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All sources NASA NTRS DOE OSTI

DOE OSTI2020

Intrinsic size dependent plasticity in BCC micro-pillars under uniaxial tension and pure torsion

The mechanical behavior of submicron body-centered cubic (BCC) micro-pillars is investigated by three-dimensional dislocation dynamics (DD) simulations to better understand the governing mechanisms for size dependent plasticity under uniaxial tension and pure torsion. A formula is developed to compute the incremental plastic twist due to dislocation motion in DD simulations. The DD simulations show that different dislocation microstructures are created depending on the loading conditions, which leads to different size dependent mechanical behavior. While in tension plasticity is mainly governed by the kinetics of dislocation motion controlled partly by the surface dislocation sources, plastic flow in torsion is controlled by dislocation pile-ups associated with strain gradients. The simulation results also reveal a Bauschinger effect and plastic recovery under cyclic twist, which have been observed in recent experiments.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Characterization and Modeling of Deformation Induced Damage in Titanium Alloys

Over the lifetime of their DOE support, and specifically during the past funding cycle, the PIs have primarily focused on ambient temperature studies of the mechanisms of heterogeneous deformation and shear transfer at GBs. The PIs have developed and applied a broad array of experimental approaches complemented by advanced computational methods and simulations to enable new understanding of GB shear transfer, and a new approach for modeling this behavior at the mechanistic level has been established. The PIs have examined how slip behavior differs on the surface and interior of polycrystals using a variety of approaches. Some of the associated data has been used to generate 3-D models of experimentally-characterized microstructures that both support interpretation of deformation mechanisms as well as reveal where modeling needs to be improved to more closely agree with what is experimentally observed. The PIs progress in constitutive modeling of crystal plasticity has introduced explicit GB resistance to shear that depends on the mutual geometry of active slip systems. This past work places the PIs in a good position to take on the challenges associated with mechanistically understanding the interplay between GBS and slip interactions.

42 ENGINEERING↗

NASA NTRS2019

Modeling of the Influence of a Damaged Thermally Grown Oxide (TGO) Layer in an Environmental Barrier Coating System

Environmental barrier coatings (EBC) are an enabling technology for the successful application of ceramic matrix composites (CMCs) in air-breathing gas turbine engines. EBCs are susceptible to a number of failure modes including oxidation/delamination, recessions, chemical attack and dissolution, thermomechanical degradation, erosion, and foreign object impact damage in a combustion environment. Spallation of environmental barrier coating (EBC), induced by a thermally grown oxide (TGO) layer, is a key EBC failure mode. The TGO layer, resulting from steam oxidation, grows either from a silicon bond coat layer (if present) or from a silicon carbide (SiC) based substrate itself. The TGO layer evolves (i.e., thickness increases with time) as water vapor and oxygen gradually diffuse through the EBC, and the EBC spalls off once the TGO layer reaches some critical thickness. The critical thickness of the TGO layer for failure is in the range of 20-30 microns, but it can vary due to exposure temperature, microstructure etc. Current work at NASA Glenn Research Center, under the Revolutionary Tools and Methods (RTM) subproject is aimed at addressing associated failure modes in EBC systems and developing robust analysis tools to aid in the design/analysis of these systems. The objective of the current work is to conduct a sensitivity study to examine the influence of uniformly and non-uniformly grown oxide layers on the associated driving forces leading to spallation of the EBC when subjected to isothermal loading. The effect of damage in the TGO layer on the resulting stress states is also assessed both in uniform and non-uniform TGO layers.

Mital, Subodh K.↗

DOE OSTI2020

Elevated-temperature cyclic properties of advanced manufactured materials

Microreactor developers at the 2019 GAIN Microreactors workshop expressed a need for advanced manufacturing to fabricate microreactor components. Powder metallurgy (PM) hot isostatic pressing (HIP) is more mature than other advanced manufacturing techniques for the following reasons: 1. a code case exists for Section III, Division 1, Subsection NB components of light water reactors to be manufactured using PM HIP Alloy 316L, and 2. tensile and creep properties have been shown to be equivalent to wrought material for Type 316 stainless steel and Grade 91. Thus, PM HIP is more readily deployable in the near term. Elevated-temperature cyclic properties of PM-HIP materials, however, have not been established. The scope of testing for Code qualification could be significantly reduced compared to a new material for the following reasons: 1. only a limited amount of time consuming creep testing would be required, and 2. testing of fatigue and creep-fatigue behavior could be reduced if it can be demonstrated that the properties are comparable to wrought material. The objective of this work package is to develop an understanding of the relationship of advanced materials processing on the material characteristics as they relate to elevated-temperature component design and construction. This will be achieved by the following: • Elevated-temperature fatigue and creep-fatigue testing of PM HIP and wrought Alloy 316L. • Fracture and microstructural characterization of the PM HIP and wrought Alloy 316L. • Analysis of the elevated-temperature fatigue and creep-fatigue properties of PM HIP Alloy 316L. • Draft a report evaluating the elevated-temperature fatigue and creep-fatigue properties of PM HIP Alloy 316L. • Pursue procurement of Alloy 316H and Grade 91 manufactured using PM HIP. • Initiate scoping studies of the procured Alloy 316H or Grade 91 manufactured using PM HIP contingent upon successful material procurement.

36 MATERIALS SCIENCE↗

NASA NTRS2002

Processing of IN-718 Lattice Block Castings

Recently a low cost casting method known as lattice block casting has been developed by JAM Corporation, Wilmington, Massachusetts for engineering materials such as aluminum and stainless steels that has shown to provide very high stiffness and strength with only a fraction of density of the alloy. NASA Glenn Research Center has initiated research to investigate lattice block castings of high temperature Ni-base superalloys such as the model system Inconel-718 (IN-718) for lightweight nozzle applications. Although difficulties were encountered throughout the manufacturing process , a successful investment casting procedure was eventually developed. Wax formulation and pattern assembly, shell mold processing, and counter gravity casting techniques were developed. Ten IN-718 lattice block castings (each measuring 15-cm wide by 30-cm long by 1.2-cm thick) have been successfully produced by Hitchiner Gas Turbine Division, Milford, New Hampshire, using their patented counter gravity casting techniques. Details of the processing and resulting microstructures are discussed in this paper. Post casting processing and evaluation of system specific mechanical properties of these specimens are in progress.

Hebsur, Mohan G.↗

NASA NTRS2006

Robust Joining and Integration of Advanced Ceramics and Composites: Challenges, Opportunities, and Realities

Advanced ceramics and fiber reinforced composites are under active consideration for use in a wide variety of high temperature applications within the aeronautics, space transportation, energy, and nuclear industries. The engineering designs of ceramic and composite components require fabrication and manufacturing of large and complex shaped parts of various thicknesses. In many instances, it is more economical to build up complex shapes by joining simple geometrical shapes. In addition, these components have to be joined or assembled with metallic sub-components. Thus, joining and attachment have been recognized as enabling technologies for successful utilization of ceramic components in various demanding applications. In this presentation, various challenges and opportunities in design, fabrication, and testing of high temperature joints in advanced ceramics and ceramic matrix composites will be presented. Silicon carbide based advanced ceramics and fiber reinforced composites in different shapes and sizes, have been joined using an affordable, robust ceramic joining technology. In addition, some examples of metal-ceramic brazing will also be presented. Microstructure and high temperature mechanical properties of joints in silicon carbide ceramics and composites will be reported. Various joint design philosophies and design issues in joining of ceramics and composites will be discussed.

Singh, Mrityunjay↗

DOE OSTI2026

Circularity in Sequence-Controlled Copolyamides Enabled by Regioselective Enzymatic Hydrolysis

Sequence-controlled polymers enable precise control over macromolecular structures and function, but both their synthesis and end-of-life management remain fundamental challenges. Achieving high sequence fidelity is synthetically demanding, and conventional depolymerization methods lack regioselectivity, leading to irreversible loss of encoded molecular information and limiting polymer circularity. Enzymatic catalysis offers a potential solution by combining substrate specificity with selective bond cleavage. Here, we report the synthesis, characterization, and regioselective enzymatic depolymerization of poly- (X,AMA), a sequence-controlled copolyamide composed of alternating hexamethylenediamine−adipic acid (MA) and pxylylenediamine− adipic acid (XA) repeat units. Poly(X,AMA) was synthesized via solid-state polycondensation (SSP) of sequence-defined oligomers, enabling precise control over repeat-unit order. Polymer microstructure and sequence fidelity were confirmed by 13 C NMR spectroscopy and MALDI−TOF mass spectrometry. Comparison with a statistical copolymer analogue and Nylon-66 demonstrated pronounced differences in crystallinity, morphology, and thermal behavior arising from sequence control. Screening of 96 Nylon hydrolase homologues against poly(X,AMA) revealed strongly enzyme-dependent depolymerization profiles. While tetrad formation was generally favored, enzymes displayed pronounced sequence selectivity, preferentially releasing distinct sequence-defined tetrads XAMA or MAXA. SSP of sequence-defined tetrad MAXA produced a copolyamide with near identical monomer ordering as poly(X,AMA). Computational modeling of enzyme−substrate complexes identified structural features consistent with the observed regioselectivity. Together, these results establish selective enzymatic depolymerization as a viable strategy for the circular recycling of sequence-controlled polymers and provide a foundation for the rational engineering of enzymes for programmable polymer deconstruction.

Amides↗

DOE OSTI2020

Effect of subfreezing testing temperature on tensile mechanical behavior of fine-grained magnesium

Here, the effect of testing temperature on mechanical properties and deformation mechanisms was investigated by tensile testing of fine-grained magnesium samples under a range of temperatures (i.e. room temperature 20°C, subfreezing temperatures 0°C, -30°C, and - 60°C) and microstructural observations of both untested and tested samples using electron backscatter diffraction. The results suggest that mechanical properties and deformation mechanisms were significantly affected by lowering testing temperature. Strength increased linearly and ductility decreased linearly with the decrease of testing temperature. Although twinning is generally known to be athermal, this experimental study shows that tensile twinning is the dominating deformation mechanism at room temperature, and that twinning is negligible and dislocation operation is the primary deformation mechanism at 0°C, -30°C, and -60°C

36 MATERIALS SCIENCE↗

NASA NTRS2008

Bonding and Integration Technologies for Silicon Carbide Based Injector Components

Advanced ceramic bonding and integration technologies play a critical role in the fabrication and application of silicon carbide based components for a number of aerospace and ground based applications. One such application is a lean direct injector for a turbine engine to achieve low NOx emissions. Ceramic to ceramic diffusion bonding and ceramic to metal brazing technologies are being developed for this injector application. For the diffusion bonding, titanium interlayers (PVD and foils) were used to aid in the joining of silicon carbide (SiC) substrates. The influence of such variables as surface finish, interlayer thickness (10, 20, and 50 microns), processing time and temperature, and cooling rates were investigated. Microprobe analysis was used to identify the phases in the bonded region. For bonds that were not fully reacted an intermediate phase, Ti5Si3Cx, formed that is thermally incompatible in its thermal expansion and caused thermal stresses and cracking during the processing cool-down. Thinner titanium interlayers and/or longer processing times resulted in stable and compatible phases that did not contribute to microcracking and resulted in an optimized microstructure. Tensile tests on the joined materials resulted in strengths of 13-28 MPa depending on the SiC substrate material. Non-destructive evaluation using ultrasonic immersion showed well formed bonds. For the joining technology of brazing Kovar fuel tubes to silicon carbide, preliminary development of the joining approach has begun. Various technical issues and requirements for the injector application are addressed.

Halbig, Michael C.↗

DOE OSTI2020

Constitutive behavior and processing maps of a new wrought magnesium alloy ZE20 (Mg-2Zn-0.2Ce)

ZE20 (Mg-2Zn-0.2Ce) 2 is a new wrought magnesium alloy with improved extrudability and mechanical properties [1]. To understand the constitutive behavior and workability of this new alloy, Gleeble thermomechanical testing has been carried out in this study. The flow stress behavior of ZE20 was investigated between 250 °C–450 °C and 10 –3 s –1 –1.0 s –1 in isothermal compression. Constitutive descriptions of the flow stress are provided. A new general approach at application of the extended Ludwik equation is demonstrated and was found to be more accurate than the hyperbolic sine Arrhenius model while having a similar number of model constants. Processing maps were developed based on the experimental results and are verified with microstructural investigation. A region of safe processing with non-basal texture and high activity of dynamic recrystallization (DRX) was found between 375 °C and 450 °C, from 10 –1 s –1 to 10–2.5 s –1 . A region of potentially safe processing with annealing that is associated with shear band nucleation of non-basal grains was identified for temperatures as low as 300 °C and rates as high as 10 –1 s –1 .

36 MATERIALS SCIENCE↗

NASA NTRS1992

Creep fatigue life prediction for engine hot section materials (isotropic)

A series of high temperature strain controlled fatigue tests have been completed to study the effects of thermomechanical fatigue, multiaxial loading, reactive environments, and imposed mean stresses. The baseline alloy used in these tests was cast B1900+Hf (with and without coatings); a small number of tests of wrought INCO 718 are also included. A strong path dependence was demonstrated during the thermomechanical fatigue testing, using in-phase, out-phase, and non-proportional (elliptical and 'dogleg') strain-temperature cycles. The multiaxial tests also demonstrated cycle path to be a significant variable, using both proportional and non-proportional tension-torsion loading. Environmental screening tests were conducted in moderate pressure oxygen and purified argon; the oxygen reduced the specimen lives by two, while the argon testing produced ambiguous data. Both NiCoCrAlY overlay and diffusion aluminide coatings were evaluated under isothermal and TMF conditions; in general, the lives of the coated specimens were higher that those of uncoated specimens. Controlled mean stress TMF tests showed that small mean stress changes could change initiation lives by orders of magnitude; these results are not conservatively predicted using traditional linear damage summation rules. Microstructures were evaluated using optical, SEM and TEM methods.

Nelson, R. S.↗

NASA NTRS2006

Evaluation of Open Cell Foam Heat Transfer Enhancement for Liquid Rocket Engine

As NASA pursues the exploration mission, advanced propulsion for the next generation of spacecraft will be needed. These new propulsion systems will require higher performance and increased durability, despite current limitations on materials. A break-through technology is needed in the thrust chamber. In this paper the idea of using a porous metallic foam is examined for its potential cooling enhancement capabilities. The goal is to increase the chamber wall cooling without creating an additional pressure drop penalty. A feasibility study based on experiments at laboratory-scale conditions was performed and analysis at rocket conditions is underway. In the experiment, heat transfer and pressure drop data were collected using air as the coolant in a copper or nickel foam filled annular channel. The foam-channel performance was evaluated based on comparison with conventional microchannel cooling passages under equal pressure drop conditions. The heat transfer enhancement of the foam channel over the microchannel ranges from 130% to 172%. The enhancement is relatively independent of the pressure drop and increases with decreasing pore size. A direct numerical simulation model of the foam heat exchange has been built. The model is based on the actual metal foam microstructure of thin ligaments (0.2- 0.3 mm in diameter) that form a network of interconnected open-cells. The cell dimension is around 2 mm. The numerical model was built using the FLUENT CFD code. Comparison of the pressure drop results predicted by the current model with those experimental data of Leong and Jin [8] shows favorable comparisons. Pressure drop predictions have been made using hydrogen as a coolant at typical rocket conditions. Conjugate heat transfer analysis using the foam filled channel is planned for the future.

Chung, J. N.↗

DOE OSTI2026

Role of Si substitution in modulating the coercivity and magnetic anisotropy in Fe3CoB2 nanocrystallites

In this work, we report the impact of Si substitution on the structural and magnetic properties of Fe3CoB2 nanocrystallites as a rare-earth-free hard-magnet candidate. X-ray diffraction confirmed the formation of the tetragonal phase with an average crystallite size of ∼40 nm, while the transmission electron microscopy image revealed nanosized crystallites embedded in an amorphous matrix. Room-temperature Mössbauer spectra exhibited two sextets and two doublets, indicating magnetically ordered Fe sites in the tetragonal phase along with high-spin paramagnetic FeIII species in disordered regions. ZFC–FC magnetization curves displayed field-dependent blocking behavior, consistent with paramagnetic Fe species. Singular point detection measurements revealed a high anisotropy field of ∼10.7 kOe in the pristine Fe3CoB2, and systematically decreased with Si substitution. Magnetization measurements revealed a monotonic decrease in saturation magnetization with Si content, while coercivity was observed to increase, likely due to microstructural refinement. These results establish Fe3CoB2 as a rare-earth-free material with strong magnetic anisotropy, ideal for hard magnets.

Abbas, Hur [Department of Physics, University of T↗

DOE OSTI2026

High pressure effects on EBC systems in high temperature environments

Environmental barrier coatings (EBCs) are designed to protect SiCfiber/SiCmatrix ceramic matrix composites (CMCs) in turbine engines by mitigating wear in high-temperature water vapor environments. The failure of EBCs is frequently attributed to the accelerated oxidation of the silicon bond coating layer when exposed to high-temperature steam, leading to the formation of a thickened thermally grown oxide (TGO). TGO growth increases interfacial stress, weakens adhesion, and results in coating spallation. Understanding the impact of high-temperature oxidation of EBC systems is essential for developing accurate lifespan models for turbine components, although pressurized oxidation testing is extremely sparse in the open literature. In this work, oxidation tests were performed on rare earth silicate EBCs coated onto SiC substrates under increased pressure conditions. The coated specimens were tested at 1100°C, 1200°C, and 1300°C at both 1 atm and 10 atm total pressure in steam environments. Subsequent characterization focused on the microstructural evolution of the EBC/Si/SiC system. The experimental findings indicated that TGO behavior is dependent on high-pressure conditions, with elevated pressure leading to an increase in oxide scale thickness and modifications in its morphology.

Ardrey, Kristyn [ORNL] (ORCID:0000000184407796)↗

DOE OSTI2021

Experimental and computational analysis of bending fatigue failure in chopped carbon fiber chip reinforced composites

With a better balance among good mechanical performance, high freedom of design, and low material and manufacturing cost, chopped carbon fiber chip reinforced sheet molding compound (SMC) composites show great potential in different engineering applications. Here in this paper, bending fatigue behaviors of SMC composites considering the heterogeneous fiber orientation distributions have been thoroughly investigated utilizing both experimental and computational methods. First, four-point bending fatigue tests are performed with designed SMC composites, and the local modulus is adopted as a metric to represent the local fiber orientation of two opposing sides. Interestingly, SMC composites with and without large discrepancy in local modulus of opposing sides show different fatigue behaviors. Interrupted tests are conducted to explore the bending fatigue failure mechanism, and the damage processes of valid specimens are also closely examined. We find that the fatigue failure of SMC composites under four-point bending is governed by crack propagation instead of crack initiation. Because of this, the heterogeneous local fiber orientations of both sides of the specimen influence fatigue life. The microstructure of the lower side shows a direct influence while that of the upper side also exhibiting influence which becomes more prominent for high cycle fatigue cases. Furthermore, a hybrid micro–macro computational model is proposed to efficiently study the cyclic bending behavior of SMC composites. The region of interest is reconstructed with a modified random sequential absorption algorithm to conserve all the microstructural details including the heterogeneous fiber orientation, while the rest of the regions are modeled as homogenized macro-scale continua. Combined with a framework to capture the progressive fatigue damage under cyclic bending, the bending fatigue behaviors of SMC composites are accurately captured by the hybrid computational model comparing with our experimental analysis.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Combinatorial measurement of critical cooling rates in aluminum-base metallic glass forming alloys

Direct measurement of critical cooling rates has been challenging and only determined for a minute fraction of the reported metallic glass forming alloys. Here, we report a method that directly measures critical cooling rate of thin film metallic glass forming alloys in a combinatorial fashion. Based on a universal heating architecture using indirect laser heating and a microstructure analysis this method offers itself as a rapid screening technique to quantify glass forming ability. We use this method to identify glass forming alloys and study the composition effect on the critical cooling rate in the Al–Ni–Ge system where we identified Al 51 Ge 35 Ni 14 as the best glass forming composition with a critical cooling rate of 10 4 K/s.

36 MATERIALS SCIENCE↗

DOE OSTI2021

Post-irradiation examination of legacy high burnup fuel to support safety testing

Safety/transient testing to evaluate performance under off-normal conditions is an essential pillar for both the development of Accident Tolerant Fuels (ATF) and the optimization of fuel operation economics beyond current discharge burnups. Among other factors, the successful interpretation of the transient testing results relies upon the knowledge of the initial conditions of the test, including the characteristics of the fuel system under scrutiny. When testing pre-irradiated material, the assumptions that the fuel and the cladding still have the same properties as in the pre-irradiation stage is obviously wrong and could affect the results of the test. This is particularly true the more burnup accumulates in the fuel rod and irradiation progresses. The knowledge of the initial microstructure of both fuel and cladding allows a clearer interpretation of the subsequent transient testing results, provides validation of the physical phenomena underlying the model predictions and eliminates the uncertainties related to the limited knowledge of the sample status before the test. One example is the phenomenon of fine fragmentation that occurs in Light Water reactor (LWR) fuel. During a Loss of Coolant Accident (LOCA) or Reactivity Initiated Transient (RIA) the fuel can severely fragment. During LOCA, high burnup fuel tend to finely fragment, which has raised safety concerns due to the increased likelihood of dispersal of such small particles once the cladding has burst and due to the increased fission gas release. Therefore, efforts have been devoted to the assessment of a pulverization threshold that could determine the conditions under which fine fragmentation is predominant. However, the lack of information regarding the initial conditions of the fuel, and the connections between those conditions and the pre-transient irradiation history, have hindered the development of a fully mechanistic fragmentation and pulverization criterion. The empirical relationships rely on conservative estimations, due to the lack of information on critical material properties and characteristics. More generally, experimental evidence of the irradiation-induced modifications at microstructural scale are necessary to determine the behavior of the material at the macroscopic scale, with the latter being the one of technological interest. Significant progress has been made in the last two decades in the developments of analytical materials science techniques that can be applied to highly radioactive materials, such as high burnup fuels. The availability of new techniques and the improvement of existing ones has enabled investigations previously not possible that can deepen the understanding of the fuel characteristics and properties at high burnup. The better knowledge of material behavior and irradiation-induced phenomena could help the prediction of its performance. In this context, the scope of the present work is to apply a wide portfolio of advanced characterization techniques to determine properties that are relevant for safety and performance. The results are interpreted in the context of engineering scale post-irradiation examinations and available information on the irradiation conditions.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

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.↗