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All sourcesNASA NTRSDOE OSTI
DOE OSTI2025

Degradable Biocomposite Thermoplastic Polyurethanes

In this project, the team developed tough and degradable biocomposite thermoplastic polyurethanes (TPUs) by incorporating bacterial spores into TPUs as a biofunctional living filler. The team screened various bacteria and selected the Bacillus subtilis ATCC 6633 strain as the final candidate, primarily due to its genomic availability, sporulation ability and TPU assimilation activity. The heat-shock tolerance of ATCC 6633 spores was further improved through evolutionary engineering via Adaptive Laboratory Evolution (ALE), demonstrating a 17.7-fold enhanced germination efficiency post heat-shock treatment compared to the wild-type strain (WT). The team fabricated biocomposite TPUs by incorporating lyophilized powder of heat-shock tolerized (HST) spores during the hot melt extrusion (HME) of TPU at 135 °C. The baseline TPU used in this project is a commercially available soft-grade TPU (BCF45) manufactured by BASF. Colony forming unit (CFU) assays quantified that WT and HST spores in the TPU matrix retained approximately 20% and 100% survivability, respectively, after HME. Tensile testing demonstrated that the spores behaved as a polymer-reinforcing filler, positively affecting the overall tensile properties of the biocomposite TPU. For example, biocomposite TPU with WT and HST spores (BC TPU WT and BC TPU HST , respectively) exhibited up to 25% and 37% improved toughness, respectively, compared to TPU without spores. BC TPU HST showed remarkably improved disintegration in autoclaved compost (92% mass loss in 5 months), which simulated a microbially poor environment for TPU degradation. When compared to TPU without spores (44% mass loss in 5 months) the acceleration of degradation is marked. Respirometry confirmed that 72% of BC TPU HST was biomineralized into CO2 within 6 months, indicating that spores in the biocomposite TPU were germinated by utilizing nutrients in the autoclaved compost, facilitating TPU degradation at the end of the material's life. The team demonstrated the scale-up of biocomposite TPU fabrication using continuous extrusion and injection molding techniques. Processing conditions optimized in a lab-scale microcompounder were successfully transferred to a continuous extruder with a 30-fold increased throughput. Biocomposite TPUs prepared using these industry-relevant processes showed comparable toughness improvements to samples prepared in the lab-scale extruder. Excitingly, following compounding in the pilot-extruder the composite material could be injection molded, while retaining high spore viability and similar toughness improvements. The team also found that spores in biocomposite TPU served as antioxidants, preventing toughness decay during the recycled extrusion of BC TPU HST . Long-term storage tests over one year showed that the addition of spores had no negative effect on the longevity of the TPU. Furthermore, the team demonstrated the fabrication of spore-bearing biocomposite polymers with other polyesters such as PBAT, PLA, and PCL. We obtained promising preliminary data that showed overall toughness improvements for all polymers with spore addition. Finally, life cycle assessment (LCA) and techno-economic analysis (TEA) were carried out, which indicated minimal additional cost of fabrication. Overall, a tough and degradable biocomposite thermoplastic was successfully developed through this project, with all tasks completed successfully, achieving >100% of the objectives.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Predictive Tools for Customizing Heat Treatment of Additively Manufactured Aerospace Components

Laser-bed powder fusion (LBPF) additive manufacturing is increasingly being used to produce components of complex geometries using the Ni-base superalloy Inconel 718. The composition and the microstructure of the alloy are currently well optimized for wrought components made using conventional manufacturing processes such as rolling, forging, extrusion, etc. The attractive mechanical properties of the alloy result from the underlying austenitic matrix with fine equiaxed grains, and a high density and uniform distribution of the precipitation hardening phase, γ". Heat treatment steps such as homogenization, solutioning and aging are well documented for the wrought alloy. However, when the same wrought alloy compositions are used for the additive manufacturing (AM) processes, the asprocessed microstructure is significantly different, because of the different thermal history associated with LBPF, including rapid solidification and multiple temperature excursions that lead to multiple re-melting and reheating in the solid state. Rapid solidification introduces potential non-equilibrium effects at the moving solid-liquid interfaces that impact the extent of solute segregation, as well as the morphology of the dendritic grains that form. In order to recover the target mechanical properties, AM components have to undergo post-process heat treatments. However, such heat treatments have to be custom designed for the AM process and the component geometry because of the expected vast differences in the microstructure at various locations of a component with complex geometry. The homogenization and precipitation steps should be optimized for the component so that target mechanical properties can be obtained throughout the part. The objective of this research is to utilize High Performance Computing in phase field simulations of microstructure evolution during post-processing of AM components. The physics-based modeling will be beneficial in reducing the experimental effort required for heat treatment process selection, optimization, and certification, thus leading to a significant reduction in energy consumption for AM and post-processing heat treatment. The optimization study will help identify heat treatments steps that are critical for development of a final desired microstructure with the minimum energy input. This combined with shortening of the production cycle (time-to-market) by reducing the number of failed parts (property targets), and reduction in the number of iterations for process optimization, will enable 30-40% savings in the energy costs. Phase field simulations of the degree of homogenization and the effect of local matrix composition on the nucleation and growth of competing precipitating phases were performed using the Microstructure Evolution Using Massively Parallel Phase Field Simulations code developed in-house at the Oak Ridge National Laboratory. The simulations were able to successfully capture the kinetics of nucleation and growth, and morphologies of various precipitating phases as a function of local matrix compositions and composition gradients characteristic of local microstructures arising from location-dependent variations in the thermal conditions. Future work will involve extending the simulations to a length scale consisting of multiple dendrites, so that the effect of homogenization on the coarsening of the dendrites can be simulated and used as an additional input to the optimization of the heat treatment process.

36 MATERIALS SCIENCE↗
DOE OSTI2013

Characterization of 430L porous supports obtained by powder extrusion moulding for their application in solid oxide fuel cells

The characterization of 430L stainless steel planar porous supports obtained by powder extrusion moulding was performed in this work. A thermoplastic multicomponent binder based on high density polyethylene and paraffin wax was selected for the process. Green supports were shaped by extrusion moulding, and subsequently the binder was removed by a thermal cycle previously optimized. Sintering was carried out at different temperatures in low vacuum. Density of sintered parts was measured by Archimedes' method and porosity was also evaluated through a microstructural analysis by optical microscopy. The porosity degree of samples sintered at low temperature was close to 35% which is a very suitable value for their application in SOFCs. Tensile tests were carried out in order to determine mechanical strength as a function of porosity degree. Based on these results, the best feedstock composition and processing parameters were selected. The oxidation behaviour in static air at high temperature was studied, and formed oxides were characterized in a scanning electron microscope equipped with energy dispersive analysis of X-rays. X-ray diffraction experiments were performed in order to identify the formed oxides based on formula Fe{sub 2−x}Cr{sub x}O{sub 3}. The results of these studies showed that this kind of ferritic stainless steel would be more suitable to be used as anodic supports where a rich hydrogen atmosphere is employed. Preliminary deposition tests allowed obtaining a homogeneous Ni–YSZ anode layer with a thickness of 10 μm on the porous metallic substrates. - Highlights: • 430L stainless steel porous supports were obtained by powder extrusion moulding. • Porosity degree was controlled sintering at different temperatures in low vacuum. • Tensile tests allowed determining mechanical strength of porous supports. • A study about its oxidation behaviour in static air at high temperature was realized. • After oxidation, formed oxides were characterized by EDS–SEM and XRD.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Upcycling of Mixed Aluminum Alloy Shredder Scrap using Shear Processing

Conservation of critical materials is an increasing area of focus in the Unites States. In 2023, aluminum was added to the US Department of Energy Final Critical Materials List which has spurred public and private research into sustainable management of these resources. Additionally, efficiency in manufacturing and conservation of natural resources are growing concerns with targets to lower global carbon emissions, as primary aluminum alloy production is energy intensive, requiring 14 MWh of electricity plus 0.4 tonnes of CO2 per tonne of Al. Due to these factors, is essential that more sustainable manufacturing methods for aluminum alloys are developed going forward. To this end, much research is ongoing on the topic of more efficient utilization and recovery. However, most of this research still requires primary aluminum in the production process. Here, it will be attempted to bypass the use of primary aluminum and produce useful material recycled from 100% post-consumer scrap. Even considering recent developments in recycling of Al scrap, there is still a large amount of post-consumer scrap that is underutilized due to high impurity content, and that amount will increase significantly as more and more aluminum alloys are utilized in vehicles. This “scrap wave” is expected to cover 80% of the demand for automotive aluminum alloys by 2050 . A challenge to be addressed before the coming scrap wave can be fully utilized is that the tolerance of manufacturing techniques to impurities or off-spec alloy compositions must be increased. Particularly, in 5000-and 6000-series alloys (the most common wrought alloys in durable products), excess iron, copper, and silicon create brittle intermetallics during casting that remain in the extruded microstructure which limit the formability, ductility, and corrosion resistance of the alloy. Concerningly, many of the highest-volume post-consumer aluminum scrap streams such as automotive shredder scrap contain a mix of alloys including both wrought and cast alloys. Their compositions can vary widely depending on geography and the time of year. Because they are mixed, they often contain high content of multiple alloying elements such as Si and Cu in higher concentrations than are found in typical wrought alloys. They may also be contaminated with non-Al alloys from fasteners that get mixed in and often have high content of unwanted elements such as Fe. As a method for utilizing these underused scrap streams that are high in tramp elements, an emerging extrusion technology is being developed at the Pacific Northwest National Laboratory (PNNL) that aims to upcycle 100% post-consumer aluminum scrap directly into extruded components without the addition of primary aluminum . This new technology, called Shear Assisted Processing and Extrusion (ShAPE), is enabling a shift away from today’s recycling paradigm by reaching deeper into lower-value scrap streams, using shredder scrap as the extrusion billet material. Sometimes referred to as Twitch or Tweak, these scrap streams result from shredding and sorting of automobiles, building materials, appliances, and consumer goods. ShAPE combines the linear axis of conventional extrusion with a rotating extrusion die. This rotating die applies large strain to the material during extrusion, which breaks up large impurity-containing intermetallic particles, reducing their deleterious effects. This has been demonstrated for 6063 machining scrap spiked with excess Fe, and Twitch scrap high in Fe, Si and Cu where strength and ductility were retained for both feedstock compositions. Additionally, the extreme plastic deformation during ShAPE enables extrusion of billets with high Si that are too brittle for processing by conventional extrusion. By using 100% post-consumer shedder scrap as feedstock, ShAPE has the potential to slash embodied energy and carbon in extruded components by >80% compared to conventional extrusion of primary aluminum alloys.

Milligan, Brian K.↗
DOE OSTI2026

Use of friction stir processing to synthesize nanocrystalline, grain boundary segregating Fe-Ti alloys

Grain boundary segregating alloys, a class of alloys designed such that nanocrystalline grain sizes are thermodynamically stabilized by the presence of high segregation energy solutes at the grain boundaries, are typically produced through geometrically limited processing techniques such as equal channel angular extrusion or thin film sputtering. Here, this study explores the use of friction stir processing (FSP) as a novel means of studying and producing these alloys using a test system of Fe-6at%Ti. Spot FSPs with a range of processing parameter sets were produced on bulk, coarse grained bars of material and optimal parameters were identified. Microscopy identified a range of processed materials which achieved nanocrystalline grains on the order of 100 nm, delineating a critical window of processing parameters which limit heat input while inducing sufficient plastic deformation for grain refinement. The finest grained nanocrystalline Fe-Ti achieved a hardness of 7.68 GPa, a significant increase in hardness over pure Fe with a similar microstructure due to increased dislocation density from FSP as well as several strengthening mechanisms produced through the presence and segregation of Ti. These results demonstrated the feasibility of using FSP to produce nanocrystalline grain boundary segregating alloys.

Fe alloys↗
DOE OSTI2024

Ink Casting and 3D‐Extrusion Printing of Yb 14 MnSb 11 for High‐Temperature Thermoelectric Material

Abstract Complex shapes are created from Yb 14 MnSb 11 , a high‐temperature thermoelectric Zintl phase, via a two‐step process: i) layer‐by‐layer 3D‐extrusion of ink containing partially‐reacted powders which are ball‐milled from a blend of Yb, MnSb, and Sb powders; ii) heat treatment to synthesize the ternary compound Yb 14 MnSb 11 and densify the extruded powders. A high phase purity for Yb 14 MnSb 11 (83–94%) is achieved in both cast and 3D‐extruded ink specimens via a solid‐state reaction between Yb, MnSb, and Yb 4 Sb 3 during reactive sintering. Pressure‐free sintering at temperatures of 1200–1400 °C densifies the powders to 82% relative density but can also induce the decomposition of the Yb 14 MnSb 11 phase due to Yb sublimation. A process window with optimized sintering temperature and time is identified, achieving both low porosity and high phase purity and reaching a maximum zT = 0.61 at 1000 °C, about half of the maximum zT value for bulk Yb 14 MnSb 11 made via conventional processes (pressure sintering of precursor powders). The present approach – direct ink writing of ball‐milled powders, combined with reactive sintering – is a scalable and affordable method to fabricate thermoelectric legs with intricate 3D shapes, for enhanced performances in high‐temperature thermoelectric applications.

Chen, Ming [Department of Materials Science &amp, ↗
DOE OSTI2019

Spark Plasma Extrusion and the Thermal Barrier Concept

Spark plasma sintering (SPS) is currently a major powder consolidation process with many advantages; however, it is still largely limited to the processing of simple shapes such as discs due to its geometric restrictions. Alternatively, spark plasma extrusion (SPE) is a recently developed process that has superiority over SPS in terms of faster consolidation, generating products of extended geometries and potential grain refinement capabilities under applied current. So far, work on SPE has resulted in large temperature gradients within the extruding material with microstructural and properties in-homogeneities. The present paper reports on a novel approach (thermal barrier concept) that allows the SPE of materials with enhanced uniformity in terms of microstructures and properties. Both aluminum and aluminum-carbon nanotube composites have been successfully processed using this new approach.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗
DOE OSTI2013

Optimization Using Metamodeling in the Context of Integrated Computational Materials Engineering (ICME)

Predictive Design Technologies, LLC (PDT) proposed to employ Integrated Computational Materials Engineering (ICME) tools to help the manufacturing industry in the United States regain the competitive advantage in the global economy. ICME uses computational materials science tools within a holistic system in order to accelerate materials development, improve design optimization, and unify design and manufacturing. With the advent of accurate modeling and simulation along with significant increases in high performance computing (HPC) power, virtual design and manufacturing using ICME tools provide the means to reduce product development time and cost by alleviating costly trial-and-error physical design iterations while improving overall quality and manufacturing efficiency. To reduce the computational cost necessary for the large-scale HPC simulations and to make the methodology accessible for small and medium-sized manufacturers (SMMs), metamodels are employed. Metamodels are approximate models (functional relationships between input and output variables) that can reduce the simulation times by one to two orders of magnitude. In Phase I, PDT, partnered with Mississippi State University (MSU), demonstrated the feasibility of the proposed methodology by employing MSU?s internal state variable (ISV) plasticity-damage model with the help of metamodels to optimize the microstructure-process-property-cost for tube manufacturing processes used by Plymouth Tube Company (PTC), which involves complicated temperature and mechanical loading histories. PDT quantified the microstructure-property relationships for PTC?s SAE J525 electric resistance-welded cold drawn low carbon hydraulic 1010 steel tube manufacturing processes at seven different material states and calibrated the ISV plasticity material parameters to fit experimental tensile stress-strain curves. PDT successfully performed large scale finite element (FE) simulations in an HPC environment using the ISV plasticity model in Abaqus FE analyses of the tube forming, sizing, drawing, welding, and normalizing processes. The simulation results coupled with the manufacturing cost data were used to develop prototype metamodeling (quick response) codes which could be used to predict and optimize the microstructure-process-property-cost relationships. The developed ICME metamodeling toolkits are flexible enough to be applied to other manufacturing processes (e.g. forging, forming, casting, extrusion, rolling, stamping, and welding/joining) and metamodeling codes can run on laptop computers. Based on the work completed in Phase I, in Phase II, PDT proposes to continue to refine the ISV model by correlating and incorporating the uncertainties in the microstructure, mechanical testing, and modeling. Following the model refinement, FE analyses will be simulated and will provide even more realistic predictions as they include an appropriate window of uncertainty. Using the HPC output (FE analyses) as input, the quick-response metamodel codes will more accurately predict and optimize the microstructure-process-property-cost relationships. Furthermore, PDT propose to employ the ICME metamodeling toolkits to help develop a new tube product using entirely new high strength steel. The modeling of the high strength steel manufacturing process will replace the costly and time consuming trial-and-error methods that were used in the tubing industry previously. This simulation-based process prototyping will greatly benefit our industrial partners by opening up new market spaces due to new products with greater capabilities.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Microstructure Evolution and Microhardness Distribution of Copper Processed Using Multiple Passes of Elliptical Cross-Sectional Spiral Equal-Channel Extrusion

The aim of this work is to study the effect of six-pass elliptical cross-sectional spiral equal-channel extrusion (ECSEE) on the microstructure and performance of ultrafine-grained (UFG) copper. Equiaxed grains of average grain size of less than 1 μm are formed into shear bands in the low strain region of ECSEE deformed specimen. More homogeneous and equiaxed microstructure with high misorientation angles is obtained in the high strain. Moreover, the microstructure evolution of ECSEE-induced copper is a dynamic equilibrium process of shear deformation accompanying the interactions of high dislocation density, cellular structure and high-angle grain boundaries. The grain ECSEE refinement mechanism is described as the formation process of dislocations, cells, local grain sub-boundaries rotation and large angle grain restructure. The significantly non-uniform hardness distribution is consistent with the deformation behavior and microstructure refinement in the ECSEE-induced specimen. The homogeneity of microstructure and hardness improves as the ECSEE pass increases.

36 MATERIALS SCIENCE↗
DOE OSTI2014

Fabrication of fine-grain tantalum diffusion barrier tube for Nb{sub 3}Sn conductors

Diffusion barriers used in Nb{sub 3}Sn wire are often fabricated by wrapping Ta sheet into a tube with an overlap seam. A common result of such practice is non-uniform deformation in the Ta sheet as it thins by wire drawing because of non-uniform grain size and texture in the original Ta sheet. Seamless Ta tube with a fine-grain and uniform microstructure would be much better for the diffusion barrier application, but such material is expensive and difficult to manufacture. This report presents results on a new fabrication strategy for Ta tube that shows promise for manufacture of less costly tube with an improved microstructure. The fabrication method begins with seam-welded tube but gives a fine-grain uniform microstructure with little difference between the longitudinal seam weld region and the parent metal after post-weld processing. Severe plastic deformation processing (SPD) applied by area reduction extrusion and tube equal channel angular extrusion (tECAE) are used to refine and homogenize the microstructure. Microstructure and mechanical property results are presented for Ta tubes fabricated by this new processing strategy.

36 MATERIALS SCIENCE↗
DOE OSTI2018

Reinforcement of Wood–Polymer Composites by Prestressed Elements

The reinforcement of wood–polymer composite beams and other long structural components by means of strong continuous prestressed elements is considered, in theoretical and practical terms. The use of plunger extrusion to introduce such reinforcement during the shaping process is proposed.

36 MATERIALS SCIENCE↗
DOE OSTI2011

Powder Metallurgy of Uranium Alloy Fuels for TRU-Burning Reactors Final Technical Report

Overview Fast reactors were evaluated to enable the transmutation of transuranic isotopes generated by nuclear energy systems. The motivation for this was that TRU isotopes have high radiotoxicity and relatively long half-lives, making them unattractive for disposal in a long-term geologic repository. Fast reactors provide an efficient means to utilize the energy content of the TRUs while destroying them. An enabling technology that requires research and development is the fabrication metallic fuel containing TRU isotopes using powder metallurgy methods. This project focused upon developing a powder metallurgical fabrication method to produce U-Zr-transuranic (TRU) alloys at relatively low processing temperatures (500ºC to 600ºC) using either hot extrusion or alpha-phase sintering for charecterization. Researchers quantified the fundamental aspects of both processing methods using surrogate metals to simulate the TRU elements. The process produced novel solutions to some of the issues relating to metallic fuels, such as fuel-cladding chemical interactions, fuel swelling, volatility losses during casting, and casting mold material losses. Workscope There were two primary tasks associated with this project: 1. Hot working fabrication using mechanical alloying and extrusion • Design, fabricate, and assemble extrusion equipment • Extrusion database on DU metal • Extrusion database on U-10Zr alloys • Extrusion database on U-20xx-10Zr alloys • Evaluation and testing of tube sheath metals 2. Low-temperature sintering of U alloys • Design, fabricate, and assemble equipment • Sintering database on DU metal • Sintering database on U-10Zr alloys • Liquid assisted phase sintering on U-20xx-10Zr alloys Appendices Outline Appendix A contains a Fuel Cycle Research & Development (FCR&D) poster and contact presentation where TAMU made primary contributions. Appendix B contains MSNE theses and final defense presentations by David Garnetti and Grant Helmreich outlining the beginning of the materials processing setup. Also included within this section is a thesis proposal by Jeff Hausaman. Appendix C contains the public papers and presentations introduced at the 2010 American Nuclear Society Winter Meeting. Appendix A—MSNE theses of David Garnetti and Grant Helmreich and proposal by Jeff Hausaman A.1 December 2009 Thesis by David Garnetti entitled “Uranium Powder Production Via Hydride Formation and Alpha Phase Sintering of Uranium and Uranium-Zirconium Alloys for Advanced Nuclear Fuel Applications” A.2 September 2009 Presentation by David Garnetti (same title as document in Appendix B.1) A.3 December 2010 Thesis by Grant Helmreich entitled “Characterization of Alpha-Phase Sintering of Uranium and Uranium-Zirconium Alloys for Advanced Nuclear Fuel Applications” A.4 October 2010 Presentation by Grant Helmreich (same title as document in Appendix B.3) A.5 Thesis Proposal by Jeffrey Hausaman entitled “Hot Extrusion of Alpha Phase Uranium-Zirconium Alloys for TRU Burning Fast Reactors” Appendix B—External presentations introduced at the 2010 ANS Winter Meeting B.1 J.S. Hausaman, D.J. Garnetti, and S.M. McDeavitt, “Powder Metallurgy of Alpha Phase Uranium Alloys for TRU Burning Fast Reactors,” Proceedings of 2010 ANS Winter Meeting, Las Vegas, Nevada, USA, November 7-10, 2010 B.2 PowerPoint Presentation Slides from C.1 B.3 G.W. Helmreich, W.J. Sames, D.J. Garnetti, and S.M. McDeavitt, “Uranium Powder Production Using a Hydride-Dehydride Process,” Proceedings of 2010 ANS Winter Meeting, Las Vegas, Nevada, USA, November 7-10, 2010 B.4. PowerPoint Presentation Slides from C.3 B.5 Poster Presentation from C.3 Appendix C—Fuel cycle research and development undergraduate materials and poster presentation C.1 Poster entitled “Characterization of Alpha-Phase Sintering of Uranium and Uranium-Zirconium Alloys” presented at the Fuel Cycle Technologies Program Annual Meeting C.2 April 2011 Honors Undergraduate Thesis by William Sames, Research Fellow, entitled “Uranium Metal Powder Production, Particle Distribution Analysis, and Reaction Rate Studies of a Hydride-Dehydride Process"

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2022

Interlayer fusion bonding of semi-crystalline polymer composites in extrusion deposition additive manufacturing

This work focuses on the evolution of interlayer fracture toughness properties of fiber-reinforced, semi-crystalline polymers in the extrusion deposition additive manufacturing (EDAM) process. Further, this work bridges the gap between the additive process conditions (time-temperature history) and the effective layer-to-layer fracture properties developed within a printed component. This is the first step to predict delamination that can occur during printing, during cooling to room temperature after printing, and during service performance of an additively manufactured geometry. A phenomenological model is developed for fusion bonding of semi-crystalline polymer matrix composites by coupling the interdiffusion of polymer chains with the evolution of polymer crystallinity. While the interdiffusion is captured by reptation theory of polymer dynamics, the evolution of crystallinity is modeled by phenomenological crystallization kinetics and crystal melting dynamics. Further, a methodology is developed to determine the critical strain energy release rate, G IC of the interlayer interface and experiments are conducted utilizing the double cantilever beam fracture test geometry. In conclusion, predictions of GIC as a function of thermal history are compared with experiments.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Effect of Internal Structure on Warpage in a Large-Scale Additive Manufacturing Process With Bio-Derived Composites

Extrusion-based large-format additive manufacturing (LFAM) often results in unintended deformation and failures due to thermal residual stress between layers. This LFAM involves a hot molten polymer deposited on a previously deposited and cooled layer, generating a temperature mismatch between the layers. The temperature discrepancy causes a thermal contraction mismatch, generating thermal residual stress. Due to the residual stress, printed structures experience warpage and delamination Therefore, understanding the heat distribution behavior is essential to preventing undesired deformation and failures. The goal of this study is to investigate the effect of infill patterns on heat distribution and deformation in an LFAM system. Wood fiber-reinforced polylactic acid was used as a sustainable and low-cost reinforcement material. A numerical model was developed to predict the temperature and deformation field with thermo-mechanical properties, which were measured by a dynamic mechanical analysis and a thermal expansion test. Simulations were performed on a box geometry with three different infill patterns. The simulation model was verified with temperature data gathered from an infrared camera. The results show good agreement between predicted and measured temperature profiles. The developed simulation model was applied to a roof tray with different infill patterns for a case study. We found that the different thermal mass distributions resulting from the various infill patterns affected the heat distribution and deformation. These findings contribute to a better understanding of the thermal and mechanical behavior of LFAM.

Jo, Eonyeon↗
DOE OSTI2022

A machine learning approach to determine the elastic properties of printed fiber-reinforced polymers

This work focuses on the simultaneous determination of the elastic constants and the fiber orientation state for a short fiber-reinforced polymer composite by performing a minimum of experimental tests. Here we introduce a methodology that enables the inverse determination of fiber orientation state and the in-situ polymer properties by performing tensile tests at the composite coupon level. We demonstrate the approach for the extrusion deposition additive manufacturing (EDAM) process to illustrate one application of the methodology, but the development is such that it can be applied to short fiber-reinforced polymer (SFRP) systems processed via other methods. Currently, developing composites additive manufacturing digital twins require extensive material characterization. In particular, the mechanical characterization of the orthotropic elastic properties of a composite involves extensive sample preparation and testing, therefore the elasticity tensor is generally populated using a micromechanics model. This, however, requires measuring the fiber orientation state in addition to knowing the constituent material properties. Experimentally measuring the fiber orientation state can be tedious and time consuming. Further, optical methods are limited to resolving the orientation of cylindrical fibers or cluster of non-cylindrical fibers, and computed tomography (CT) methods scan regions of volume that are much smaller than a full printed bead. Therefore, we propose a methodology, accelerated by machine learning, to identify the anisotropic mechanical properties and fiber orientation state at the same time. Early results show that inference of the fiber orientation and composite properties is possible with as few as three tensile tests. Our results show that a combination of the choice of the micromechanics model and reliable set of experiments can yield the nine elastic constants, as well as, the fiber orientation state.

36 MATERIALS SCIENCE↗
NASA NTRS2000

Solid Freeform Fabrication of Continuous Fiber Reinforced Composites for Propulsion Applications

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500'C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible- manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. This is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths With carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites-, they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP process.

Vaidyanathan, R.↗
NASA NTRS2001

Solid Free-Form Fabrication of Continuous Fiber Reinforced Composites for Propulsion Application

For propulsion related applications, materials must be able to demonstrate excellent ablation and oxidation resistance at temperature approaching 3500 C, adequate load bearing capabilities, non-catastrophic failure modes, and ability to withstand transient thermal shock. A potential list of propulsion-material property requirements includes, low density, high elastic modulus, low thermal-expansion coefficient, high thermal conductivity, excellent erosion and oxidation/corrosion resistance, and flaw-insensitivity. In many cases, they will also need to be able to be joined, survive thermal cycling and multi-axial stress states, and for reusable applications, the materials must maintain the above attributes after prolonged exposure to extremely harsh chemical environments. The final and possibly most important attribute for these materials are the need to be lower cost and readily available in large quantities. Recently, Advanced Ceramics Research, Inc. (ACR) has developed low cost, flexible-manufacturing processes for Zr & Hf-based carbon fiber reinforced composites, materials with good oxidation and ablation resistance up to 3500 C. This process, called Continuous Composite Co-extrusion (C(sup 3)), incorporates carbon fibers to fabricate 'in-situ' carbide and boride-matrix/carbon fiber composites. M is a variation of ACR's manufacturing process for low-cost structural ceramic materials called Fibrous Monoliths with carbon fiber reinforcements. Fibrous Monolithic materials have a distinct fibrous texture, consist of intertwined cells of a primary phase, separated by cell boundaries of a tailored secondary phase and show very high fracture energies, damage tolerance, and graceful failure. Since they are monolithic powder based composites; they can be manufactured by conventional powder processing techniques using inexpensive raw materials. This combination of high performance and low cost is a breakthrough that could enable wider application of ceramics in high temperature applications. Typical volume fractions of the two phases are 80 to 95% for the cell phase and 5 to 20% for the interpenetrating cell boundary phase. ACR is currently developing an innovative solid freeform form fabrication (SFF) approach to produce Hf and Zr based ceramic composite components reinforced with continuous carbon fiber tows for critical structural components such as tubes and blisks. The process is simple, robust and will be widely applicable to a number of material systems. This technique was originally developed at the University of Delaware Center for Composite Materials (UD-CCM) for rapid fabrication of polymer matrix composites by a technique called automated tow placement or ATP. The current process is being developed in collaboration with UD-CCM. The paper will detail the freeform fabrication process to create low-cost ceramic fiber reinforced composites for high-temperature applications. The results of mechanical properties and microstructural characterization will be presented, together with examples of complex shapes and parts. It is believed that the process will be able to create complex shaped parts for propulsion applications at an order of magnitude lower cost than current CVI and PIP processes.

Vaidyanathan, R.↗
NASA NTRSDate not supplied

Preserving and Curating the Moon: Adventures in Lunar Core Processing

The lunar crust is the most easily accessible part of the Moon to both remote sensing and sample analyses and provides an archive of information about planetary formation, crustal evolution, and contains a wealth of information about the origin of the Earth-Moon system [e.g., 1-5]. The Apollo mission returned 382 kg of rocks, soil and core samples. Studies of these lunar samples are crucial for our understanding of the Moon’s formation and geological evolution, and for the past 50 years these returned samples have provided the foundation for lunar science [5]. The returned samples are stored and cared for in the lunar curation facility at NASA’s Johnson Space Center. This facility is comprised of a large suite of clean rooms, sample vaults for pristine and return samples, thin section labs, core and saw rooms, storage and working areas, and ancillary labs all designed to minimize contamination from the environment and other samples. Some of the returned samples were intentionally set aside and left unopened. Recently, the Apollo Next Generation Sample Analysis (ANGSA) initiative was designed to examine these pristine samples so the next generation of lunar scientists can further our insight into the Moon’s history. Here, we present the meticulous process that involves preparing for, and ultimately opening, one of the unopened core samples: Apollo 17 drive tube 73002,0,which was collected on the Moon from a landslide deposit near Lara Crater by astronauts Gene Cernan and Jack Schmitt. In order to open, examine, and curate 73002,0withminimalpotential contamination, great care had to be taken prior to opening its container. Beginning18 months before extrusion of the sample, all core processing equipment was pulled out of storage, identified, sorted, cleaned, and purged with nitrogen gas. However, limited institutional memory has made this step challenging as most of the former core processors from the Apollo area have retired or passed away. Twelvemonths prior to extrusion, table-top rehearsals were initiated to identify equipment and learn how it fits together and operates. Five months before extruding the real core, preparations further evolved to include the extrusion and dissection of a lunar core simulant. In addition, a mock-up glovebox was designed and built to allow for a more realistic practice environment. One month prior to extrusion, the actual core cabinet was prepared for use, which included fitting it with lights, a webcam, and power. The tool and equipment cleaning procedure was also modified to include increased cleanliness and sterility requirements. While still sealed, the core was CT scanned at the University of Texas at Austin to maximize its scientific return. Days before the extrusion, witness plates and foil were deployed inside the core cabinet to monitor potential particle and organic contamination within the cabinet. On Nov. 5th, 2019, core sample 73002,0 was successfully opened and extruded(Fig.1). Dissection of 73002,0 began immediately afterwards and is still under way. Processing this sample will help us prepare for future sampling missions and core extrusions and will enable new scientific discoveries about the Moon.

C H Krysher↗