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DOE OSTI2024

Fundamentals of Scalable Nanoparticle Assembly in Engineering Polymres

Systematically improving the properties of polymer nanocomposites is contingent on effectively controlling nanoparticle (NP) dispersion; further, it is necessary to attain this at scale if these methods are to impact practical applications. While most past work has focused on amorphous polymers, ≈ 70% of all polymers sold annually are semicrystalline. Inspired by this apparent disconnect, our work in the current DOE funded grant and this renewal proposal employs a novel handle, polymer crystallization, to organize NPs into the various amorphous zones of the lamellar semicrystalline morphology (interlamellar, interfibrillar and interspherulitic domains) of stereoregular polymers. We hypothesize that the isothermal crystallization rate of a polymer host, G, and NP diffusivity, are the two relevant control parameters in this context. In the case where the NPs are miscible in the melt, they remain spatially well-dispersed when the polymer is crystallized at a rate that is fast relative to NP diffusion. In contrast, monolayer-thick NP sheets with intersheet spacing of ~10-100nm form in slowly crystallized samples. This sheet stacking is remarkably similar to that seen in natural materials, e.g., Nacre. There is also ordering of the NPs at the larger interfibrillar scale. Importantly, the relative fraction of engulfed, interlamellar and interfibrillar NPs is determined by G. Further, the modulus of these materials can increase by a factor of 2-3 due to the organization state of the NPs, while leaving fracture toughness unaffected. We have established the broad applicability of this approach in two polymers, polyethylene (PE) and polyethyleneoxide (PEO). To achieve this goal we developed a method for grafting long PE chains from NPs with controlled graft density and molecular weight, giving us the ability to tailor their dispersion in the PE melt prior to crystallization. In this renewal proposal, we will develop the fundamental, quantitative understanding that will allow us to independently tailor polymer crystallization rate, NP diffusivity and NP agglomeration state in semicrystalline polymers so as to facilely control NP ordering and hence properties. A program that tightly integrates experiment and theory is proposed, and a key outcome of this research will be a three-dimensional design map for different regimes of NP organization (and hence properties) that can be achieved by polymer crystallization. A second independent outcome is the role of directional solidification and how it competes with the rates of polymer crystallization and NP mobility to affect the organization of the NP.

36 MATERIALS SCIENCE↗

DOE OSTI2024

TEAMER Technical Support for Aquantis (Materials) (Final Report)

The Aquantis Tidal Power Tug is a unique synthesis of best-available technologies and materials configured as a novel spar vessel to create an optimal platform for tidal stream energy conversion. The Power Tug utilizes an upstream-facing horizontal, 2-bladed rotor. To drive down capital costs and extend life, Aquantis proposes to employ new materials for the blades that are both less expensive than current state-of-the-art materials and are potentially better suited for survival in a submerged, seawater environment. Coupons from a novel geopolymer material will be tested in a load frame to characterize material properties. The Requestor is requesting technical assistance for evaluating mechanical properties of a novel geopolymer material for application in tidal stream energy conversion systems. This work will establish characteristic properties of a geopolymer material under dry and saturated conditions through material coupon testing. Material coupons will be tested to characterize properties including: a) Tensile strength, b) Compression strength, c) Flexural strength, d) Modulus of elasticity, e) Fatigue strength at varying load levels. The types of material tests performed will be guided by characteristics required to validate material properties for use in full-scale structures. Characterization of material properties that consider the demands of a full-scale structure is a necessary step in research and development that can enable the use of geopolymer materials in tidal stream energy conversion systems.

16 TIDAL AND WAVE POWER↗

DOE OSTI2024

Self-Organized Stress Distributions in Polycrystalline Materials [Dissertation]

Understanding stress distributions in solid materials is complicated by the fact that most materials are polycrystalline in nature, with each crystal having an elastically anisotropic reaction to force. This study is to gain a better understanding on how external forces placed on a polycrystal are related to internal reactions within and between the grains. The hypothesis is that the stress distribution in porous to fully dense materials are self-organized based on strong contacts between and within the individual grains created by force chains. Force chains, commonly known in loaded granular materials, and could be the phenomenon that connect micro to macro deformation. Scale bridging measurements conducted through Raman spectroscopy, Atomic Force Microscopy, and Digital Image Correlation will be used to create stress maps, modulus maps, and elastic strain maps across a variety of geological and pharmaceutical polycrystals. When possible, the resulting maps will be compared to current homogenization schemes and a full field models. Finite element modeling will be used to assess whether the patterning seen in the experimental map is a reasonable approximation based on the orientation data of the samples used. A minimum of three publications is projected to be accomplished focusing each on a different method to experimentally test and analyze stress distributions.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Facilitating Implementation of High-Volume Fly Ash Use in Pre-cast Concrete Construction to Increase Beneficial Utilization

The main goal of this project was to increase the beneficial use of fly ash as a supplementary cementitious material for precast concrete applications. A major focus was to develop balanced concrete mix design strategies which collectively satisfy the follow objectives: 1) increase fly ash beneficial use by at least 15% in the precast concrete industry, 2) maintain or exceed stringent structural property requirements (e.g., compressive strength at initial prestress, modulus of rupture, etc.), 3) exhibit little or no additional cost relative to conventional mixtures, and 4) mitigate detrimental environmental consequences inadvertently caused by increased beneficial use. Outcomes from this project include recommendations for design guidelines and code provisions for sustainable concrete mix designs, facilitating diversion and harvesting of large quantities of fly ash from landfills or impoundments, and multiple frameworks for incorporating discarded fly ash materials (i.e., landfilled or ponded fly ash after separating the impurities) in concrete construction.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2024

Inexpensive and durable aerogel-based VIP cores

The goal of this project was development of low-cost aerogels to be used as cores of Vacuum Insulated Panels (VIP). The specific aims were: 1. Aerogels to be based on phenolic chemistry to minimize flammability. 2. Aerogels to be in monolithic form and to have mechanical properties sufficient to allow their use as cores of VIPs without collapsing after evacuation. 3. Aerogels to have a cost per kg lower than the cost of fumed silica, one of the most common VIP cores. The achievements are: 1. Phenolic aerogels have been fabricated in monolithic form with thermal conductivity of 0.023 W/m·K, density ~ 0.25 g/cm 3 and a modulus of compression > 10 MPa. The aerogels can withstand the stresses of VIP evacuation without any appreciable deformation. 2. Drying of aerogels was carried in the initial stages of the project via sublimation of frozen solvents, following the procedure described in M. F. Bertino and T. Selden, “Fabrication of Aerogels and Aerogel Composites by Ambient Pressure Sublimation of Frozen Solvents”, PCT/US20/39485. Monoliths as large as 30 x 30 x 2 cm can be fabricated with the proprietary ambient fabrication technique which are free of cracks and warping. 3. Cost analysis was carried out and refined multiple times, cost drivers were identified, and the fabrication procedure was streamlined. Our cost model yields an aerogel cost of $\$$5.78/kg, which compares well with the price of fumed silica ($\$$6.2/kg FOB New York as of March 2023). 4. The monoliths can be cut into custom shapes and used as VIP cores. Cores fabricated with our technique have a thermal conductivity λ = 0.011 W/m·K at a pressure >10 mbar. 5. A variant of the technology yielded fireproof materials, described in M. F. Bertino, T. Moon, G. Waller, J. Ko and D. Clifford, “Fireproof thermal insulation”, Provisional Patent Application 63/415,386. 6. A spin-off company was created (ThermaGel Innovations, Inc.) which licensed technologies developed under this award. PI Bertino is a board member of the newco which is now raising capital to build a pilot plant.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Risk of theft and malicious use of radiation sources in transit

Remote radioactive source applications require frequent transportation of sources from storage locations to remote sites. This introduces risk of theft of a source during the transportation process, with the level of risk proportional to the radioactivity of the source. To that end, theft of smaller sources, such as microcurie-level moisture density gauges, are of minor concern, but larger sources, such as those used for radiography and well logging, present more risk. Radiography sources include 192 Ir, 75 Se, or 60 Co radionuclides with radioactivity amounts at or exceeding IAEA Category 2. Well-logging sources, primarily 241 Am/Be, are used for their neutron-emission properties. 137 Cs is also used in well-logging at lower activities than in radiography but at levels that still present some risk. The vulnerability for malicious use of such sources to cause contamination and associated economic effects is dependent on the elemental chemical and physical properties, especially melting point and bulk modulus. Theft of radiography sources is somewhat common, well-logging sources less so. Theft of sources commonly occurs in concert with theft of the vehicle, with the source subsequently abandoned. There have been some instances where a source appears to have been specifically targeted. There are a variety of security measures and protocols, available and under development, to mitigate the risk of theft and assist in source recovery.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

DOE OSTI2024

2D Amorphous Carbon Dielectric Prepared from Solution Precursor for Nanoelectronics

The preparation of amorphous 2D nanodielectrics represents a major challenge due to the metastable nature of amorphous phases. We describe a scalable and solution-based strategy to prepare wafer-scale 2D amorphous carbon with thickness down to 1–2 atomic layers from coal-derived carbon quantum dots as precursors. The prepared atomically thin 2D amorphous carbon can be suspended over cavities as freestanding membranes with high modulus of 400±100 GPa and demonstrate robust dielectric properties with dielectric strength above 20 MV·cm-1 and leakage current density below 10-4 A·cm-2 through a scaled thickness of three-atomic layers. When implemented as ultrathin gate dielectrics in 2D transistors or ion-transport media in memristors, they enable exceptional device performance and spatiotemporal uniformity, resulting from their amorphous form, intrinsic ultrathinness, and 2D atomic structures.

Pham, Viet Hung↗

DOE OSTI2024

Solution-Based Synthesis of Ultrathin Quasi-2D Amorphous Carbon for Nanoelectronics

The synthesis of ultrathin 2D amorphous dielectric film represents a major challenge due to the metastable nature of amorphous phases. We describe a scalable and solution-based strategy to prepare wafer-scale 2D amorphous carbon with thickness down to 1–2 atomic layers from coal-derived carbon quantum dots as precursors. The prepared atomically thin 2D amorphous carbon can be suspended over cavities as freestanding membranes with high modulus of 400±100 GPa and demonstrate robust dielectric properties with dielectric strength above 20 MV·cm-1 and leakage current density below 10-4 A·cm-2 through a scaled thickness of three-atomic layers. When implemented as ultrathin gate dielectrics in 2D transistors or ion-transport media in memristors, they enable exceptional device performance and spatiotemporal uniformity, resulting from their amorphous form, intrinsic ultrathinness, and 2D atomic structures.

Pham, Viet Hung [NETL Site Support Contractor, Nat↗

DOE OSTI2024

Lithium Dendrite-Free Li 7 N 2 I-LiOH Solid Electrolytes for High Energy Lithium Batteries

All-solid-state lithium batteries (ASSLBs) hold great potential to improve the safety and energy density of today’s lithium-ion batteries by using non-flammable inorganic solid electrolytes. Solid electrolytes (SEs) are believed to prevent Li dendrite growth because of high mechanical strength and high Li+ transference numbers. Significant advances in SE have been achieved, among which, Li7La3Zr2O12 (LLZO) and Li2S–P2S5 (LPS) are the most promising SEs for bulk-type solid-state lithium batteries because of high ionic conductivities (>10-4 S/cm2). However, in contrast to our expectations, the growth of lithium dendrites is not suppressed but is facilitated in LLZOs and LPSs regardless of dopants, porosity, and crystallinity of the electrolytes. Despite the unity Li transference number and over two-times of shear modulus than that of Li metal, the critical current densities for Li plating and stripping in these SEs are less than 1.0 mA cm-2, which is one-fourth to one-tenth of that in liquid electrolytes at room temperature. The incompatibility between LLZO and LPS with Li metal seriously limits the energy density of all-solid-state batteries. The mechanism for lithium dendrite formation and growth in SEs are still disputable. Lack of understanding of the Li dendrite formation mechanism seriously impeded the development of solid-state lithium batteries. The development of the criterion for Li dendrite suppression is essential for the success of solid electrolyte lithium batteries. In this project, a criterion for Li dendrite suppression will be developed through thermodynamics and kinetics analysis of lithium dendrite nucleation/growth, which will guide the solid-state electrolyte design. Li7N2I-LiOH, Li5NI2-LiOH and Li3YCl6 solid electrolyte with high ionic conductivity and low electronic conductivity were used to validate the criterion for lithium dendrite suppression. Different surface modifications were also explored to enhance the dendrite suppression capability of SSEs.

25 ENERGY STORAGE↗

DOE OSTI2024

DECOVALEX-2023: Task D Final Report

Task D of DECOVALEX-2023 is focused on the simulation of the coupled thermal hydraulic-mechanical (THM) behaviour in the full-scale engineered barrier system (EBS). The Horonobe EBS experiment is the demonstration of the full-scale EBS in the underground research laboratory (URL) (performed by JAEA in the Horonobe URL in Japan). Task D consisted of the three steps, a preliminary step (Step 0), simulation of the laboratory tests (Step 1) and simulation of the in-situ full-scale EBS experiment (Step 2). Since the Horonobe EBS experiment demonstrates the vertical emplacement option of the EBS, the experiment gallery is also backfilled with the backfill material. Therefore, interaction between the EBS and the backfill material can also be demonstrated, such as deformation (change of density) of the buffer material. The underground water in the Horonobe URL is saline. This fact adds chemical processes to THM behaviour. For example, mechanical properties (such as swelling pressure of the buffer material and backfill material) and hydraulic properties (such as permeability of the buffer material and backfill material) change depending on the water chemistry. Task D was therefore a challenging Task focused on not only the relatively simple THM behaviour but also complex THM behaviour including chemical processes. Six research teams (BGR, CAS, JAEA, KAERI, SNL and Taipower) participated the Task D. BGR, CAS, JAEA, KAERI and Taipower research teams selected a THM approach, while the SNL research team selected a TH approach. Step 1 involved the simulation of laboratory test results and was important to check the numerical codes developed by the research teams. Step 1 was divided into four sub steps. The simulation results through the Step 1 identified the parameters for simulation of the Step 2. Basic parameters of the materials (buffer material, backfill material, rock mass, concrete, sand) were provided by JAEA. Special parameters which research team needed were identified by back analysis of Step 1. Most notably the mechanical behaviour of swelling and displacement depended on the applied model (elastic model or elastoplastic model). Parameters such as Young’s modulus were found to need smaller values than characterised in the fundamental laboratory test results (Step 1-1, 1-2) for the elastic model. Although laboratory experiments are usually simple, test results contained some error. For example, if the saturation level is 100 % or higher, it should be considered an error. This situation was presented in the Step 1-3. A possible reason is that the buffer material is a mixture of bentonite and silica sand. When a specimen is cut to measure volume or weight, sand grains will affect the measurement data. In Step 2, boundary conditions such as temperature on the surface of the simulated overpack, heater power of the electrical heaters installed in the simulated overpack, injection pressure and inflow rate of the test water, were applied. The outer boundary conditions can be selected using measured data (injection pressure and inflow rate of the test water that is controlled by the injection systems installed in the sand layer around the buffer material and in the boundary between backfill material and concrete support). Since such measured data has some noise, research teams developed their own simplified boundary conditions. Inner boundary conditions can be selected using measured data as heater power and temperature on the surface of the simulated overpack. These data also contain some noise, so research teams developed their own simplified developed boundary conditions. Task D validated various approaches thorough the simulation of the in-situ full scale EBS system including backfill of the gallery: variations in the coupling processes (THM or THC), analysis codes, and boundary conditions. Temperature distribution in the buffer material was simulated well by all research teams. This means thermal behaviour is not sensitive to the simulation approaches. Although the water content distribution on the outside of the buffer material was well simulated by all research teams, the simulation results differ from the measured values inside the buffer material (at the centre and inside, near the simulated overpack). The buffer material is made from tap water, but in the in-situ experiment, saline groundwater infiltrates the buffer material. Therefore, the selection of the hydraulic parameters of the buffer material greatly affects the simulation results of the re saturation behaviour of the buffer material. In the Horonobe EBS experiment, measured values suitable for validating the simulation results were not obtained near the simulated overpack. When simulating the pressure and deformation of the buffer material, the measurement data is easily affected by the installation conditions of the measurement sensors, so verifying the measurement data itself remains an issue. Mechanical simulation results differ depending on whether they are considered as elastic or elastoplastic phenomena. The accuracy of measured in-situ data can be assessed by detailed analysis comparing sampling specimen analysis and measured data. The Horonobe EBS experiment is scheduled to be dismantled in the future (FY2026 and 2027). This detailed dismantling investigation will finally confirm the measured data.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Coal to Carbon Fiber (C2CF) Continuous Processing for High Value Composites (Final Report)

Coal tar is a condensed and recovered by-product of the coking of metallurgical coal for steel production. The heaviest fraction of distilled coal tar is an isotropic pitch largely used as a binder in the manufacturing of carbonaceous electrodes for primary aluminum smelting and in electric arc furnaces. Coal tar pitch offers high carbon yield upon carbonization. In this project, a process to convert the domestically sourced isotropic coal tar pitch, containing very low particulates (QI = 0.32 wt.%), to form flow-domain mesophase pitch amenable for melt spinning into precursor (green) fibers for carbon fiber, was developed and optimized. The final reproducible processing developed is reviewed in this report, along with several characterizations of the mesophase pitch. A final definition of the characteristics of a ‘spinnable’ mesophase pitch is presented. With this mesophase pitch, reproducible and stable multifilament melt spinning was developed, producing green fiber tows with filament diameters of approximately 20 m. The multifilament melt spinning was the most challenging aspect of the project and required the most effort. The best practices learned from this project for melt spinning are reviewed in this report. Once spun, the green fibers were oxidatively stabilized, carbonized and graphitized under inert gas atmosphere to form the final carbon fibers. Given the relatively high softening point of the mesophase pitch, no issues of interfilament fusion were observed during batch oxidation, and subsequent batch carbonization and graphitization went smoothly in all cases. An ~ 80 wt.% conversion of the green fiber mass to final carbon fiber was achieved. After graphitization, the carbon fibers showed high tensile moduli (most were ~ 600 GPa, or 87 Msi) consistent with commercially-available high-performance pitch-based carbon fiber. However, tensile strength and strain to failure were comparatively low. Further work to reduce defects in and on the fiber surfaces would increase these properties. SEM imaging of the graphitic fiber textures is presented herein. Rudimentary composites were fabricated from the carbon fibers and characterized showing similar modulus to baseline composites fabricated with commercial carbon fiber. Finally, a basic economic analysis was done showing the potential to increase the value of the isotropic coal tar pitch by up to 13.6 to 136 times based on a carbon fiber value of $\$$5/lb to $\$$50/lb, respectively. Moreover, the site case study suggests that the coal tar from the single integrated steel mill could supply production of up to 16 kt/yr of carbon fiber. Finally, a technological gap analysis was done which shed light on remaining technical challenges. These challenges included: recovery and utilization of condensates from the mesophase pitch processing, further advancing and increasing stability of the multifilament melt spinning processing, optimization of the oxidation processing, defect reduction for increased carbon fiber strength, and the development of a weaving process towards carbon fiber fabrics. To maximize the coal value chain, the primary objectives of this project were to (a) develop and scale efficient processing technology for producing melt-spinnable mesophase pitch from isotropic coal tar pitch, (b) clarify and simplify tedious continuous fiber processing technologies (particularly multifilament melt spinning of mesophase pitch) towards the efficient production of high performance carbon fiber, and (c) demonstrate and characterize representative composite parts derived from the final carbon fiber. Immense progress was made on all 3 objectives and is detailed in this report.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2025

Rapid Bayesian High Entropy Alloy Designs Fabricated via Wire Arc Additive Manufacturing

Purpose: This project seeks to demonstrate a new high-throughput (rapid) alloy design technique applied to creating new high entropy alloys (HEAs) for extreme environments. High entropy alloys shift the design paradigm from being focused on a single principal element (e.g. nickel-based alloys) to target alloys that include high atomic fractions (X >10%) of multiple elements. These HEA materials can exhibit sluggish diffusion and enhanced corrosion resistance, ideal for potential applications in advanced ultra supercritical (A-USC) steam cycles for power generation. Scope: The addition of multiple elements in high atomic fractions creates an enormous design space that cannot easily be investigated by traditional material design strategies such as designed of experiments (DOE). This project utilizes a Bayesian machine learning algorithm that has been modified to work with calculation of phase diagrams (CALPHAD) software. This Bayesian algorithm reduces manual inputs and increase the likelihood of achieving an optimal solution. Compositional inputs to this algorithm will be assessed using existing material property models for high temperature strength and corrosion resistance. The target for alloy performance will be a 15% (~100 ⁰C) increase in allowable service temperature beyond heat-resistant stainless steels while maintaining or improving alloy cost and corrosion resistance. Haynes 230 was selected as a baseline, which is 57 wt% Ni with 22 wt% Cr 14 wt% W, and 2 wt% Mo as solid solution strengtheners. In addition to rapid design via Bayesian machine learning, the alloys were rapidly fabricated using a multi-wire arc additive manufacturing (mWAAM) technique which allows for precise control of alloy composition and assessing of alloy design “windows” to study composition effects. Build speeds for wire-arc additive processes are among the highest for additive technologies enabling rapid and reliable sample fabrication when compared to conventional methods such as arc button melting. The mWAAM samples will be rapidly characterized via instrumented indentation for room temperature modulus and strength and for elevated temperature strength via hot hardness tests. After being screened with hardness testing, potential alloys will be further evaluated with conventional microscopy techniques including scanning electron microscopy (SEM) and transmission electron microscopy (TEM) to assess agreement with modeling results. The most promising compositions will also be evaluated by printing full sized tensile specimens for mechanical behavior tests at elevated temperatures. Results: Bayesian machine learning of a single performance function was initially used to optimize five performance metrics: 1) single phase stability, 2) yield strength, 3) creep resistance (low diffusion coefficient), 4) freezing range (weldability), and 5) material cost. The single performance function was suboptimal as assumptions had to be made about the results while formulating the optimization. A goal-oriented Bayesian optimization strategy (Hanaoka, 2021) was implemented with CALPHAD for use with the five metrics above. This multi-objective Bayesian optimization (MOBO) enabled the design of NiCrCoFe alloys with V and W additions. A base composition of NiCoCr was selected as Ni provides a stable FCC matrix, Cr aids corrosion/oxidation resistance, and Co is a solid-solutions strengthener that also improves creep by increasing the activation energy. Fe helps reduce diffusion coefficients and cost. Finally, V and W were selected for their reasonable solubility and high atomic misfit to aid in solid solution strengthening. Cracking of the mWAAM specimens was an early issue, and the Easton solidification cracking model (Easton et al., 2014a) was selected for addition to the MOBO function. High performing alloys fabricated by mWAAM included Ni 28 Cr 25 Co 26 Fe 15 V 8 and Ni 62 Cr 18 Co 1 Fe 3 W 15 . It was observed that even after adapting the mWAAM process for W, the W did not fully dissolve. To fully evaluate the Ni 62 Cr 18 Co 1 Fe 3 W 15 composition, a cored wire (80-20 NiCr sheath/powder core) was manufactured and printed via WAAM, and HIP’ing was utilized to homogenize and densify the printed alloy. The V and W alloys produced met metrics 1 (solid solution), 4 (solidification cracking), and 5 (cost). However, an unmodeled mechanism of thermal stress cracking was identified in the WAAM produced materials, perhaps exacerbated by the lack of grain boundary strengthening elements (B, C). Conclusions & Recommendations: A high-throughput (rapid) alloy design technique was applied to designing and manufacturing new high entropy alloys (HEAs) for extreme environments utilizing MOBO and mWAAM. The developed process was rapid and effective in addressing the mechanisms included in the model. The lack of grain boundary strengthening element additions (e.g., B, C) was a simplification that likely produced thermal stress cracking that turned into a large part of the investigation. Additions on the order of 0.005 wt% B and 0.05 wt% C likely would have minimized thermal stress grain boundary cracking. Overall, the high throughput design strategy is promising for rapid design of metrics-driven alloys for advanced ultra supercritical (A-USC) steam cycles for power generation. The MOBO and mWAAM process could be commercialized to accelerate metrics-driven alloy design. In addition, the cored-wire process utilized for scale-up is a promising high-volume process for WAAM alloy development and scale-up.

36 MATERIALS SCIENCE↗

DOE OSTI2024

Low-Cost, High-Performance Carbon Fiber for Compressed Natural Gas Storage Tanks (Final Technical Report – Down Select Report)

The aim of this project is to reduce the cost of Type IV, carbon fiber (CF) composite overwrap compressed gas storage tanks by reducing the cost of CF and CF composites. The project team worked to reduce the cost of CF by exploring and testing opportunities for a low-cost alternative precursor material for CF production to supplant market-dominant and costly polyacrylonitrile (PAN). Concurrently, the team aimed to reduce the cost of the tanks at the composite level by improving the interfacial adhesion between the fibers and the matrix resin through the incorporation of low-cost nanoparticles recycled from waste materials, which would reduce the volume of costly CF required to achieve the same tank performance. At the end of the first year, the project team selected mesophase pitch as the primary precursor candidate from a field of materials based on the superior mechanical performance and cost-saving potential. During the second year, the team produced CFs derived from mesophase pitch achieving an average tensile strength of 365.6 ksi and average tensile modulus of 40.74 Msi. Facility availability for spinning and converting these fibers at greater scale has hindered scale-up demonstration, but the team has identified opportunities to conduct this work in the near term. Cost modeling shows that these mesophase pitch-derived CFs can be up to 40% less expensive than PAN-derived CFs due to the lower cost of the feedstock material, higher throughput, greater conversion yield, and lower cost spinning method and compared to PAN. Additionally, the team has demonstrated at lab-scale that nanoparticle coating CFs can significantly increase the interfacial shear strength and load transfer efficiency of CFs in a matrix. Single filament pull-out testing showed a 27% average increase in max interfacial shear strength due to this coating. A continuous method of applying these coatings to a tow of CF has been developed for scale-up. 26 m tows of coated CFs were produced using this system and formed into composite ring samples for ASTM ring burst testing. Issues with the testing protocol have limited assessment of these results. A prototype Type IV tank was designed to meet ANSI HGV2 standards, and the design criteria set out by DOE, using the CF properties developed by the team paired with a proprietary resin matrix, a polyamide liner, and aluminum end bosses. The tank weighs 153.1 kg and with a total capacity of 5.8 kg H2 (5.6 kg usable), which yields a gravimetric capacity of 1.17 kWh/kg. Cost modeling predicts that the tank will have a projected cost of $15.73/kWh. Tank performance modeling does not include considerations for fiber-matrix load transfer efficiency improvements offered by nanoparticle coating method.

08 HYDROGEN↗

DOE OSTI2025

Coal Enhanced PEEK Filament Production for Additive Manufacturing in Industrial Services

The project (Award DE-FE0032146), led by Baker Hughes in collaboration with the University of Wyoming, aims to develop composite PEEK (Polyether-ether-ketone) materials enhanced using coal-derived graphene-based additives suitable for additive manufacturing (3D printing). Coal char (CC), graphene oxide (GO), and reduced graphene oxide (rGO), derived from Powder River Basin (PRB) coal, were successfully integrated into commercial PEEK feedstock. The composite PEEK materials demonstrated tensile and flexural strengths and modulus, Shore hardness, and thermal properties similar to unfilled PEEK. Dielectric strength of 0.5% GO/PEEK is twice that of unfilled PEEK. However, tensile elongation and Izod impact toughness of the composite materials are lower than unfilled PEEK. The 10% CC/PEEK material also shows good recyclability albeit with slightly increased glass transition and cold crystallization temperatures. Filaments of the composite PEEK materials were fabricated using a Filabot system. 3D printing of the composite PEEK initially encountered feeding stoppage caused by the non-uniform diameter of the filament, which was resolved by reducing the nominal diameter from 1.75 to 1.65 mm. The printability of the composite PEEK filaments is limited in geometry and build time, driven by differences in base PEEK feedstock from the commercial PEEK filament at printing conditions. Prototype part printed using the composite filaments shows inconsistent bead width and bead interruption resulting in porosity. Preliminary process and economic evaluation using PRB coal char estimates the cost of GO to be $0.5/lb. Considering the small fraction expected in the composite PEEK, the GO cost is several orders of magnitude lower than the commercial PEEK filament. It is recommended that the printability of composite PEEK filaments to be improved by optimizing the composite PEEK material at the printing conditions and reducing the variations in filament extrusion. Also important is to identify the mechanisms of how coal-derived additives affect the composite PEEK performance and printing characteristics to allow customized material design and processing for target performance.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2025

Resin Testing and Modeling for Optimal Composite Processing

Polymer composites have properties such as high strength and stiffness, low weight, good thermal and chemical stability, as well as impact and abrasion resistance that make them ideal for high-performance applications. The chemistries of these materials are continuously improving, so determining their properties is vital for successfully producing them and achieving the desired results. Multiple methods can be employed to monitor characteristics such as heat flow, weight, dimension, and modulus as a function of time and temperature. By analyzing this information, models can be developed to predict outcomes of parameters not tested for. In one application, materials proposed for wet filament winding and the production of high pressure vessels can be analyzed to verify they will have the necessary low viscosity for good fiber wetting and long pot life for the extended handling inherent to this process. Such data about a prospective system provides valuable information on how that material could ultimately be processed to yield the desired part.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Additively manufacturing high-temperature aluminum alloy for automotive engine pistons

The purpose of the project was to evaluate DuAlumin-3D, an ORNL designed Al alloy, for additive manufacturing of high-performance automotive components. The project consisted of additively manufacturing a cylindrical block of representative material which was then heat treated before machining into test coupons. Testing included tensile tests as a function of temperature, high-cycle fatigue testing as a function of temperature, density and elastic modulus measurements, and thermophysical property measurements. Fractography was also performed on failed high-cycle fatigue specimens. The results were compared against benchmark AM Al alloys and current high-performance conventionally manufactured alloys. Overall, the DuAlumin-3D material outperformed the incumbent materials in mechanical properties, especially at elevated temperatures, while maintaining broadly similar thermophysical properties. The results of this study support further maturation of the material for additive manufacturing of high-performance automotive components.

36 MATERIALS SCIENCE↗

DOE OSTI2025

ULTIMATE Phase I project: Development of Niobium-based alloys for Turbine Applications

Current Ni-based alloys used in turbine blade applications are operating at 1100°C which is approximately 90% of the solidus of Ni-based alloys. Further increases in temperature can be achieved only through the use of alloys with higher solidus temperatures such as refractory alloys which include Mo, Nb, W, Ta alloys. Niobium has a unique combination of physical properties that include a high melting point (2468°C), lowest density (8.57 g/cc), and the lowest modulus amongst refractory alloys, a good thermal conductivity that increases from 45 W/mK at room temperature to 62 W/mK at 1093°C, good ductility with fabricability using traditional techniques, high strength, good creep resistance, and general chemical inactivity. Hence niobium alloys offer many advantages for use at the desired temperature of 1300°C. One of the major deterrents to the use of niobium and its alloys at high temperatures is achieving good oxidation resistance. In addition, achieving balanced properties of room temperature strength, ductility, fracture toughness, high temperature strength, and creep resistance required for 1300°C operation at a density of 9 g/cm 3 is extremely challenging since the addition of W which is a potent strengthener increases the density of the alloy. This project seeks to enable the development of a tri-layered turbine blade that can operate continuously at 1300°C with the core of the turbine blade providing good creep resistance, the second layer providing improved oxidation resistance over the core layer, and the third layer being an environmental barrier providing oxidation resistance. The objective of this Phase 1 project was to use computational modeling and advanced characterization tools to develop two classes of Nb alloys which could be used as the core layer and the transition layer. The first class of alloys developed in this project was a Nb-alloy designed to serve as the turbine blade core with excellent room temperature strength, ductility, and high temperature strength and creep resistance required for 1300°C operation. These alloys were designed to contain sufficient solute solution strengthening elements (W, Mo) but constrained by the density of alloy, along with the addition of elements such as Zr, Hf, Ta, C, and N to achieve a combination of primary and secondary carbide precipitation. A total of 38 “creep-resistant” alloys were designed and cast during the duration of the project. Processing techniques were developed to keep the oxygen contents as low as possible with typical oxygen contents less than 250 ppm. One alloy with a density of < 9.5 g/cc was successful in meeting the Phase 2 intermediate project mechanical property milestone requirements of room temperature ductility greater than 1.0%, 1200°C creep strain of less than 3% at 150 MPa and 100 hours in vacuum, and with solidus temperature greater than 1500ᵒC. The second class of alloys was designed to be a Nb-rich alloy with improved oxidation resistance when compared to the core layer and was designed specifically to be compatible with the core layer and the outer environmental barrier coating. This Nb- alloy will be specifically designed to be microstructurally stable at these temperatures when in contact with the core alloy and provide protection against catastrophic failure of the barrier coating. Two alloys were cast and processed but further development was discontinued to focus on the development of the creep resistant alloy.

36 MATERIALS SCIENCE↗

DOE OSTI2025

Development of Niobium-based alloys for Turbine Applications: 20/CJ000/08/09 (ULTIMATE Phase I project)

36 MATERIALS SCIENCE↗