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NASA NTRS2013

Copper Multiwall Carbon Nanotubes and Copper-Diamond Composites for Advanced Rocket Engines

This paper reports on the research effort to improve the thermal conductivity of the copper-based alloy NARloy-Z (Cu-3 wt.%Ag-0.5 wt.% Zr), the state-of-the-art alloy used to make combustion chamber liners in regeneratively-cooled liquid rocket engines, using nanotechnology. The approach was to embed high thermal conductivity multiwall carbon nanotubes (MWCNTs) and diamond (D) particles in the NARloy-Z matrix using powder metallurgy techniques. The thermal conductivity of MWCNTs and D have been reported to be 5 to 10 times that of NARloy-Z. Hence, 10 to 20 vol. % MWCNT finely dispersed in NARloy-Z matrix could nearly double the thermal conductivity, provided there is a good thermal bond between MWCNTs and copper matrix. Quantum mechanics-based modeling showed that zirconium (Zr) in NARloy-Z should form ZrC at the MWCNT-Cu interface and provide a good thermal bond. In this study, NARloy-Z powder was blended with MWCNTs in a ball mill, and the resulting mixture was consolidated under high pressure and temperature using Field Assisted Sintering Technology (FAST). Microstructural analysis showed that the MWCNTs, which were provided as tangles of MWCNTs by the manufacturer, did not detangle well during blending and formed clumps at the prior particle boundaries. The composites made form these powders showed lower thermal conductivity than the base NARloy-Z. To eliminate the observed physical agglomeration, tangled multiwall MWCNTs were separated by acid treatment and electroless plated with a thin layer of chromium to keep them separated during further processing. Separately, the thermal conductivities of MWCNTs used in this work were measured, and the results showed very low values, a major factor in the low thermal conductivity of the composite. On the other hand, D particles embedded in NARloy-Z matrix showed much improved thermal conductivity. Elemental analysis showed migration of Zr to the NARloy-Z-D interface to form ZrC, which appeared to provide a low contact thermal resistance. These results are consistent with the quantum mechanics-based model predictions. NARloy-Z-D composites have relatively high thermal conductivities and are promising for further development.

Bhat, Biliyar N.↗

NASA NTRS2014

Evaluation of Geopolymer Concrete for Rocket Test Facility Flame Deflectors

The current paper presents results from a combined research effort by Louisiana Tech University (LTU) and NASA Stennis Space Center (SSC) to develop a new alumina-silicate based cementitious binder capable of acting as a high performance refractory material with low heat ablation rate and high early mechanical strength. Such a binder would represent a significant contribution to NASA's efforts to develop a new generation of refractory 'hot face' liners for liquid or solid rocket plume environments. This project was developed as a continuation of on-going collaborations between LTU and SSC, where test sections of a formulation of high temperature geopolymer binder were cast in the floor and walls of Test Stand E-1 Cell 3, an active rocket engine test stand flame trench. Additionally, geopolymer concrete panels were tested using the NASA-SSC Diagnostic Test Facility (DTF) thruster, where supersonic plume environments were generated on a 1ft wide x 2ft long x 6 inch deep refractory panel. The DTF operates on LOX/GH2 propellants producing a nominal thrust of 1,200 lbf and the combustion chamber conditions are Pc=625psig, O/F=6.0. Data collected included high speed video of plume/panel area and surface profiles (depth) of the test panels measured on a 1-inch by 1-inch giving localized erosion rates during the test. Louisiana Tech conducted a microstructure analysis of the geopolymer binder after the testing program to identify phase changes in the material.

Allgood, Daniel C.↗

NASA NTRS2014

MSFC Electrostatic Levitator (ESL) Rapid Quench System

The NASA Marshall Space Flight Center (MSFC) Electrostatic Levitator (ESL) Laboratory is a unique facility for investigators studying high-temperature materials. The laboratory boasts two levitators in which samples can be levitated, heated, melted, undercooled, and resolidified, all without the interference of a container or data-gathering instrument. The ESL main chamber has been upgraded with the addition of a rapid quench system. This system allows samples to be dropped into a quench vessel that can be filled with a low melting point material, such as a gallium or indium alloy. Thereby allowing rapid quenching of undercooled liquid metals. Up to 8 quench vessels can be loaded into the quench wheel, which is indexed with LabVIEW control software. This allows up to 8 samples to be rapidly quenched before having to open the chamber. The system has been tested successfully on several zirconium samples. Future work will be done with other materials using different quench mediums. Microstructural analysis will also be done on successfully quench samples.

SanSoucie, Michael P.↗

NASA NTRS2014

A Fully Non-metallic Gas Turbine Engine Enabled by Additive Manufacturing

The Non-Metallic Gas Turbine Engine project, funded by NASA Aeronautics Research Institute (NARI), represents the first comprehensive evaluation of emerging materials and manufacturing technologies that will enable fully nonmetallic gas turbine engines. This will be achieved by assessing the feasibility of using additive manufacturing technologies for fabricating polymer matrix composite (PMC) and ceramic matrix composite (CMC) gas turbine engine components. The benefits of the proposed effort include: 50 weight reduction compared to metallic parts, reduced manufacturing costs due to less machining and no tooling requirements, reduced part count due to net shape single component fabrication, and rapid design change and production iterations. Two high payoff metallic components have been identified for replacement with PMCs and will be fabricated using fused deposition modeling (FDM) with high temperature capable polymer filaments. The first component is an acoustic panel treatment with a honeycomb structure with an integrated back sheet and perforated front sheet. The second component is a compressor inlet guide vane. The CMC effort, which is starting at a lower technology readiness level, will use a binder jet process to fabricate silicon carbide test coupons and demonstration articles. The polymer and ceramic additive manufacturing efforts will advance from monolithic materials toward silicon carbide and carbon fiber reinforced composites for improved properties. Microstructural analysis and mechanical testing will be conducted on the PMC and CMC materials. System studies will assess the benefits of fully nonmetallic gas turbine engine in terms of fuel burn, emissions, reduction of part count, and cost. The proposed effort will be focused on a small 7000 lbf gas turbine engine. However, the concepts are equally applicable to large gas turbine engines. The proposed effort includes a multidisciplinary, multiorganization NASA - industry team that includes experts in ceramic materials and CMCs, polymers and PMCs, structural engineering, additive manufacturing, engine design and analysis, and system analysis.

manufacturing↗

NASA NTRS2015

A Fully Non-Metallic Gas Turbine Engine Enabled by Additive Manufacturing

The Non-Metallic Gas Turbine Engine project, funded by NASA Aeronautics Research Institute, represents the first comprehensive evaluation of emerging materials and manufacturing technologies that will enable fully nonmetallic gas turbine engines. This will be achieved by assessing the feasibility of using additive manufacturing technologies to fabricate polymer matrix composite and ceramic matrix composite turbine engine components. The benefits include: 50 weight reduction compared to metallic parts, reduced manufacturing costs, reduced part count and rapid design iterations. Two high payoff metallic components have been identified for replacement with PMCs and will be fabricated using fused deposition modeling (FDM) with high temperature polymer filaments. The CMC effort uses a binder jet process to fabricate silicon carbide test coupons and demonstration articles. Microstructural analysis and mechanical testing will be conducted on the PMC and CMC materials. System studies will assess the benefits of fully nonmetallic gas turbine engine in terms of fuel burn, emissions, reduction of part count, and cost. The research project includes a multidisciplinary, multiorganization NASA - industry team that includes experts in ceramic materials and CMCs, polymers and PMCs, structural engineering, additive manufacturing, engine design and analysis, and system analysis.

Ceramics↗

NASA NTRS2015

High Temperature Joining and Characterization of Joint Properties in Silicon Carbide-Based Composite Materials

Advanced silicon carbide-based ceramics and composites are being developed for a wide variety of high temperature extreme environment applications. Robust high temperature joining and integration technologies are enabling for the fabrication and manufacturing of large and complex shaped components. The development of a new joining approach called SET (Single-step Elevated Temperature) joining will be described along with the overview of previously developed joining approaches including high temperature brazing, ARCJoinT (Affordable, Robust Ceramic Joining Technology), diffusion bonding, and REABOND (Refractory Eutectic Assisted Bonding). Unlike other approaches, SET joining does not have any lower temperature phases and will therefore have a use temperature above 1315C. Optimization of the composition for full conversion to silicon carbide will be discussed. The goal is to find a composition with no remaining carbon or free silicon. Green tape interlayers were developed for joining. Microstructural analysis and preliminary mechanical tests of the joints will be presented.

Joining↗

NASA NTRS2016

Joining and Integration of Silicon Carbide-Based Materials for High Temperature Applications

Advanced joining and integration technologies of silicon carbide-based ceramics and ceramic matrix composites are enabling for their implementation into wide scale aerospace and ground-based applications. The robust joining and integration technologies allow for large and complex shapes to be fabricated and integrated with the larger system. Potential aerospace applications include lean-direct fuel injectors, thermal actuators, turbine vanes, blades, shrouds, combustor liners and other hot section components. Ground based applications include components for energy and environmental systems. Performance requirements and processing challenges are identified for the successful implementation different joining technologies. An overview will be provided of several joining approaches which have been developed for high temperature applications. In addition, various characterization approaches were pursued to provide an understanding of the processing-microstructure-property relationships. Microstructural analysis of the joint interfaces was conducted using optical, scanning electron, and transmission electron microscopy to identify phases and evaluate the bond quality. Mechanical testing results will be presented along with the need for new standardized test methods. The critical need for tailoring interlayer compositions for optimum joint properties will also be highlighted.

Ceramic Matrix Composites↗

NASA NTRS2018

Sphene Emotional: How Titanite Was Shocked When the Dinosaurs Died

Accessory mineral geochronometers such as zircon, monazite, baddeleyite, and xenotime are increasingly being recognized for their ability to preserve diagnostic microstructural evidence of hypervelocity processes. However, little is known about the response of titanite to shock metamorphism, even though it is a widespread accessory phase and U-Pb geochronometer. Here we report two new mechanical twin modes in titanite within shocked granitoids from the Chicxulub impact structure, Mexico. Titanite grains in the newly acquired International Ocean Discovery Program Site expedition 364 M0077A core preserve multiple sets of polysynthetic twins, most commonly with composition planes (K1), = ~{1̅11}, and shear direction (η1) = <110>, and less commonly with the mode K1 = {130}, η1 = ~<522>. In some grains, {130} deformation bands have formed concurrently with shock twins, indicating dislocation glide with Burgers vector b = [341] can be active at shock conditions. Twinning of titanite in these modes, the presence of planar deformation features in shocked quartz, and lack of diagnostic shock microstructures in zircon in the same samples highlights the utility of titanite as a shock indicator for a shock pressure range between ~12 and ~17 GPa. Given the challenges of identifying ancient impact evidence on Earth and other bodies, microstructural analysis of titanite is here demonstrated to be a new avenue for recognizing impact deformation in materials where other impact evidence may be erased, altered, or did not manifest due to low shock pressure.

Timms, Nicholas E.↗

NASA NTRS2019

Myco-Architecture off Planet: Growing Surface Structures at Destination

Our work focused on filling major select key technical knowledge gaps, and technical aspects to be addressed in a Phase II proposal were identified such as the secretion of glues or plastics by the fungi or bacteria to form biocomposites. Specifically, we raised the technical TRL by assessing the growth of in-house mycelial-producing strains on potential food substrates and analyzed the advantages and disadvantages to their use off planet. Growth of the mycelia on sawdust and powdered nutrients including dried, powdered algae, was used as a baseline. We measured growth as a function of temperature, tested the relevant material properties of the mycelia products produced, and measured the mass of input and output volume for production per volume of material. Mycotecture was produced in a bag simulating the proposed mission implementation. Post-production such as heat treatment (as is done with terrestrial mycotecture)was assessed.The material properties of the dried, frozen and baked mycelial outputs included density, strength,thermal insulation and flame retardation. Tensile/compression testing on biocomposite material specimens was performed to obtain three-dimensional elastic constants, as well as to examine deformation and fracture behavior. These mechanical tests were performed on both dormant and activated samples to understand the evolution of the structural material. In addition, experimental data obtained from the mechanical testing was used to build a failure prediction model that accounts for material anisotropy. This aided in future structural design through a quantitative understanding of the mechanical limits of the material. To examine the texture, defects, fracture surfaces of the material, high-resolution microstructural imaging was utilized before and after the mechanical tests. This microstructural analysis informed us about the macro-structural behavior and influenced structural design. Thermal decomposition analysis was also performed tounderstand the thermal limits.

Biocomposites↗

NASA NTRS2020

Efficient production of a high-performance dispersion strengthened, multi-principal element alloy

Additive manufacturing currently facilitates new avenues for materials discovery that have not been fully explored. In this study we reveal how additive manufacturing can be leveraged to produce dispersion strengthened (DS), multi-principal element alloys (MPEA) without the use of traditional mechanical alloying or chemical reactions. This new processing technique employed resonant acoustic mixing to coat an equiatomic NiCoCr powder with nano-scale yttrium oxides. Then, through laser powder bed fusion (L-PBF), the coated powder was successfully consolidated into 99.9% dense parts. Microstructural analysis confirmed the successful incorporation and dispersion of nano-scale oxides throughout the build volume. Furthermore, high temperature mechanical testing of the DS alloys showed significant improvements in strength and ductility over the baseline NiCoCr. As a result, this recently discovered processing route opens a new alloy design and production path that is synergistic between additive manufacturing and dispersion strengthening, possibly enabling a new generation of high-performance alloys.

T.M. Smith↗

NASA NTRSDate not supplied

Updates to the Predictive Materials Modeling Software Tools

Updates on NASA's efforts to build predictive material models from the micro-scale to the macro-scale are presented. To complement the mission design cycle process and reduce the need for extensive testing, NASA is developing modeling and simulation tools that enable characterizing material properties and response to hot plasma experienced during atmospheric entry. The PuMA (microstructure analysis), PATO (macroscale material response), SPARTA (direct simulation Monte Carlo) and ARCHeS (arc heater modeling) codes are described. A range of applications, encompassing calculating effective material properties, study of high shear boundary layer flow over woven materials, new model of silicone-based coatings, new model of mechanical erosion, as well as approach to loose multi-physics coupling, are presented.

material modeling↗

NASA NTRSDate not supplied

Computation of Effective Mechanical Properties and Mechanical Erosion Modeling of TPS Materials

The goal of this presentation is to provide a general overview of the multi-scale modeling formulation to determine if there is additional surface recession in Thermal Protection Systems (TPS) materials as a result of mechanical erosion due to high shear conditions during atmospheric entry. This modeling process is performed at different scales by leveraging two computational frameworks developed at NASA: the Porous Microstructure Analysis (PuMA) software, and the Porous material Analysis Toolbox based on OpenFOAM (PATO). PuMA specializes in computing effective macro-scale material properties by performing material response simulations on 3D digital micro-scale representations of porous micro-structures. The modeling of TPS materials at the micro-scale is essential to understand how they behave as part of a heat shield assembly. The first part of the presentation will detail the implementation of PuMA’s cell-centered finite volume elasticity solver, which allows the computation of macro-scale effective mechanical properties of heterogeneous and anisotropic materials such as fibrous and woven TPS composites. These homogenized mechanical properties are used by PATO’s mechanical erosion model to predict the TPS material’s recession at a larger scale. This work will also provide some examples of multi-scale analysis from the fiber level up to the unit cell. The second part of the presentation will focus on the macro-scale approach to determine if erosion at the heat shield’s surface occurs due to mechanical and thermal loads experienced during atmospheric entry. To accomplish this, a solid mechanics module was integrated within PATO enabling it to model the potential mechanical erosion in three steps: first, after obtaining the effective mechanical properties with PuMA, the implemented stress analysis solver computes the stress and the displacement fields for the TPS material using the wall shear stress tensor, computed using a CFD solver, as boundary conditions; then, regions on the surface where the stress meets the failure criteria are identified; finally, the failed material is removed and the mesh is redistributed accordingly. The outcome is a model capable of predicting the total recession in the material due to surface chemistry and mechanical erosion.

Mechanical Properties↗

NASA NTRSDate not supplied

Overview of Ablative TPS Modeling at NASA Ames

Over the past decade, NASA has invested in efforts to build predictive thermal protection system (TPS) material models from the micro-scale to the macro-scale. To complement the mission design cycle process and reduce the need for extensive testing, NASA is developing modeling and simulation tools that enable characterizing material properties and response to hot plasma experienced during atmospheric entry. Traditional material response and ablation modeling tools, such as the heritage code FIAT, and its multidimensional siblings, TITAN and 3dFIAT, are being complemented with newly developed software such as Icarus and PATO. Both of these programs are three-dimensional, finite-volume solvers that use unstructured meshes and 21st century programming paradigms to allow for efficient parallel simulations. FIAT and Icarus are also used for TPS sizing purposes. Today, these traditional tools are being supplemented with computational materials models at the atomistic level. The scales of interest range from computational chemistry (Density Functional Theory [DFT]), to atomistic simulations (Molecular Dynamics [MD]), to the microscale with the Porous Microstructure Analysis (PuMA) software that was recently awarded the 2022 NASA Software of the Year award. Finally, thermo-structural modeling is also of interest to the TPS Materials branch and done using commercial tools such as MSC MARC, MENTAT, NASTRAN and PATRAN. The present talk will also link the use of these computational tools to current NASA missions and projects associated with challenging and complex vehicles entries/reentries.

materials modeling↗

NASA NTRSDate not supplied

Thermochemical Interactions of Yttria-Stabilized Zirconia and Molten Lunar Regolith Simulants

Oxygen produced from lunar resources through in-situ resource utilization (ISRU) is critical to maintaining a permanent human presence on the lunar surface. Molten regolith electrolysis and carbothermal reduction are two promising ISRU techniques for generating oxygen directly from lunar regolith, which is primarily a mixture of oxide minerals; however, both processes require operating temperatures of 1600C to melt lunar regolith and dissociate the molten oxides. These conditions limit the use of many oxide refractory materials, such as Al2O3 and MgO, due to rapid degradation resulting from reactions between the refractory materials and molten lunar regolith. Yttria-stabilized zirconia (YSZ) is a promising refractory oxide to provide containment of molten regolith while demonstrating limited reactivity. This work focuses on corrosion studies of YSZ powders and dense YSZ crucibles in contact with molten lunar mare and highlands regolith simulants at 1600C. The interactions between YSZ and molten regolith are characterized using SEM/EDS, XRD, and EBSD with an emphasis on elemental and microstructural analysis to assess reactivity and degradation of YSZ. Due to lunar regolith’s similar composition to calcium-magnesium-aluminosilicates (CMAS) and YSZ’s usage as a thermal barrier coating, these interactions can serve to inform YSZ/CMAS behavior by simulating cases of elevated CMAS/YSZ ratios and for higher than intended gas turbine temperatures.

Kevin Yu↗

NASA NTRSDate not supplied

Simulation of Oxidative Etch Pit Formation and Growth on FiberForm

Erosion of carbon surfaces due to oxidation does not occur uniformly but through the formation of localized etch pits because of active surface sites. These active sites are formed due to the presence of atomic defects on the carbon surface and have much higher reactivity compared to average non-defective sites. Thus, these active sites are the first to react during ablation, resulting in their removal. This causes all the neighboring atoms to be defective, and increasing their reactivity, thus leading to localized carbon removal around these “active” sites. In this manner, these highly reactive defects serve as nucleation sites for the formation and growth of etch pits, with detrimental effects on the structural integrity. In order to understand the influence of these etch pits on the material properties of carbon fiber microstructures, we have developed a new capability within direct simulation Monte Carlo (DSMC) to capture the etch pit formation process. This capability is developed within the DSMC code SPARTA (Stochastic PArallel Rarefied-gas Time-accurate Analyzer) and can model the material removal in the presence of active sites leading to the formation of etch pits. The focus of the current work will be to study the effect of etch pits on the material properties of FiberForm, the precursor substrate of the PICA Thermal Protection System (TPS) material. The microstructure of virgin FiberForm obtained directly from X-ray microtomography scans is used within SPARTA to obtain the ablated geometries with etch pits. These pitted microstructures are then imported into the Porous Microstructure Analysis (PuMA) software and various material properties such as thermal conductivity, elasticity, and permeability are computed. The variation of these properties because of the complex evolution of the surface topology due to the formation of etch pits is studied and analyzed. Furthermore, the effect of pitting is compared to the case of uniform radial shrinking of fibers, which has been the standard for modelling ablation of carbon structures, and significant differences are observed. Thus, a physically realistic model of material removal through the formation of etch pits will be helpful in predicting the degradation of carbon-based TPS more accurately during oxidation; as well as other mechanisms such as spallation, which involves the removal of chunks of material into the flow due to the growth of etch pits. This will ultimately improve our understanding of the failure modes in these materials due to ablation.

DSMC↗

NASA NTRSDate not supplied

In-situ Imaging of Pyrolyzing Aerospace Materials

Tracking morphological changes of materials during heating is crucial to understand its response in fire protection, biofuel production, thermal protection systems (TPS) for hypersonic flight. As materials are heated, they undergo physical and chemical changes due to water loss, stretching or shrinking, pyrolysis and chemical reactions in the ambient environment. The effects of these changes can have a profound impact on the material’s performance, indicated by changes in on the porosity and volume. While materials such as wood shrink as they pyrolyze and lose mass, others swell due to their inherent characteristics when exposed to heat [1]. This study focuses on experiments conducted at the Advanced Light Source (ALS) beamline 8.3.2, where in situ micro-computed tomography (µ-CT) is performed on materials as they are being pyrolyzed. Through in situ µ-CT, the change in total volume and porosity can be obtained in real-time, allowing for better understanding of the underlying thermophysical and chemical processes as a function of temperature. This study also focuses on the implementation of the Porous Microstructure Analysis software (PuMA) [2] to obtain thermal conductivity, permeability, and other properties of the material from the 3D tomographies. The information gained from these tomographies will supplement microscale model development of material morphological change and will aid macroscale modeling for high-temperature applications. For this study, Room Temperature Vulcanizing silicone (RTV) [3-5] is heated from room temperature to 1000°C using an infrared lamp heating system, and tomographies are continuously collected as the sample is heated. The tomographies are then segmented to obtain solid and void phases, from which estimates of pore size, porosity and total volume are extracted as a function of temperature. PuMA is deployed on the segmented tomographies to obtain thermal conductivity, permeability, and other properties as a function of temperature. Preliminary results show that RTV first intumesces (swells) as pyrolysis begins, due to build-up of pyrolysis gases in closed pores, and then shrinks significantly as more open pores are formed and the pyrolysis gases outgas. Pore network visualization of the tomographies using OpenPNM [6] showed the increase in pore connectivity with increase in temperature. Future work will focus on using PuMA to obtain macroscopic properties of RTV as a function of temperature.

Tomography↗

NASA NTRSDate not supplied

Simulation of Oxidative Etch Pit Formation and Growth on FiberForm

DSMC↗

NASA NTRS2024

A Diversity of Temperature and Pressure Conditions Recorded by Zircon within Suevite from Ries Crater, Germany

The temperature and pressure conditions experienced by rocks during an impact event can be constrained using petrologic and microstructural analysis and is crucial to providing ground truth to the impact cratering process. Suevite is a polymict, impact melt-bearing breccia, specific to Ries crater in Germany. There are competing models for suevite formation and emplacement, such as clastic flows pushed out of the crater rim or ejecta plume fallback. Knowledge of the temperature and pressure pathways recorded by grains within the suevite can help distinguish between these and other models. The accessory phase zircon (ZrSiO4) and its high-pressure polymorph reidite are particularly useful in such circumstances as they are highly refractory minerals that can record the high-temperature and/or high-pressure conditions of an impact event. Here we present evidence for a wide array of temperature and pressure conditions recorded in zircon grains within a single thin section of suevite. Zircons in this study range from unshocked to highly shocked (>53 GPa), and record temperatures more than 1673 °C. These findings confirm previous studies concluding that suevites contain material exposed to very diverse pressure and temperature conditions during initial shock compression and excavation but do not, as a whole, experience extreme temperatures (>1673 °C) or pressures (>30 GPa).

mineralogy↗