicals, in general, and propellants, in particular, are explored quantitatively. It is seen that, for several candidate space mission scenarios, space processing of both space resources and earth-carried resources can make decisive differences in the mission success for a given payload. To fix ideas and demonstrate trends, the specific case of water splitting to extract oxygen, discard (or use without storage) the resulting hydrogen, and burn earth-carried noncryogenic liquid fuel(s) in a simple rocket motor, designed for periodic thrusting, is treated in some detail. Experimental hardware is assembled and demonstrated to perform adequately, besides showing compactness of the space-packaged 'capsule' module that is self-contained. Building upon previous studies, the concept of in situ propellant production (ISPP) is reexamined in light of more recent energy and materials technologies. Missions to comets and Mars Sample Return are mentioned as candidate scenarios. The mission duration, reliability-repairability of hardware, resource availability in low earth orbit (LEO), and the thrust requirements are considered in turn. It is seen that space storage of hydrogen for extended durations (5-10 years) involves problems that require detailed studies, besides involving many presently unanswered issues. A study of the energy option in LEO and in deep space is developed in simple terms. The different solar, radioisotope, and nuclear power sources are mentioned. Storage and handling of raw and processed chemicals are considered.

Ramohalli, Kumar↗

Using real-time data analysis to conduct next-generation synchrotron fatigue studies

Next-generation experimental techniques, like high energy X-ray diffraction microscopy (HEDM), usher in new opportunities to collect the grain-scale data necessary for understanding the evolving processes that drive fatigue failure. In this study, we present a framework for monitoring the evolution of a deforming polycrystal, in real-time, by applying principal component analysis (PCA) to raw X-ray diffraction image data. We applied this framework to inform in-situ HEDM measurements of a cyclically loaded Inconel-718 superalloy. Further, we discovered correlations between PCA of the diffraction data and the physical processes in the polycrystal. Lastly, we discuss extending this framework in future HEDM fatigue studies.

36 MATERIALS SCIENCE↗

Graphite Oxidation Rate Study on ET-10 and ETU-10 Grades - Task 4: QA Support and Testing for Structural Graphite Oxidation

INL performed targeted oxidation tests to measure oxidation rates for samples of ET-10 and ETU-10 graphite under CRADA No. 21CRA22 Mod. 3, Annex A, “Tritium Testing to Support Kairos Power Advanced Reactor Demonstration” (04/02/2024). All testing was conducted within INL’s Carbon Characterization Laboratory (CCL) using test standard ASTM D7542-21 "Standard Test Method for Air Oxidation of Carbon and Graphite in the Kinetic Regime" [ASTM International, 2021]. Kairos Power provided all test specimens through its graphite vendor Ibiden, Inc. to INL and ASTM specimen specified dimensions. Information within this report only provides the Arrhenius oxidation rate plots as a function of temperature for each graphite grade tested. The raw mass loss per time data will be provided on the Nuclear Data Management and Analysis System (NDMAS) portal located on the INL information system.

36 MATERIALS SCIENCE↗

Update on Apollo Data Restoration by the NSSDC and the PDS Lunar Data Node

The Lunar Data Node (LDN) , under the auspices of the Geosciences Node of the Planetary Data System (PDS) and the National Space Science Data Center (NSSDC), is continuing its efforts to recover and restore Apollo science data. The data being restored are in large part archived with NSSDC on older media, but unarchived data are also being recovered from other sources. They are typically on 7- or 9-track magnetic tapes, often in obsolete formats, or held on microfilm, microfiche, or paper documents. The goal of the LDN is to restore these data from their current form, which is difficult for most researchers to access, into common digital formats with all necessary supporting data (metadata) and archive the data sets with PDS. Restoration involves reading the data from the original media, deciphering the data formats to produce readable digital data and converting the data into usable tabular formats. Each set of values in the table must then be understood in terms of the quantity measured and the units used. Information on instrument properties, operational history, and calibrations is gathered and added to the data set, along with pertinent references, contacts, and other ancillary documentation. The data set then undergoes a peer review and the final validated product is archived with PDS. Although much of this effort has concentrated on data archived at NSSDC in the 1970's, we have also recovered data and information that were never sent to NSSDC. These data, retrieved from various outside sources, include raw and reduced Gamma-Ray Spectrometer data from Apollos 15 and 16, information on the Apollo 17 Lunar Ejecta And Meteorites experiment, Dust Detector data from Apollos 11, 12, 14, and I5, raw telemetry tapes from the Apollo ALSEPs, and Weekly Status Reports for all the Apollo missions. These data are currently being read or organized, and supporting data is being gathered. We are still looking for the calibrated heat flow data from Apollos 15 and 17 for the period 1975-1977, any assistance or information on these data would be welcome. NSSDC has recently been tasked to release its hard-copy archive, comprising photography, microfilm, and microfiche. The details are still being discussed, but we are concentrating on recovering the valuable lunar data from these materials while they are still readily accessible. We have identified the most critical of these data and written a LASER proposal to fund their restoration. Included in this effort are data from the Apollo 15 and 16 Mass Spectrometers and the Apollo 17 Par-UV Spectrometer and ancillary information on the Apollo 17 Surface Electrical Properties Experiment.

Williams, David R.↗