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DOE OSTI2026

Citric Acid Functionalized Natural Fibers to Enhance Thermal Stability and Moisture Resistance in Polylactic Acid Composites

Cellulosic fibers can impart many unique benefits into composite applications, such as reduced weight or structural reinforcement; however, these materials also increase hygroscopicity and decrease thermal stability, restricting broader applications. The present work adapted an experimental process for functionalizing the cellulose surface using citric acid (CA) for three fibers: a 100% cellulose bleached soft Kraft pulp (e.g., creafill) and two natural fibers with similar composition but different fiber morphology, flax fiber and banana fiber. The process uses CA with a sodium hypophosphite (SHP) catalyst to chemically functionalize fiber surfaces, and the reaction mechanism was investigated through Fourier Transform Infrared Spectroscopy (FTIR), which suggested a grafting mechanism rather than a surface-based crosslinking between neighboring sites. Functionalized fibers were compounded into polylactic acid (PLA) at 20 wt.% to better understand how this functionalization might impact critical performance properties like thermal stability, crystallization, thermal mechanical properties, and water uptake of these composites. The study demonstrated varying levels of efficacy for the functionalization of cellulosic fibers with CA/SHP and the fiber with the most open microstructure, e.g., banana fiber, exhibited the largest change in its properties with a 38% reduction in water uptake compared to untreated banana fiber composites. Parallel evaluation of the functionalization process for different fibers demonstrates the importance of fiber morphology on surface modification and can enable their use in composites by demonstrating the efficacy of this potentially low-cost, low-toxicity method for reducing hygroscopicity and improving thermal stability.

citric acid↗

DOE OSTI2025

Evaluation of desiccation cracking characteristics of inorganic micro-fiber-reinforced engineered barrier material (IMEBM) for geological repository

Abstract Buffer material is crucial for the engineering barrier system to dispose of high-level radioactive waste in a geological repository. A reliable buffer material should be able to maintain good sealing characteristics and minimize desiccation cracking. In this study, the effectiveness of inorganic fiber-reinforced engineering barrier material in reducing desiccation cracks in bentonite was evaluated via desiccation tests, image analysis, and air permeability tests. The effects of fiber type (E-glass fiber and basalt fiber) and fiber content (0.0%, 0.5%, 1.0%, 1.5%, 3.0%, and 5.0% of dry weight of the bentonite) on the development of desiccation cracks in the fiber–bentonite mixtures with the same given initial moisture content were evaluated. The results indicated that the addition of fibers could significantly reduce the crack size and area in bentonite during the drying. Basalt fibers showed a slightly better reinforcement effect than E-glass fibers when the fiber content was lower than 3.0%. The addition of fibers prevented the development of penetrating cracks and significantly reduced the permeability of the bentonite after drying. The permeabilities of basalt fiber- and E-glass fiber-reinforced bentonite composites with 3% reinforcement were 5.81 × 10 –11 m 2 and 7.24 × 10 –11 m 2 , respectively, which were 64 and 51 times smaller than that of pure bentonite. X-ray–CT observation of the internal structure of the samples after drying showed that the addition of fibers significantly changed the crack morphology and potentially increased the tortuosity.

Feng, Yuan↗

DOE OSTI2026

Development Fiber Optic Distributed System for Direct Detection of Subsurface Gases Leakages

Carbon, natural gas, and hydrogen gas storage is an emerging solution to safeguard us against pollution, support goals of negative carbon emission, and protect sources of renewable energy. Properly constructed storage wells provide a virtually impervious barrier to any unintended subsurface transmission. The ability to ensure the long-term integrity of such wells is vital to the success of any storage operation and be successful in the public eyes. Therefore, robust monitoring of any gas migration into the subsurface is highly sought. A fiber-optic distributed chemical sensor (DCS) enables monitoring of long-term well integrity along its depth, ensuring the success of any storage operation and bolsters public acceptance of the safety of the reservoir via leak early detection. The same technique can be applied to gas monitoring in pipeline networks and nuclear stockpile monitoring applications. Fiber based Raman spectroscopy enables DCS, as optical fibers can be deployed in virtually any environment and relay spectroscopic information over long distances back to the user. Hollow core fibers (HCF) make excellent DCSs as the air core of the fiber allows gas from the environment to diffuse into the core, which interacts with the laser signal that is carried in the air core. This work builds upon the previous LDRD project, Fiber Optic System for Direct Detection of Carbon Dioxide Leakage in Carbon Storage Wells (21-FS-003), in which the feasibility of Raman spectroscopy detection of Carbon Dioxide (CO2) in HCF detection was demonstrated. We mitigated the risk of this DCS technology by establishing and completing five objectives. The first objective was to model and optically characterize HCF uptake of CO2, establishing the relationship between HCF length, gas diffusion time, detectable gas concentration, and measured Raman intensity. In objective two, we developed a fiber core drilling recipe to enable additional diffusion ports in the fiber core and established a method for maintaining fiber strength and integrity post drilling. Objective three characterized the drilled fibers against the undrilled fibers, establishing the differences in the gas mechanics and optical properties and provided parameters to iterate the drilling process. In objective four, a fusion splicing technique was developed to join the HCF to conventional single-mode fibers, localizing the gas detection point at the drilled HCF hole, emulating a DCS. Lastly, objective five was the testing of the sensor in Edgar Mines at Colorado School of Mines on a CO2 pipeline with a simulated leak, to showcase the ability to detect CO2 leaks. This capstone result showed CO2 leak detection in < 10 minutes, raising the technology readiness level of HCF segments as deployable DCS.

organic↗

DOE OSTI2026

Hybrid Bio-Based Composites: Enabling Cellulose Nanofiber (CNF) Incorporation into Composites via Macroscale Natural Fiber Carriers

Cellulose nanofibers (CNFs) have significant potential in composites as additives to improve mechanical properties, melt rheology, and more. However, agglomeration of CNFs is a key challenge in composite melt processing as obtaining nano-level dispersion of CNFs often requires cost- and energy-intensive processes (e.g., solvent exchange or freeze drying) due to the strong hornification tendencies of CNF. Herein, we avoid these challenges by using a natural fiber carrier method to integrate CNF into thermoplastic composites. Fibers are co-dried to create a hybrid fiber feedstock for compounding in which natural fibers are decorated with dispersed nanofibers. The hybridized fibers result in up to a 24% increase in tensile strength and up to a 35% increase in Young’s modulus compared to composites only containing natural fibers. The lignocellulosic nanofibers are found to outperform their purely cellulosic counterpart, which is theorized to be due to either an increased propensity for fibrillation of the lignocellulosic fibers or the increased hydrophobicity of the fibers due to the presence of lignin. Surface analysis of fiber feedstocks, via streaming potential measurements and dynamic light scattering (DLS), confirmed a significant change in the feedstock hydrophobicity before and after hybridization. While mild additions of CNF (1 wt.% on the macroscale fiber) do not impact the composite melt viscosity, the viscosity is found to increase at higher CNF loadings (5 wt.% on the macroscale fiber), indicating its utility as a rheology modifier. Lastly, use of these materials as novel feedstocks for medium-scale additive manufacturing in high-fidelity part production was demonstrated.

bio-based↗

DOE OSTI2025

Sizing of discontinuous natural fibers: Effect of sizing approach and sizing concentration on composite properties

Natural fiber reinforced composites (NFRCs) are gaining attention in automotive applications as an alternative to glass fiber composites due to their lightweight and renewable sourcing. However, the inherent hydrophilicity of natural fibers leads to poor compatibility with hydrophobic polymers which adversely affects the mechanical properties of the composites and can limit their application to non-structural parts. Sizing is a common approach used for synthetic fibers to improve the interface between fiber and matrix. However, there is limited study on the sizing of natural fibers, and hence the focus of this work. Here, in this study, two different approaches to sizing discontinuous coir fibers were investigated, namely; (1) ex-situ sizing and (2) in-situ sizing. A commercial polypropylene (PP) based sizing agent was used and the effects of varying sizing solution concentrations (1.5, 2.5, and 3.5 wt%) on the properties of the composites was studied. Results showed that composites prepared via the in-situ sizing process had better fiber–matrix adhesion and improved tensile properties compared to ex-situ sized composites. On studying the effect of different sizing concentrations on composite properties, we found that the tensile strength of the composites increased (by ∼ 42 %) up to 2.5 wt% sizing concentration (in solution) and then decreased. However, the impact strength decreased significantly on increasing the sizing content beyond 1.5 wt% (by ∼ 40 %). Additionally, the study was further extended to investigate the effect of sizing on different NFRCs (coir, banana, and cottonized hemp fiber) where effectiveness of sizing was found to be influenced by the fiber surface morphology.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Scale up production of carbon fibers from petroleum mesophase pitch

This work investigates the scale-up of pitch precursors for the carbon fiber market using mesophase pitch formulated and produced by Advanced Carbon Products Technologies’ (ACPT’s) patented mesophase pitch processing technology. Through use of its patented process, ACPT developed strategic materials by converting petroleum-based pitch into a high-value, low-cost, carbon-rich feedstock for carbon fiber and other materials critical to our national security. The team successfully developed processing criteria for the tailored mesophase pitch material that can be processed further into precursor and carbon fiber. Processability of the mesophase pitch into precursor and carbon fiber was demonstrated at scale. The resulting materials sequester the carbon that would otherwise be burned and released into the atmosphere, making this an environmentally friendly way to produce these materials in the United States.Pitch-based carbon fibers offer a promising pathway toward cost-effective, high-performance materials for structural and high-modulus composite applications; however, adoption has been limited by challenges in precursor processability and scale-up. In this work, tailored isotropic and mesophase petroleum-derived pitch materials were developed and evaluated for precursor and carbon fiber production through a collaborative effort between Oak Ridge National Laboratory (ORNL) and ACPT. Processing conditions were established at ORNL’s Carbon Fiber Technology Facility to enable stable melt-blowing of pitch-based precursors under continuous operation. Mesophase pitch precursor fibers were produced following oxidation and carbonization, corresponding to a diameter shrinkage of approximately 12%–13% and an estimated mass yield of about 75%–80%. Continuous melt-blowing steady-state operation was demonstrated over time, indicating robust process stability. Melt-blowing was achieved at throughput rates of approximately 20 lb/h⁻¹, validating the commercial viability of petroleum-derived pitch feedstocks for fiber production. Further studies are required to tailor carbon fiber microstructure and properties for specific composite applications.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2024

Fiber Sorbents – A Versatile Platform for Sorption-Based Gas Separations

Increasing demand for high-purity fine chemicals and a drive for process intensification of large-scale separations have driven significant work on the development of highly engineered porous materials with promise for sorption-based separations. While sorptive separations in porous materials offer energy-efficient alternatives to longstanding thermal-based methods, the particulate nature of many of these sorbents has sometimes limited their large-scale deployment in high-throughput applications such as gas separations, for which the necessary high feed flow rates and gas velocities accrue prohibitive operational costs. These processability limitations have been historically addressed through powder shaping methods aimed at the fabrication of structured sorbent contactors based on pellets, beads or monoliths, commonly obtained as extrudates. These structures overcome limitations such as elevated pressure drops commonly recorded across powder adsorption beds but often accrue thermal limitations arising from elevated particle density and aggregation, which ultimately cap their maximum separation performance. Furthermore, the harsh mechanical strain to which powder particles are subjected during contactor fabrication, in the form of extrusion/compression forces, can result in partial pore occlusion and framework degradation, further limiting their performance. Here, we present the development of porous fiber sorbents as an alternative sorbent contactor design capable of addressing sorbent processability limitations while enabling an array of performance-maximizing heat integration capabilities. This new sorbent form factor leverages pre-existing know-how from hollow fiber spinning to produce fiber-shaped sorbent contactors through the phase inversion of known polymers in a process known as dry-jet/wet quenching. The process of phase inversion allows microporous sorbent particles to be latched onto a macroporous polymer matrix under mild processing conditions, thus making it compatible with soft porous materials prone to amorphization under traditional pelletization conditions. Sorbent fibers can be created with different geometries through control of the spinning apparatus and process, offering the possibility to produce monolithic and hollow fibers alike, the latter of which can be integrated with thermalization fluid flows. In this Account, we summarize our progress in the field of fiber sorbents from both design and application standpoints. We further guide the reader through the evolution of this field from the early inceptive work on zeolite hollow fibers to recent developments on MOF fibers. We highlight the versatile nature of fiber sorbents, both from the composition, fabrication and structure points of view, and further demonstrate how fiber sorbents offer alternative paths in tackling new and challenging chemical separation challenges like direct air capture (DAC), with a final perspective on the future of the field.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Enhanced Carbon Dioxide Uptake in Drilled Hollow Core Fibers for Raman Spectroscopy

Fiber-based Raman spectroscopy enhances the Raman signal by maximizing the overlap of the optical field and the gas species. However, filling the hollow-core fiber (HCF) with gas requires time that is dependent on the fiber core diameter, fiber length, and pressure of the gas. At ambient pressure, the fiber gas uptake is driven by diffusion into the fiber ends, severely limiting the response time of the system. By laser drilling access holes to the core along the length of the fiber, the uptake time of the gas is reduced, improving the system response time. In this work, we study the carbon dioxide (CO 2 ) sensor dynamics based on Raman signal intensity generated in HCFs. The signal intensity versus gas concentration is characterized by controlling the CO 2 concentration in the surrounding environment of the fiber. Next, we characterize the gas uptake time in HCFs as a function of fiber length. Finally, we optimize the access hole configuration along the fiber, demonstrating reduced sensor uptake time by a factor of three.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2025

The Anisotropic Adsorption of De Novo Allosteric Two‐Component Protein Fibers on Mica Surfaces

Protein adsorption at solid–liquid interfaces underlies many biomedical and materials applications, yet the mechanisms governing adsorption of proteins and their assemblies remain poorly understood. Here we investigate de novo–designed proteins that self-assemble into three fibrillar morphologies — small (S), large (L), and helical (H)—on muscovite mica. S-fibers are metastable, forming first but diminishing as L- and H-fibers develop and deposit. Adsorption of both fibers and monomers depends on fiber morphology and solvent environment, which is modulated by the substrate. The anisotropic surface features of the fiber types—long axis of S- and L-fibers and helical grooves of H-fibers—correlate with specific crystallographic directions on mica (001). S- and L-fibers align along the unique lattice axis, while the substrate-facing groove of H-fibers preferentially aligns along the remaining symmetry-related directions. Increasing potassium chloride (KCl) concentrations to molar levels alters adsorption, decreasing monomer coverage relative to fibers. These observations, interpreted through the effect of interfacial interface, indicate that ion-mediated modulation of hydration layers governs electrostatic interactions and alignment. This study reveals how coupling between protein topography, substrate crystallography, and hydration structure dictates selective adsorption and orientation of protein assemblies, offering insights for rational biomolecular material design.

AFM↗

DOE OSTI2025

Fiber orientation and porosity in large-format extrusion process: The role of processing parameters

Controlling fiber orientation and porosity in short-fiber thermoplastic composites is important for enhancing mechanical, electrical and thermal properties in large-format additive manufacturing. This study employs a factorial design of experiments (DoE) to assess the effects of nozzle diameter (5.08 mm–10.16 mm), temperature (230–250 °C), and extruder screw speed (150–280 rpm) on flow rate, shear rate, porosity, fiber orientation, fiber length and tensile strength in 20 % carbon fiber-filled acrylonitrile butadiene styrene. ANOVA results show that screw speed significantly impacts flow rate, while nozzle diameter and temperature have lesser effects. Shear rate increases with smaller nozzles and higher speeds. Porosity decreases from 5.58 % with a 10.16 mm nozzle to 3.11 % with a 5.08 mm nozzle at 150 rpm due to increased shear rates, which induce shear thinning, reducing viscosity and facilitating gas escape. Larger nozzles (10.16 mm) produce larger, more heterogeneous pores, while smaller nozzles (5.08 mm) yield smaller, uniform pores. Beads produced with the 5.08 mm nozzle exhibit longer fiber lengths due to reduced residence time, lower shear stress, and better alignment. Fiber orientation improves with smaller nozzles due to higher shear rates but decreases with higher screw speeds (280 rpm) due to shorter residence times. The highest fiber alignment (A xx ∼ 0.65) and low porosity (∼3%) were achieved with a 5.08 mm nozzle at 150 rpm, while equivalent additive manufacturing-compression molding samples exhibited better tensile strength (∼93 MPa) under these conditions. In conclusion, these findings emphasize the importance of optimizing processing parameters to enhance fiber alignment and reduce porosity for improved mechanical performance.

Design of experiments↗

DOE OSTI2025

Segregation of Chromium and Titanium in Sapphire Optical Fiber Grown via the Laser-Heated Pedestal Growth Technique

Our research involves growth of single crystal (SC) optical fibers to be used for sensing applications in harsh environments. Silica optical fibers are an affordable and reliable option for a wide variety of applications including optical fiber sensors and fiber lasers. However, for applications in harsh environments, such as high temperatures, radioactivity, corrosivity, etc., silica fibers are not suitable due to their instability under such conditions. Fibers composed of SC materials such as sapphire and YAG are mechanically, chemically, and thermally more robust to harsh conditions, and thus are more appropriate for sensing applications in environments such as nuclear reactors, jet engines, and boiler. However, SC fibers grown via the laser-heated pedestal growth (LHPG) technique do not intrinsically have a functional cladding layer. A cladding layer is required to reduce the modal volume for distributed sensing applications, to reduce frustrated total internal reflection induced by surface contact of the fiber in certain applications, and to improve transmissivity. Our lab investigates introduction of dopant materials during LHPG to induce an effective core-cladding structure while maintain the crystallinity of the host material. This process results in optical fiber that is not only robust to harsh environments, but also has improved optical properties for distributed sensor applications.

distributed sensing↗

DOE OSTI2025

Segregation of Chromium and Titanium in Sapphire Optical Fiber Grown via the Laser-Heated Pedestal Growth Technique

distributed sensing↗

NASA NTRS1995

Bend Properties of Sapphire Fibers at Elevated Temperatures: Bend Survivability - 1

The effect of temperature on the bend radius that a c-axis-oriented sapphire fiber can withstand was determined for fibers of various diameter. Bend stress rupture tests were performed for times of 1-100 h and temperatures of 300-1700 C. Fibers would survive the bend test undeformed, would fracture or would deform. The bend survival radius was determined to be the radius above which no fibers fractured or deformed for a given time-temperature treatment. It was found that the ability of fibers to withstand curvature decreases substantially with time and increasing temperature and that fibers of smaller diameter (46-83 micron) withstood smaller bend radii than would be expected from just a difference in fiber diameter when compared with the bend results of the fibers of large diameter (144 micron). This was probably due to different flaw populations, causing high temperature bend failure for the tested sapphire fibers of different diameters.

Sapphire↗

DOE OSTI2025

Structure and Sulfur: Tuning the Viscoelastic and Surface Properties of Natural Keratin Fibers

Natural keratin fibers, such as wool, possess a complex hierarchical structure that governs their mechanical properties and surface energy. However, the extent to which these characteristics are influenced by combined contributions of structural variations (e.g., fiber diameter, intermediate filament (IF) packing) and chemical composition (e.g., disulfide bond density) remains poorly understood. In this study, we investigate wool fibers from five sheep breeds (Merino, Polwarth, Cheviot, Eider, and Devon) to elucidate how these factors influence viscoelasticity and surface interactions. Using a multimodal approach integrating interfacial and bulk characterization methods, including inverse gas chromatography (IGC), atomic force microscopy-infrared spectroscopy (AFM-IR), X-ray photoelectron spectroscopy (XPS), uniaxial tensile testing, and synchrotron small-angle X-ray scattering (SAXS), we show that the nanometer-thick 18-methyleicosanoic acid (18-MEA) layer is consistently present across all wool types and plays a key role in governing hydrophobicity and surface heterogeneity. A controlled isothermal treatment at 200 °C, designed to cleave disulfide bonds, results in a nearly 40% reduction in specific surface area across all fiber types, accompanied by a significant decrease in tensile strength and 80% reduction in elongation at break for Merino and Devon wool, but limited influence on the mechanical properties of Eider fibers. Furthermore, rate-dependent tensile testing within the elastic regime reveals distinct viscoelastic responses among the fiber types, suggesting that the sulfur-rich protein matrix surrounding IFs and its structure contribute actively to stress partitioning. Altogether, when combined with conclusions from SAXS measurements of IF spacing, our work offers compelling insights into the role of the keratin-associated protein (KAP) matrix in shaping wool fiber mechanics. Differences in mechanical behavior among wool types, despite similar IF spacing or sulfur content, highlight the importance of matrix composition and cross-linking density, suggesting that the molecular architecture of the KAP network may be a dominant factor in determining fiber performance.

X-ray scattering↗

DOE OSTI2025

Birefringence axis rotation and nonlinear response of a side-hole fiber pressure sensor

The pressure-induced birefringence of side-hole fibers has been widely explored for hydrostatic pressure measurement. Here, this paper studies the effects of the initial birefringence of a side-hole fiber on the pressure response of polarimetric sensors based on side-hole fibers. A mathematical model, where the stress field induced by the pressure is assumed to be uniform in the core region of the fiber, was established to calculate the birefringence and optical axis rotation as a function of the differences between the two principal stress components of the stress field in the core region. Simulation results show that when there is misalignment between the initial birefringence axes and the principal axes of the stress field, pressure changes cause rotations of the birefringence axis, leading to complicated and nonlinear changes of birefringence as a function of pressure. Experiments were conducted using fiber-Bragg-grating-based resonators on side-hole fibers with different initial birefringence, and the results agree well with the simulation. The results underscore the importance of the control of magnitude and direction of the initial birefringence of the side-hole fiber and provide guidelines for the design and fabrication of side-hole fiber pressure sensors.

42 ENGINEERING↗

NASA NTRSDate not supplied

Natural Fiber Simulations and Analysis for Composites

As the U.S. government and the aviation industry strive to achieve net-zero carbon emissions by 2050, the Sustainable Manufacturing of Aircraft (SUMAC) project, supported by the Convergent Aeronautics Solutions (CAS) program of the National Aeronautics and Space Administration (NASA), aims to develop sustainably derived thermoplastic composites and manufacturing technologies for future aviation. A multidisciplinary team of experts drives this initiative through a collective effort. The team’s key focus areas are sustainably derived thermoplastic resins, natural fiber reinforcement, composite manufacturing, structural health monitoring, computational materials modeling, and systems analysis. This presentation will give an overview of the SUMAC project. Fiber-scale microscopy analysis characterized fiber cross sections finding that hemp and flax fibers are very deformable and non-circular (circularities of 0.2 were observed), and diameters range from submicron to 20 μm. Fiber shapes range from flattened, with aspect ratios Rlong/Rshort up to 5, to round, Rlong/Rshort =1. And Fiber core perimeters, which likely drives deformability, were calculated Pcore=7 μm. Explicit-fiber yarn simulations, parameterized from single-fiber measurements, resolved and identified slack as a cause for yarn strain-hardening tensile behavior. The bonded network model of PLA, PHA and PA11 resins captures tensile behavior, and can model an infused weave. Computational models of the weave unit cells matched the pattern (including plain, twill and triaxial braid), yarn ply (1to 2), and yarn twist from optical microscopy.

thermoplastic↗

NASA NTRSDate not supplied

Natural Fiber Simulations and Analysis for Composites

thermoplastic↗

DOE OSTI2026

Mechanistic insights into low-temperature oxidation of carbon fibers: Influence of hydrogen defects and crystallite size

Although oxidation mechanisms have been exhaustively studied for graphite, similar analyses of carbon fibers are comparatively sparse. Most prior work has focused on quantifying weight loss or assessing protective surface coatings designed to slow oxidation. The use of optical spectroscopic techniques for oxidation analyses is comparatively unexplored, but such techniques could provide an early indicator of fiber oxidation that would undermine carbon fiber performance. Here, in this work, we applied Raman spectroscopy to study oxidation-induced spectral alterations in 16 carbon fiber types from 7 manufacturers oxidized at 300 °C for 72 h, 400 °C for 8 h, and 500 °C for 1 h. We connect these results with structural properties of the carbon fibers obtained through wide-angle X-ray scattering, identifying a linear dependence between the reactivity of carbon fibers and the crystallite size of the unperturbed fibers. We then demonstrate that substituted hydrogen defects are likely removed from the fiber surface during oxidation and use the relative defect concentration to predict the Raman spectral change as a function of temperature and time, assuming Arrhenius behavior.

Carbon fiber↗