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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 433 records · Page 24
All sourcesNASA NTRSDOE OSTI
NASA NTRS1992

Analysis of a space-exposed thermoplastic resin

The chemical characterization of a thermoplastic resin exposed to the low Earth orbit (LEO) environment for 10 months and for 5.8 years is reported. The resin, processed as a thick film and as a matrix for a graphite fiber reinforced composite, few exposed in the RAM direction on the NASA Long Duration Exposure Facility (LDEF). Differences attributable to environmental exposure were detected in infrared spectra and in various molecular weight parameters of film after 10 months in LEO. Those effects were not as apparent in composites after 5.8 years in LEO. Increased exposure to atomic oxygen toward the end of the LDEF mission probably scrubbed these effects from specimens exposed for 5.8 years. The intent of this study is to increase our fundamental understanding of space environmental effects on polymeric materials and to develop a benchmark for enhancing our methodology for and understanding of the ground-based simulation of space environmental effects.

Young, Philip R.↗
NASA NTRSDate not supplied

Production and Characterization of Additively Manufactured Radiator Panels with Integral Branching Heat Pipes for High-Temperature Heat Rejection

Emerging concepts for fission surface power and nuclear electric propulsion necessitate lightweight, mechanically robust, and thermally efficient heat rejection radiators. State-of-the-art intermediate-temperature (~400 K) composite radiator assemblies have been developed based on titanium-water heat pipes bonded to metal, graphite, and carbon-fiber-based panels. NASA has identified a need for new radiator concepts that can operate at even higher temperatures (500 – 600 K), minimize thermal resistances and thermal stress failures at bond interfaces, and approach areal densities of 2 – 3 kg m -2 . To meet these needs, our team is developing additively manufactured (AM) radiator panels with integral branching wicking heat pipe networks. Water is selected as the working fluid for this temperature range. Based on simulations and thermal vacuum experiments, these branching embedded heat pipe networks can efficiently distribute heat over panels for finned surface efficiencies of η f >70% at T H = 500 K input heat. This paper first presents laser powder-bed fusion AM strategies to produce embedded porous structures for wicking heat pipes in Inconel 718 and titanium alloys (commercially pure and Ti-6Al-4V alloys). Post-build chemical and thermal treatments are described that yield hydrophilic wicking surfaces for operation with water. Transient rate-of-rise experiments with water and acetone are reported that yield estimates for AM wick porosity (ϵ), permeability (K), and effective pore radius (r pore ). Based on the wick characterization results, small prototype radiator panels (75 × 125 mm) with integrated heat pipe networks were manufactured. Heat rejection performance data are presented from cold thermal vacuum testing, with heat input temperatures up to ~510 K. Future efforts will focus on improving heat pipe performance, optimizing radiator mass, and evaluating larger panels to assess scalability.

thermal management↗
NASA NTRS2024

Production and Characterization of Additively Manufactured Radiator Panels With Integral Branching Heat Pipes for High-Temperature Heat Rejection

Emerging concepts for fission surface power and nuclear electric propulsion necessitate lightweight, mechanically robust, and thermally efficient heat rejection radiators. State-of-the-art intermediate-temperature (~400 K) composite radiator assemblies have been developed based on titanium-water heat pipes bonded to metal, graphite, and carbon-fiber-based panels. NASA has identified a need for new radiator concepts that can operate at even higher temperatures (500 – 600 K), minimize thermal resistances and thermal stress failures at bond interfaces, and approach areal densities of 2 – 3 kg m -2 . To meet these needs, our team is developing additively manufactured (AM) radiator panels with integral branching wicking heat pipe networks. Water is selected as the working fluid for this temperature range. Based on simulations and thermal vacuum experiments, these branching embedded heat pipe networks can efficiently distribute heat over panels for finned surface efficiencies of η f >70% at T H = 500 K input heat. This paper first presents laser powder-bed fusion AM strategies to produce embedded porous structures for wicking heat pipes in Inconel 718 and titanium alloys (commercially pure and Ti-6Al-4V alloys). Post-build chemical and thermal treatments are described that yield hydrophilic wicking surfaces for operation with water. Transient rate-of-rise experiments with water and acetone are reported that yield estimates for AM wick porosity (ϵ), permeability (K), and effective pore radius ( r pore ). Based on the wick characterization results, small prototype radiator panels (75 × 125 mm) with integrated heat pipe networks were manufactured. Heat rejection performance data are presented from cold thermal vacuum testing, with heat input temperatures up to ~510 K. Future efforts will focus on improving heat pipe performance, optimizing radiator mass, and evaluating larger panels to assess scalability.

nuclear electric propulsion↗
NASA NTRS1985

Semi-2-interpenetrating polymer networks of high temperature systems

A semi-interpenetrating (semi-IPN) polymer system of the semi-2-IPN type is described in which a polymer of acetylene-terminated imidesulfone (ATPISO2) is cross linked in the presence of polyimidesulfone (PISO2). Six different formulations obtained by mixing of either ATPISO2-1n or ATPISO2-3n with PISO2 in three different proportions were characterized in terms of glass transition temperature, thermooxidative stability, inherent viscosity, and dynamic mechanical properties. Adhesive (lap shear) strength was tested at elevated temperatures on aged samples of adhesive scrim cloth prepared from each resin. Woven graphite (Celion 1000)/polyimide composites were tested for flexural strength, flexural modulus, and shear strength. The network polymers have properties intermediate between those of the component polymers alone, have greatly improved processability over either polyimide, and are able to form good adhesive bonds and composites, making the semi-2-IPN systems superior materials for aerospace structures.

Hanky, A. O.↗
DOE OSTI2025

Spatial distribution of sp 3 defects in carbon fibers via time-of-flight secondary ion mass spectrometry

Defects play a significant role in the material properties of carbon fibers (CF). Several defects result in the formation of sp 3 bonds in an otherwise sp 2 -dominant graphitic structure. Understanding the distribution of these defects within CF provides insight into their properties and the effect of manufacturing conditions. Reports showed time-of-flight secondary ion mass spectrometry (ToF-SIMS) is capable of characterizing the spatial distribution of sp 2 and sp 3 content in carbon materials. Here, ToF-SIMS was utilized to investigate the spatial distribution of sp 3 defects in T700, T1000, and M46 CF. M46 had the lowest sp 3 content. Center-to-edge analysis revealed that T700 CF had a gradient of sp 3 defects starting from the center and increasing to the edge, whereas M46 CF had a sudden increase in sp 3 defects roughly 1 μm from the edge. Comparatively, T1000 CF had a relatively uniform radial distribution of sp 3 defects, except for a newly identified sp 2 rich region at 0.8 μm from the center. This is hypothesized to originate from a skin–core structure that forms during CF manufacturing. As a result, this work demonstrates the utility of ToF-SIMS for characterizing the spatial distribution of sp 3 defects within CF, establishing new ways to understand CF formation.

Carbon fibers↗
DOE OSTI2025

In-Situ FTIR Detection of Transition Metal (TM)-Ion Dissolution From Cathodes in Li-Ion Batteries

Transition metal (TM) ions, commonly Ni and Mn, play a crucial role in Li-ion battery cathodes as the reaction centers for rapid redox reactions. A major challenge with TM-based cathodes is capacity degradation, particularly at higher operating voltages. This degradation is closely linked to the dissolution of TMs from the cathode materials and their subsequent deposition on the anode. This process not only modifies the surface structure of the cathode but, more significantly, alters the SEI composition on the anode [1-2]. The dissolution of TMs cations into a liquid electrolyte from cathode materials, such as Mn-ion dissolution from Mn-rich cathode (LMR), is detrimental to the cycling performance of Li-ion batteries [3-4]. Much attention has been paid to this issue but there remains a lack of characterization techniques which can detect the TM-ion dissolution from the cathode during electrochemical measurements. In our study, we use in-situ ATR-FTIR as an effective technique to probe the TM-ion dissolution from the cathode. We have first demonstrated the detrimental effects of TM ions on the electrochemical performance of Li-ion batteries by adding a small amount of TM salt (50 mM Mn(PF6)) to the electrolyte of a Li-ion coin cell with LFP and graphite electrode. We observed a rapid capacity fade after the first delithiation cycle. To investigate TM ion dissolution, we established a baseline IR spectrum for various TM solvation states (such as Mn and Ni) by measuring concentration-dependent IR spectra. This baseline spectrum helps us detect TM ion dissolution during battery cycling. In this work, we discuss in detail the effect of TM ions on the electrochemical performance of Li-ion batteries and the detection of TM ions during battery cycling using in-situ FTIR spectroscopy. We will compare TM dissolution between coated and uncoated cathodes to examine the effect of cathode coatings to mitigate degradation due to TM dissolution and cross-over from cathode to anode. References: (1) Zhan, C.; Wu, T.; Lu, J.; Amine, K. Dissolution, migration, anddeposition of transition metal ions in Li-ion batteries exemplified byMn-based cathodes - a critical review. Energy Environ. Sci. 2018, 11,243-257. (2) Jung, R.; Linsenmann, F.; Thomas, R.; Wandt, J.; Solchenbach,S.; Maglia, F.; Stinner, C.; Tromp, M.; Gasteiger, H. A. Nickel,Manganese, and Cobalt Dissolution from Ni-Rich NMC and TheirEffects on NMC622-Graphite Cells. J. Electrochem. Soc. 2019, 166,A378-A389. (3) Zhao, L.; Chenard, E.; Capraz, O. O.; Sottos, N. R.; White, S.R. Direct Detection of Manganese Ions in Organic Electrolyte by UV-Vis Spectroscopy. J. Electrochem. Soc. 2018, 165, A345-A348 (4) Zhang, Y.; Hu, A.; Xia, D.; Hwang, S.; Sainio, S.; Nordlund, D.;Michel, F. M.; Moore, R. B.; Li, L.; Lin, F. Operando characterization and regulation of metal dissolution and redeposition dynamics nearbattery electrode surface. Nat. Nanotechnol. 2023, 18, 790.

25 ENERGY STORAGE↗
NASA NTRS1995

Physical aging effects on the compressive linear viscoelastic creep of IM7/K3B composite

An experimental study was undertaken to establish the viscoelastic behavior of 1M7/K3B composite in compression at elevated temperature. Creep compliance, strain recovery and the effects of physical aging on the time dependent response was measured for uniaxial loading at several isothermal conditions below the glass transition temperature (T(g)). The IM7/K3B composite is a graphite reinforced thermoplastic polyimide with a T(g) of approximately 240 C. In a composite, the two matrix dominated compliance terms associated with time dependent behavior occur in the transverse and shear directions. Linear viscoelasticity was used to characterize the creep/recovery behavior and superposition techniques were used to establish the physical aging related material constants. Creep strain was converted to compliance and measured as a function of test time and aging time. Results included creep compliance master curves, physical aging shift factors and shift rates. The description of the unique experimental techniques required for compressive testing is also given.

Veazie, David R.↗
NASA NTRS1998

Development of High Conductivity Lithium-Ion Electrolytes for Low Temperature Cell Applications

NASA has continued interest in developing power sources which are capable of operating at low temperatures (-20 C and below) to enable future missions, such as the Mars Rover and Lander. Thus, under a program sponsored by the Mars Exploration Program, we have been involved in developing Li-ion batteries with improved low temperature performance. To accomplish this task, the focus of the research has been upon the development of advanced electrolyte systems with improved low temperature properties. This had led to the identification of a carbonate-based electrolyte, consisting of 1.0 M LiPF6 in EC + DEC + DMC (33:33:34), which has been shown to have excellent performance at -20 C in Li-ion AA-size prototype cells. Other groups are also actively engaged in developing electrolytes which can result in improved low temperature performance of Li-ion cells, including Polystor, Yardney, and Covalent. In addition to developing cells capable of operation at -20 C, there is continued interest in systems which can successfully operate at even lower temperatures (less than -30 C) and at high discharge rates (greater than C/2). Thus, we are currently focusing upon developing advanced electrolytes which are highly conductive at low temperatures and will result in cells capable of operation at -40 C. One approach to improve the low temperature conductivity of ethylene carbonate-based electrolytes involves adding co-solvents which will decrease the viscosity and extend the liquid range. Candidate solvent additives include formates, acetates, cyclic and aliphatic ethers, lactones, as well as other carbonates. Using this approach, we have prepared a number of electrolytes which contain methyl formate (MF), methyl acetate (MA), ethyl acetate (EA), ethyl proprionate (EP), and 1,2-dimethoxyethane (DME), some of which have been characterized and reported. Other groups have also reported electrolytes based on mixtures of carbonates and acetates. In the present study, electrolytes which have been identified to have good low temperature conductivity and stability were incorporated into lithium-graphite cells for evaluation. Using various electrochemical methods, including ac impedence and DC micropolarization techniques, the film formation characteristics of graphite electrodes in contact with various lectrolyte formulations was investigated.

Smart, M. C.↗
DOE OSTI2021

Probing the Reactivity of the Active Material of a Li-Ion Silicon Anode with Common Battery Solvents

Calculations and modeling have shown that replacing the traditional graphite anode with silicon can greatly improve the energy density of lithium-ion batteries. However, the large volume change of silicon particles and high reactivity of lithiated silicon when in contact with the electrolyte lead to rapid capacity fading during charging/discharging processes. In this report, we use specific lithium silicides (LS) as model compounds to systematically study the reaction between lithiated Si and different electrolyte solvents, which provides a powerful platform to deconvolute and evaluate the degradation of various organic solvents in contact with the active lithiated Si-electrode surface after lithiation. Nuclear Magnetic Resonance (NMR) characterization results show that a cyclic carbonate such as ethylene carbonate is chemically less stable than a linear carbonate such as ethylmethyl carbonate, fluoroethylene carbonate, and triglyme as they are found to be more stable when mixed with LS model compounds. Furthermore, guided by the experimental results, two ethylene carbonate (EC)-free electrolytes are studied, and the electrochemical results show improvements with graphite-free Si electrodes relative to the traditional ethylene-carbonate-based electrolytes. More importantly, the study contributes to our understanding of the significant fundamental chemical and electrochemical stability differences between silicon and traditional graphite lithium-ion battery (LIB) anodes and suggests a focused development of electrolytes with specific chemical stability vs lithiated silicon which can passivate the surface more effectively.

25 ENERGY STORAGE↗
NASA NTRS1986

Acoustic characterization of composite cure

The relationship between the time evolution of ultrasonic longitudinal velocities, measured in the course of the cure of 3501-6 neat and fiber-reinforced resin, and the time evolution of the degree of cure was studied. The resin samples were placed in a mold, one side of which was a graphite plate, while the rest was made of stainless steel. After placing the mold in a press and applying a single-cycle 5-MHz pulse to the transducer bonded to the outer side of the graphite plate, the echo resulting from the resin-graphite interface and the subsequent echoes from within the resin layer were recorded with a 200-MHz, 8-bit digitizer. The degree of cure was calculated from the acoustic response, using the relationships derived by Winfree and Parker (1986). The calculated degree of cure had the expected time dependence, and the agreement between the degree of cure measured for the neat resin and the prepreg was reasonable.

Parker, F. R.↗
NASA NTRS1990

Scaling effects in the static and dynamic response of graphite-epoxy beam-columns

Scale model technology represents one method of investigating the behavior of advanced, weight-efficient composite structures under a variety of loading conditions. It is necessary, however, to understand the limitations involved in testing scale model structures before the technique can be fully utilized. These limitations, or scaling effects, are characterized. in the large deflection response and failure of composite beams. Scale model beams were loaded with an eccentric axial compressive load designed to produce large bending deflections and global failure. A dimensional analysis was performed on the composite beam-column loading configuration to determine a model law governing the system response. An experimental program was developed to validate the model law under both static and dynamic loading conditions. Laminate stacking sequences including unidirectional, angle ply, cross ply, and quasi-isotropic were tested to examine a diversity of composite response and failure modes. The model beams were loaded under scaled test conditions until catastrophic failure. A large deflection beam solution was developed to compare with the static experimental results and to analyze beam failure. Also, the finite element code DYCAST (DYnamic Crash Analysis of STructure) was used to model both the static and impulsive beam response. Static test results indicate that the unidirectional and cross ply beam responses scale as predicted by the model law, even under severe deformations. In general, failure modes were consistent between scale models within a laminate family; however, a significant scale effect was observed in strength. The scale effect in strength which was evident in the static tests was also observed in the dynamic tests. Scaling of load and strain time histories between the scale model beams and the prototypes was excellent for the unidirectional beams, but inconsistent results were obtained for the angle ply, cross ply, and quasi-isotropic beams. Results show that valuable information can be obtained from testing on scale model composite structures, especially in the linear elastic response region. However, due to scaling effects in the strength behavior of composite laminates, caution must be used in extrapolating data taken from a scale model test when that test involves failure of the structure.

Jackson, Karen E.↗
DOE OSTI2020

Tracking nanoparticle growth in pulsed carbon arc discharge

The dynamics of nanoparticle growth in pulsed anodic arc discharge has been studied in time-resolved mode. To this end, a fast moving probe was employed to extract the material generated in a pulsed arc plasma held between two graphite electrodes. The probe motion was synchronized with the pulse phase and the exposure time to the plasma was set to 10 ms. The graphite anode was eroded in a helium atmosphere (300 Torr) by an arc plasma pulsed at 1 Hz with a 10% duty cycle and showing 250 A of peak current. The structure and morphology of the probe depositions were characterized by Raman spectroscopy, scanning electron microscopy, and focused ion beam. A maximal deposition rate of 260 μm/s was measured 5 mm away from the arc core during the active 0.1 s of the pulse. Such a rate yields a growth flux of 1.3 × 10 21 cm –2 s –1 , rich in carbon nanostructures (graphene platelets, nanotubes) with a characteristic aggregate size within 1–10 μm. The deposition during the inactive 0.9 s of the pulse was several orders of magnitude slower and consisted of amorphous carbon traces. Furthermore, the nanoparticle distribution along the collecting probe is correlated with the pulse phase, thereby providing information on particle transport. Pulsed nanosynthesis can be modeled as a periodical growth process, where the volume and propagation velocity of the growth region can be adjusted through modulation of the pulse signal waveform. The proposed model constitutes a suitable framework to investigate the pulsed arc synthesis of nanomaterials with tailored physical and chemical properties.

42 ENGINEERING↗
DOE OSTI2020

Detailed Characterization of an Annealed Reduced Graphene Oxide Catalyst for Selective Peroxide Formation Activity

Recently, electrochemical hydrogen peroxide (H 2 O 2 ) generation from oxygen molecules has been extensively studied. Thus far, the best peroxide activity under alkaline conditions has been reported at the surface of a mild reduced graphene oxide annealed at 600 °C (mrGO-600). However, the detailed material information, such as chemical functionality and structural morphology, is unknown, which results in ambiguous debates on its catalytic active sites. Therefore, to solve this problem, we intensively characterize the structure of mrGO-600 to clarify the origin of its catalytic activity. Various characterizations, including X-ray photoelectron spectroscopy, Raman spectroscopy, infrared spectroscopy, near-edge X-ray absorption fine spectroscopy, and high-resolution transmittance electron microscopy coupled with in situ infrared spectroelecrochemistry, reveal that the annealing process generates not only various hole edge defects that are related to the ring ether group but also numerous point defects that result in a small-sized disconnected graphitic carbon region. These defects are believed to form a unique atomic level configuration in mrGO-600, which enables it to facilitate high peroxide-generated activity from oxygen molecules in an alkaline electrolyte.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2021

Effect of graphitic anode surface functionalization on the structure and dynamics of electrolytes at the interface

Surface termination on a graphitic surface and the type of electrolytes in lithium-ion batteries (LIBs) play an important part in determining the structure, composition, and thus, the quality of the emergent solid electrolyte interphase. In this paper, we analyze the structure and dynamics of electrolyte molecules in multi-component electrolyte with varying species compositions combinatorially paired with four different graphitic surfaces terminated with hydrogen, hydroxyl, carbonyl, and carboxyl to explore the interplay between surface chemistry and electrolyte dynamics at electrode/electrolyte interfaces. Addition of dimethyl carbonate and fluoroethylene carbonate brought substantial changes in the ethylene carbonate (EC) and LiPF6 surface population density for hydroxyl and carbonyl surfaces. Strong density oscillation and drastic slowing of the dynamics of the electrolyte molecules at the interface are reported for all the systems. While these observations are universal, carboxyl surfaces have the strongest local and long-range effects. Characterization of the average dipole direction at the interface shows strong orientational preferences of ethylene carbonate molecules. EC molecules are preferred to be oriented either almost parallel or perpendicular to the hydroxyl surface, are tilted between parallel and perpendicular with a higher angle of incidence of the dipole vs surface normal on the carbonyl surface than on the hydroxyl surface, and are oriented perpendicularly against the carboxyl surface. These differences highlight the significant effect of graphite surface termination on the dynamics of the electrolytes and provide insight into the complex interplays between electrolyte species and graphite anode in LIBs.

Rustam, Sabiha (ORCID:0000000224248153)↗
NASA NTRS1980

Influence of excess diamine on properties of PMR polyimide resins and composites

By varying the stoichiometry of the reactants in the preparation of PMR polyimide resin, changes occur in molecular weight distribution which influence the rheological properties and thus the processability of the resin, as well as the mechanical properties of the composite. The influence of 1-10 percent molar excess MDA on the molecular weight distribution and rheological properties of an imidized PMR system were exposed. Molecular weight distribution is characterized by gel permeation chromatography of the imidized molding compound; shear viscosity is related to changes in average molecular weight. The thermo-oxidative stability at 600 F, glass transition temperature, flexural and interlaminar shear properties of PMR polyimide/Celion 6000 graphite fiber composites are compared as a function of the percent excess MDA in the monomer reactant mixture.

Hurwitz, F. I.↗
NASA NTRS1980

Influence of excess diamine on properties of PMR polyimide resins and composites

This preliminary study explores the influence of 1-10 percent molar excess MDA on the molecular weight distribution and rheological properties of an imidized PMR system. Molecular weight distribution is characterized by gel permeation chromatography of the imidized molding compound; shear viscosity is related to changes in average molecular weight. The thermo-oxidative stability at 600 F glass transition temperature, flexural and interlaminar shear properties of PMR polyimide/Celion 6000 graphite fiber composites are compared as a function of the percent excess MDA in the monomer reactant mixture.

Hurwitz, F. I.↗
NASA NTRS1993

LDEF polymeric materials: 10 months versus 5.8 years of exposure

The chemical characterization of several polymeric materials which received 10 months of exposure and 5.8 years of exposure on a Row 9 Long Duration Exposure Facility (LDEF) experiment (A0134) is reported. Specimens include fluorinated ethylene propylene (FEP) teflon film, polysulfone film, and graphite fiber reinforced epoxy amd polysulfone matrix composites. The responses of these materials to the two LEO exposures are compared. The results of infrared, thermal, x-ray photoelectron, and scanning electron microscope analyses are reported. Solution property measurements of various molecular weight parameters are presented for the thermoplastic polysulfone materials. Molecular level effects attributable to exposure that were present in 10-month exposed specimens were not found in 5.8-year exposed specimens. This result suggests that increased atomic oxygen fluence toward the end of the LDEF mission may have eroded away selected environmentally induced changes in surface chemistry for 5.8-year exposure specimens.

Young, Philip R.↗
DOE OSTI2023

Irreparable Interphase Chemistry Degradation Induced by Temperature Pulse in Lithium‐Ion Batteries

Abstract While it is widely recognized that the operating temperature significantly affects the energy density and cycle life of lithium‐ion batteries, the consequence of electrode‐electrolyte interphase chemistry to sudden environmental temperature changes remains inadequately understood. Here, we systematically investigate the effects of a temperature pulse (T pulse) on the electrochemical performance of LiNi 0.8 Mn 0.1 Co 0.1 O 2 (NMC811) pouch full cells. By utilizing advanced characterization tools, such as time‐of‐flight secondary‐ion mass spectrometry, we reveal that the T pulse can lead to an irreversible degradation of cathode‐electrolyte interphase chemistry and architecture. Despite negligible immediate impacts on the solid‐electrolyte interphase (SEI) on graphite anode, aggregated cathode‐to‐anode chemical crossover gradually degrades the SEI by catalyzing electrolyte reduction decomposition and inducing metallic dead Li formation because of insufficient cathode passivation after the T pulse. Consequently, pouch cells subjected to the T pulse show an inferior cycle stability to those free of the T pulse. This work unveils the effects of sudden temperature changes on the interphase chemistry and cell performance, emphasizing the importance of a proper temperature management in assessing performance.

Cui, Zehao↗