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DOE OSTI2021

Spontaneous rearrangement of acetylated xylan on hydrophilic cellulose surfaces

The interaction of xylan, an abundant plant polysaccharide, with cellulose microfibrils is essential for secondary cell wall strength. A deeper understanding of these interactions is crucial both to improve our understanding of plant cell wall architecture and to design alternate strategies to overcome cellulose recalcitrance for the production of biofuels and sustainable biomaterials. Naturally occurring acetate or glucuronic acid substitutions on xylan have been shown to influence xylan-cellulose interactions. In this work, we use unrestrained molecular dynamics simulations to determine the interactions with the (110) hydrophilic face of cellulose fibers of four different xylans. In the absence of cellulose, all xylans, independent of the substitution pattern, adopt a highly flexible threefold helical screw conformation. However, when xylan is spatially close to a cellulose surface 1,2 linked acetyl xylans (2AcX) adopt rigid twofold helical screw conformations. The 2AcX conformations are primarily stabilized by interactions between the acetylated oxygen and the glycosidic linkage with C-O6 of cellulose. In contrast, the glycosidic oxygens and acetyl decorations for 1,3 linked acetyl groups (3AcX) are oriented away from the cellulose surface and the 3AcX xylans maintain threefold helical screw conformations on the cellulose surface. Our results show that evenly spaced chemical functionalization (with acetyl groups) and the position of substitution (1,2) on xylan backbone play key roles in tuning the xylan-cellulose interactions to stabilize the twofold helical screw conformations of xylan on the cellulose surface. A comparison with previous experimental findings further suggests that 1,2 substitutions induce twofold helical screw conformations of xylan on the cellulose surface irrespective of the chemical nature of the substituent, while 1,3 substitutions primarily bind lignin in threefold helical screw conformations rather than cellulose in plant cell walls.

1,2 Ac↗

NASA NTRS2001

Use of a Multiwavelength Pyrometer in Several Elevated Temperature Aerospace Applications

A multiwavelength pyrometer was developed for applications unique to aerospace environments. It was shown to be a useful and versatile technique for measuring temperature, even when the emissivity is unknown. It has also been used to measure the surface temperatures of ceramic zircomia thermal barrier coatings and alumina. The close agreement between pyrometer and thin film thermocouple temperatures provided an independent check. Other applications of the multiwavelength pyrometer are simultaneous surface and bulk temperature measurements of a transparent material, and combustion gas temperature measurement using a special probe interfaced to the multiwavelength pyrometer via an optical fiber. The multiwavelength pyrometer determined temperature by transforming the radiation spectrum in a broad wavelength region to produce a straight line (in a certain spectral region), whose intercept in the vertical axis gives the temperature. Implicit in a two-color pyrometer is the assumption of wavelength independent emissivity. Though the two data points of a two-color pyrometer similarly processed would result immediately in a similar straight line to give the unknown temperature, the two-color pyrometer lacks the greater data redundancy of the multiwavelength pyrometer, which enables it to do so with improved accuracy. It also confirms that emissivity is indeed wavelength independent, as evidenced by a multitude of the data lying on a simple straight line. The multiwavelength pyrometer was also used to study the optical transmission properties of a nanostructured material from which a quadratic exponential functional frequency dependence of its spectral transmission was determined. Finally, by operating the multiwavelength pyrometer in a very wide field of view mode, the surface temperature distribution of a large hot surface was obtained through measurement of just a single radiation spectrum.

Ng, Daniel↗

NASA NTRS2003

Graphite/Ultra-High Modulus Polyethylene Hybrid Fiber Composites with Epoxy and Polyethylene Matrices for Cosmic Radiation Shielding

One of the most significant technical challenges in long-duration space missions is that of protecting the crew from harmful radiation. Protection against such radiation on a manned Mars mission will be of vital importance both during transit and while on the surface of the planet. The development of multifunctional materials that serve as integral structural members of the space vehicle and provide the necessary radiation shielding for the crew would be both mission enabling and cost effective. Additionally, combining shielding and structure could reduce total vehicle mass. Hybrid laminated composite materials having both ultramodulus polyethylene (PE) and graphite fibers in epoxy and PE matrices could meet such mission requirements. PE fibers have excellent physical properties, including the highest specific strength of any known fiber. Moreover, the high hydrogen (H) content of polyethylene makes the material an excellent shielding material for cosmic radiation. When such materials are incorporated into an epoxy or PE matrix a very effective shielding material is expected. Boron (B) may be added to the matrix resin or used as a coating to further increase the shielding effectiveness due to B s ability to slow thermal neutrons. These materials may also serve as micrometeorites shields due to PE s high impact energy absorption properties. It should be noted that such materials can be fabricated by existing equipment and methods. It is the objective of this work therefore to: (a) perform preliminary analysis of the radiation transport within these materials; (b) fabricate panels for mechanical property testing before and after radiation exposure. Preliminary determination on the effectiveness of the combinations of material components on both shielding and structural efficiency will be made.

Source record↗

DOE OSTI2026

Synergistic cellulase–xylanase formulations for enhanced dewatering and fiber bonding toward energy-efficient and sustainable paper and packaging production

A mechanistic understanding of the synergistic effects of enzymes on cellulosic fibers dewatering and fiber bonding is essential for advancing energy-efficiency and lightweight production of paper and packaging materials. This study investigates the impact of varying cellulase and xylanase formulations on equilibrium moisture content (EMC) after pressing and tensile strength of cellulosic fiber webs using a factorial experimental design. Nine custom enzyme formulations were evaluated at controlled dosages ranging from ∼20 to 76 FPU/mL cellulase and ∼500–1130 IU/mL xylanase. Response surface modeling revealed a significant synergy, particularly at 20–40 FPU/mL cellulase combined with ≥ 1000 IU/mL xylanase. Under these conditions, EMC decreased by up to 3.6% compared with the untreated refined control, while tensile index gains of up to 16% were statistically significant for optimized blends (p < 0.05). The interaction between cellulase and xylanase was also significant for the tensile response (p = 0.010). Protein efficiency analysis showed that optimized formulations containing 30–40% less protein outperformed the commercial benchmark. The nonlinear synergy between cellulase and xylanase is attributed to their complementary substrate specificities. Endoglucanase- and β‑glucosidase‑rich cellulases hydrolyze internal β‑1,4‑glycosidic bonds in amorphous cellulose, loosening fiber walls and increasing flexibility, while xylanases target hemicellulose, primarily xylan-rich domains, enhancing porosity and improve cellulase accessibility. Tailoring enzyme formulations at low loadings overcomes traditional trade-offs between strength and dewatering, enabling cost-effective, energy-efficient, low-carbon solutions for sustainable packaging and hygiene products.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2022

Spray coating for washout tooling by binder jet additive manufacturing

We report washout tooling is a process in which a removable mold or fixture is disintegrated using a solvent. Binder Jet (BJ) additive manufacturing holds promise for creating customized washout molds from common materials. BJ-based washout tooling provides an advanced strategy in manufacturing fiber-reinforced composites (FRCs), especially for customized hollow FRCs. However, washout tools formed by BJ require an impermeable barrier between the porous tooling surface and the parts laid up on the surface to prevent the resin from infiltrating the tooling surface and bonding the tool to the FRC. The conventional method for preventing resin migration into the washout mold from the FRC is winding Teflon® tape over the entire surface, which is labor-intensive and very difficult to deploy for specific geometries. Here, we report the development of a polymer spray coating method to seal the tooling surface and prevent resin infiltration without affecting the washout properties needed for sacrificial tooling. Two water-soluble polymers, poly(sodium 4-styrenesulfonate) (PSS–Na) and poly(vinylsulfonic acid, sodium salt) (PVS–Na), were investigated for spray coating. PVS-Na maintained tighter geometric tolerances and provided excellent thermal stability with the onset of decomposition at 320 °C and glass transition temperature of 280 °C. Spray coating with PVS-Na streamlines the process of forming a protective layer for the washout molds by BJ, reduces migration of the resins from the FRC, and significantly improves the production efficiency of complex washout tools.

42 ENGINEERING↗

DOE OSTI2023

Structure and dynamics of ILs-based gel polymer electrolytes and its enhanced conductive properties with the incorporation of Al 2 O 3 nanofibers

Here, this work reports the enhanced mobility of ions in ionic liquid (IL)-based gel polymer electrolytes (GPEs) with the incorporation of Al 2 O 3 nanofibers. A combination of PVDF-HFP, EMIMTFSI and LiTFSI with 3 wt% Al 2 O 3 nanofibers has been prepared through solution casting technique. The room temperature ionic conductivity of PVDF-HFP: ILs electrolyte (45:55, weight ratio of 0.82) (GPE) is found to be 2.7 × 10 –5 S cm –1 , which increases up to 7.8 × 10 –5 S cm –1 in Al 2 O 3 containing GPE (Al-GPE). Pulsed field gradient (PFG) NMR results validate the increased ionic conductivity observed in Al-GPE. We found that the diffusivity of Li + , TFSI – and EMIM + increases when Al 2 O 3 nanofibers are well-distributed in the GPE matrix. The surface morphology and the amorphicity of GPEs are examined through SEM and XRD analyses. Lastly, the local structure of Al 2 O 3 fibers and the molecular-level interactions of ions with polymer, and their effect on the diffusivity of ions are established through solid-state NMR detecting 27 Al, 1 H, 13 C, 19 F nuclei including 2D 13 C{ 1 H} HETCOR NMR experiments. The 13 C DPMAS and CPMAS experiments highlight the dynamic heterogeneity associated with the ions that are embedded in the rigid and the mobile phase of GPEs. While some of the ionic species strongly interact with polymer chains in the rigid environment, the majority of them reside in the mobile phase and contribute to the overall increased conductivity. Most importantly, Al 2 O 3 nanofibers significantly affect the dynamics of ionic species that are present in the mobile phase between the polymer chains.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2026

Insights from a coupled thermo-hydro-mechanical analysis of a layered high-temperature thermal energy storage reservoir

Coupled thermal-hydraulic-mechanical (THM) modeling is applied to investigate the performance of a seasonal high-temperature aquifer thermal energy storage operation based on data and conditions from current site investigations at the Geostorage Forsthaus pilot project in Bern (Switzerland). The model includes subhorizontal sand lenses of various lengths and dips that are embedded in a low permeability clay matrix. Thermal energy storage is simulated by seasonal injection and withdrawal of hot (up to 90 °C) water from a main well, with reservoir pressure regulated by two auxiliary wells at a distance of about 70 m from the main well. The results show how targeted injection into deeper permeable storage formations, along with active deep well pressure control, can effectively minimize geomechanical impact and the potential risk of damaging subsurface storage and sealing formations, or even surface facilities. With such pressure control, the subsurface mechanical responses are dominated by thermal strain and stress, which can be monitored with subsurface fiber optics. The study demonstrates how coupled THM modeling can be applied for the design of a safe and efficient thermal energy storage operation, and how subsurface fiber optic monitoring can be applied for performance confirmation, allowing for more confident operational forecasting.

Rutqvist, Jonny↗

DOE OSTI2020

Light-Controlled Nanoparticle Collision Experiments

Electrochemical monitoring of catalytically amplified collisions of individual metal nanoparticles (NP) with ultramicroelectrodes (UME) has been extensively used to study electrocatalysis, mass-transport, and charge-transfer processes at the single NP level. More recently, photoelectrochemical collision experiments were carried out with semiconductive NPs. Here we introduce two new types of light-controlled nano-impact experiments. The first experiment involves localized photodeposition of catalyst (Pt) on TiO 2 NPs with a glass-sheathed carbon fiber simultaneously serving as the light guide and collector UME. The collisions of in situ prepared Pt@TiO 2 NPs with the carbon surface produced blips of water oxidation current, while the activity of pristine TiO 2 NPs was too low to yield measurable signal. In another experiment, collisions of catalytic (Ir oxide) NPs with the semiconductor (Nb doped n-type TiO 2 rutile single crystal) electrode are monitored by measuring the photocurrent of water oxidation.

14 SOLAR ENERGY↗

DOE OSTI2024

Tailoring Nanoporous Silica and Natural Straw Structural Insulation Composites

Nanoporous silica exhibits ultralow thermal conductivity as a result of its nanoscale pore size, high pore volume, and specific surface area. In this study, we report the self-assembled surfactant-templated synthesis of nanoporous silica, which is integrated with cellulose fibers derived from natural straw to manufacture high thermal insulation and mechanically robust nanocomposites. The nanocomposite shows a low thermal conductivity of 22.5 mW/(m·K), a compressive modulus of 0.93 MPa, and a hydrophobicity with a water contact angle of 125°. Moreover, we observed a marked reduction in water absorption capacity and a carbon footprint of 0.21 kg CO 2 equiv/kg. Here, this study provides a pathway toward the development of nanoporous structural insulation materials for energy-efficient building applications.

36 MATERIALS SCIENCE↗

NASA NTRS1983

Analysis and acoustooptical measurements of bulk and surface acoustic wave fields

The development of multielement ultrasonic transducers having full field amplitude and phase control is discussed. In addition, the measurement of the surface particle displacement caused by an idealized impulse load on the surface, the three dimensional mapping of acoustic fields using optical scanning techniques, and the measurement of two dimensional stress distributions using embedded optical fiber sensors are addressed.

Claus, R. O.↗

NASA NTRS1988

Predicting impact induced delaminations in composite plates

A method is presented which can be used to estimate the dimensions of delaminations in fiber reinforced composite plates impacted by a solid object. The impact occurs at low velocity such that the impactor does not penetrate the surface of the plate. Comparisons between measured and calculated delamination lengths and widths are given. The use of the method in the design of impact resistant plates is discussed.

Wu, Hsi-Yung T.↗

NASA NTRS1989

A detailed investigation of the micromechanisms of compressive failure in open hole composite laminates

Micromechanisms responsible for compressive failure in open-hole composite laminates were investigated. Specimens containing circular center holes were loaded in compression to failure at a slow rate, and the surface damage development during loading was monitored. Several coupon compression tests were interrupted prior to catastrophic failure to allow for the assessment of fiber shear crippling and/or fiber microbuckling by NDE techniques. From these sectioning studies, the extent and mode of failure were determined, and a three-dimensional schematic of the shear crippling zone was developed. Results show that the majority of the damage in compression-loaded open-hole composite laminates is shear crippled or microbuckled 0-deg fibers; in many cases, however, the shear crippling damage within the 0-deg plies produced shear strains and damage in the adjacent off-axis plies.

Guynn, E. Gail↗

NASA NTRS1990

Radial Profilometry

Radial profilometry is combination of optical and electronic techniques for measurement of inner surfaces of cylindrical or nearly cylindrical cavities. Profilometer inserted in pipe or other cavity to measure its shape optically. Illumination supplied through optical fiber, and image of inspected area of cavity transmitted through bundle of optical fibers. Applications include inspection of pipes, tubes, boreholes, and possibly measurements of contours in blood vessels or other internal organs.

Gilbert, J. A.↗

NASA NTRS1998

Scaling up the Single Transducer Thickness-Independent Ultrasonic Imaging Method for Accurate Characterization of Microstructural Gradients in Monolithic and Composite Tubular Structures

Ultrasonic velocity/time-of-flight imaging that uses back surface reflections to gauge volumetric material quality is highly suited for quantitative characterization of microstructural gradients including those due to pore fraction, density, fiber fraction, and chemical composition variations. However, a weakness of conventional pulse-echo ultrasonic velocity/time-of-flight imaging is that the image shows the effects of thickness as well as microstructural variations unless the part is uniformly thick. This limits this imaging method's usefulness in practical applications. Prior studies have described a pulse-echo time-of-flight-based ultrasonic imaging method that requires using a single transducer in combination with a reflector plate placed behind samples that eliminates the effect of thickness variation in the image. In those studies, this method was successful at isolating ultrasonic variations due to material microstructure in plate-like samples of silicon nitride, metal matrix composite, and polymer matrix composite. In this study, the method is engineered for inspection of more complex-shaped structures-those having (hollow) tubular/curved geometry. The experimental inspection technique and results are described as applied to (1) monolithic mullite ceramic and polymer matrix composite 'proof-of-concept' tubular structures that contain machined patches of various depths and (2) as-manufactured monolithic silicon nitride ceramic and silicon carbide/silicon carbide composite tubular structures that might be used in 'real world' applications.

Roth, Don J.↗

NASA NTRS1998

A Novel Ultrasonic Method for Characterizing Microstructural Gradients in Tubular Structures

Ultrasonic velocity and time-of-flight (TOF) imaging that uses back surface reflections to gage volumetric material quality is highly suited for quantitative characterization of microstructural gradients including those due to pore fraction, density, fiber fraction, and chemical composition variations. However, a weakness of conventional pulse echo ultrasonic velocity and TOF imaging is that the image shows the effects of thickness as well as microstructural variations, unless the part is uniformly thick. This limits this imaging method's usefulness in practical applications. Prior studies have described a pulse echo TOF based ultrasonic imaging method that requires using a single transducer in combination with a reflector plate placed behind samples which, eliminates the effect of thickness variation in the image. In those studies, this method was successful at isolating ultrasonic variations due to material in plate like samples of silicon nitride, metal matrix composite, and polymer matrix composite. In this study, the method is engineered for inspection of more complex shaped structures- those having (hollow) tubular or curved geometry. The experimental inspection technique and results are described as applied to a polymer matrix composite "proof of concept" tube that contains machined patches of various depths and an as manufactured monolithic silicon nitride ceramic tube that might be used in "real world" applications.

Roth, Don J.↗

NASA NTRS1999

A Particulate Matter

Technical Applications Unlimited, through a contract with Kennedy Space Center, developed the an activity sensor, called the TAU- N100A, which includes a microprocessor-controlled module that detects a particular on a sensor surface and converts this information into digital data. Its original purpose for development was to detect the accumulation of potentially damaging dust and fibers on sensitive payload components.

Source record↗

NASA NTRS2008

Modeling Ablation of Fibrous Materials from Bulk to Knudsen Regime

Material-environment interactions are analyzed at microscopic scale to explain the lower than expected density observed by post-flight analysis of the char layer on the Stardust shield. Mass transfer, ablation (oxidation), and surface recession of fibrous material is simulated in 3D using a Monte-Carlo simulation tool. Ablation is found to occur either at the surface or in volume depending on Knudsen and Thiele number values. This study supports the idea of volume ablation followed by possible carbon fiber spallation that may explain post-flight analyses.

Lachaud, Jean↗

NASA NTRS2012

Open Circuit Resonant (SansEC) Sensor for Composite Damage Detection and Diagnosis in Aircraft Lightning Environments

Composite materials are increasingly used in modern aircraft for reducing weight, improving fuel efficiency, and enhancing the overall design, performance, and manufacturability of airborne vehicles. Materials such as fiberglass reinforced composites (FRC) and carbon-fiber-reinforced polymers (CFRP) are being used to great advantage in airframes, wings, engine nacelles, turbine blades, fairings, fuselage and empennage structures, control surfaces and coverings. However, the potential damage from the direct and indirect effects of lightning strikes is of increased concern to aircraft designers and operators. When a lightning strike occurs, the points of attachment and detachment on the aircraft surface must be found by visual inspection, and then assessed for damage by maintenance personnel to ensure continued safe flight operations. In this paper, a new method and system for aircraft in-situ damage detection and diagnosis are presented. The method and system are based on open circuit (SansEC) sensor technology developed at NASA Langley Research Center. SansEC (Sans Electric Connection) sensor technology is a new technical framework for designing, powering, and interrogating sensors to detect damage in composite materials. Damage in composite material is generally associated with a localized change in material permittivity and/or conductivity. These changes are sensed using SansEC. Unique electrical signatures are used for damage detection and diagnosis. NASA LaRC has both experimentally and theoretically demonstrated that SansEC sensors can be effectively used for in-situ composite damage detection.

Wang, Chuantong↗