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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 37 records · Page 2
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Direct reuse of graphite and lithium nickel manganese cobalt oxide (NMC) recovered from ultrafast-laser ablation debris in Li-ion battery electrodes

Here we demonstrate that debris collected from the ultrafast-laser ablation of graphite anodes can be directly reused in a lithium-ion battery with little to no negative effects on electrochemical performance. Further, we show that while post-ablation NMC (LiNi 0.33 Mn 0.33 Co 0.33 O) cathode debris will require additional processing before being incorporated into an electrode, its critical materials (nickel, manganese, and cobalt) are not lost during ablation and can be recovered for recycling. Pre- and post-ablation materials are characterized with a suite of diagnostics, including SEM, TEM, X-ray CT, EDS, and XRD, to study changes in material morphology, composition and crystal structure. Graphite exhibited little to no morphological or compositional changes and a slight annealing of its crystal structure. NMC underwent profound morphological and crystallographic changes, but retained its elemental composition. Finally, post-ablation materials were re-manufactured into electrodes and cycled vs lithium metal. Graphite showed equal or better capacity and Coulombic efficiency compared to pre-ablation electrodes, while the post-ablation NMC exhibited severely reduced electrochemical performance. Furthermore, we discuss the outlook for application of this work to advanced manufacturing lines that produce next-generation, laser-patterned electrodes.

25 ENERGY STORAGE↗
DOE OSTI2022

Illitization in the Mt. Simon Sandstone, Illinois Basin, USA: Implications for carbon dioxide storage

Clay mineral cementation is one of the most important controls on sandstone reservoir properties. Here, in this paper, the diagenetic history of the Mt. Simon reservoir complex is studied to reveal the origin, timing, and controls of illitization. Samples of sandstone and shale from Mt. Simon reservoir complex were acquired from the Illinois Basin–Decatur Project (IBDP), a CO 2 storage demonstration project in the central Illinois Basin. Petrographic, SEM, TEM, XRD analyses and K/Ar age dating were completed to identify the major detrital and diagenetic components of the samples and reveal illite to be the major clay component in all samples. Illitic clay coatings in the lower Mt. Simon reservoir are identified as a major control on reservoir properties by inhibiting major precipitation of authigenic quartz during illitization, resulting in highly permeable sandstone, essential for CO 2 storage. The coating box-work morphology and mineralogy are indicative of a detrital smectite origin with subsequent illite growth associated with feldspar dissolution and kaolinite alteration. The mineralogy of bulk material and separate grain size fractions (2–0.6 μm; 0.6–0.2 μm; < 0.2 μm) with illite polytypes 2M 1 , 1M, and 1M d were quantified and age dated via 40 K- 40 Ar methods. The shales or reservoir seals contain the highest proportions of detrital illite with illite in the lower Mt. Simon Sandstone reservoir identified as solely diagenetic. Two major events of illitization are identified throughout the Mt. Simon with more porous reservoir rock exhibiting the older event from approximately 360 to 315 Ma and tighter sandstone units with reservoir properties too low to be considered reservoir exhibiting illite dates from 250 to 220 Ma. This partitioning of illitization is attributed to varied mineralogy controlled by depositional changes and evolution of the greater basin.

58 GEOSCIENCES↗
DOE OSTI2025

Microstructure and mechanical behavior of a TiC nanoprecipitate strengthened V Alloy

The V-4Cr-4Ti (V44) alloys have been proposed as the prime candidate structural material for self-cooled liquid Li blanket and other designs for fusion energy applications. However, the applications of the V44 alloy are limited to a narrow operation temperature window, due to reduction in creep strength at or above 700 °C and susceptibility to irradiation hardening and embrittlement when irradiated below 400 °C. Here, in this work, we explore the feasibility of designing a novel V alloy to form a high number density of TiC nanoprecipitates, in order to simultaneously improve creep strength and provide defect sinks to mitigate irradiation hardening. Computational thermodynamics was used to design a new alloy (V44C) to achieve our goal of high TiC nanoprecipitates density within the alloy V44 matrix. To ensure scalability, the new alloy was made through arc-melting and ingot-casting followed by hot forging, cold rolling and heat treatments of homogenization and precipitation aging. The microstructure was characterized by SEM, TEM, XRD and APT, confirming the existence of nanoprecipitates predicted in the thermodynamic calculations. In addition to microstructural evaluation tensile properties at room temperature and 700 °C, and Charpy impact energy at room temperature were measured. The microstructure and mechanical properties were then compared with those from a historic reference V44 alloy. The tensile strength improvement in V44C was rationalized based on particle and solid solution strengthening mechanism. The fracture behavior was discussed based on the fractography results and necking deformation behavior.

Alloys development↗
DOE OSTI2025

Direct ink writing of shear exfoliated two-dimensional nanomaterial- elastomeric multifunctional nanocomposite

Direct ink writing (DIW) of polymer nanocomposites with high loadings of two-dimensional (2D) nanofillers (graphene and hexagonal boron nitride (hBN)) is challenging because of potential clogging, use of hazardous solvents, and agglomeration. Here, in this work, a shear exfoliation and sieving method to prepare DIW ink with high loading of nanofillers produced from low-cost bulk layered materials such as graphite and bulk hBN powder for successful DIW printing without the use of any solvents, binders, or plasticizers. The single-step exfoliation technique resulted in a composite with substantial layer reduction along the c-axis, as confirmed by SEM, TEM, XRD, and Raman analysis. Incorporating exfoliated graphene (40 wt%) increased viscosity by ∼6 orders of magnitude due to enhanced particle–matrix interactions, leading to pronounced yield stress behavior and a yield stress of approximately 1598 Pa, which enabled excellent shape retention during extrusion. Using the DIW technique, porous structures such as desalination membranes, self-sensing bone scaffolds, thermal management coating, and serpentine strain sensors were fabricated. When tested in a direct contact membrane distillation setup, the fabricated membrane demonstrated a promising permeate flux of 21.85 Lm −2 h −1 and a salt rejection of 74.3 %. The fabricated serpentine sensor exhibited stable signal variations under cyclic tensile loading, with a working range of 0–200 % strain and a maximum gauge factor of 43,735. A cell culture test using the printed bone scaffold demonstrated promising cell attachment and proliferation. The DIW printed hBN nanocomposite exhibited reversible shape change under heat, demonstrating potential 4D printing capability and efficient thermal management when exposed to high heat or flame.

Desalination↗
DOE OSTI2022

Removal and recovery of ammonia from simulated wastewater using Ti3C2Tx MXene in flow electrode capacitive deionization

Abstract Flowing electrode capacitive deionization systems (FE-CDI) have recently garnered attention because of their ability to prevent cross contamination and operate in uninterrupted cycles ad infinitum. Typically, FE-CDI electrodes suffer from low conductivity, reducing deionization performance. Utilization of higher mass loadings to combat this leads to poor rheological properties. Herein, Ti 3 C 2 T x MXene was introduced as 1 mg mL −1 slurry electrodes in an FE-CDI system for the removal and recovery of ammonia from simulated agricultural wastewater. The electrode performance was evaluated by operating the FE-CDI system with a feed solution of 500 mg L −1 NH 4 Cl running in batch mode at a constant voltage of 1.20 and −1.20 V in charging and discharging modes, respectively. Despite the low loading, Ti 3 C 2 T x flowing electrodes showed markedly improved performance, achieving 60% ion removal efficiency in a saturation time of 115 min with an adsorption capacity of 460 mg g −1 . To understand the high adsorption performance of the electrodes, physiochemical and structural analysis was done via a variety of characterization techniques such as SEM, TEM, XRD, DLS, and Raman spectroscopy. Cyclic voltammetry and galvanostatic charge/discharge profiles were obtained to evaluate the electrochemical properties of the electrodes. The system proved to be an energy-saving technology by exhibiting a charge efficiency of 58–70% while operating at an energy consumption of 0.45 kWh kg −1 . A 92% regeneration efficiency showed that the electrodes were stable and suitable for long term and scalable usage. The results demonstrate that MXenes have the potential to improve the FE-CDI process for energy-efficient removal and recovery of ammonia.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Use of imaging and mass spectrometry-based capabilities to describe microbiome interactions (Q4 Performance Metric Report, 2021)

The LLNL “Microbes Persist” Soil Microbiome Scientific Focus Area (SFA) seeks to determine how microbial soil ecophysiology, population dynamics, and microbe-mineral-organic matter interactions regulate the persistence of microbial residues and formation of soil carbon (C). In much of our research, we use imaging, mass spectrometry, and related methods to study plantmicrobe-mineral interactions, viral and microbial particles from soil, and the signatures plant and microbial necromass contribute as part of soil organic matter (SOM). Our project’s signature techniques include NanoSIMS-enabled approaches (to understand cell-cell and OM-mineral interactions at the single cell and even viral particle scale), radiocarbon (14C) analyses (to determine both the age and turnover time of soil organic matter), and a suite of soil chemical characterization techniques we describe below, and collectively refer to as ‘Multi- dimensional SOM-mineral characterization’ (SEM, TEM, STXM, NEXAFS, NMR, FTICR-MS, LC-MS). In this report, we focus on how imaging, NMR, beamline and mass spectrometry approaches can deepen our understanding of soil microbiomes and their engagement with the soil matrix.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2022

Characterization of Multi-Material Interfaces Within Fibrous Structures (CRADA Final Report)

This project aimed to characterize the electrical, ionic, and thermal material properties of printed materials onto various textile and leather substrates. Furthermore, the material interfaces were investigated as well via characterization techniques such as SEM, TEM, and FTIR for example. Results from these studies will be utilized to properly formulate and tune process variables for enhancing the durability of devices and mitigate risks during commercial scale manufacturing studies of interest to Funxion’s product development.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Exploring the Impact of N Solubility and Trace Elements on the Creep Properties of P92 Steel

Trace elements can have major consequences on the properties of creep resistant martensitic steels. To better understand the changes in microstructure and mechanical performance associated with the variation of trace elements and enable design of steels operating at more demanding conditions, we formulated three versions of P92 within the specified allowable N, B, C and Si ranges. Different service conditions were explored, and >80% decrease in creep life was observed at 625°C 155MPa for the highest B and N containing alloy. Multiscale characterization (OM, SEM, TEM) revealed key changes due to the trace element variation. The high trace content alloy formed deleterious BN precipitates with morphology that would promote crack nucleation, but also formed higher fractions of beneficial MX precipitates. The alloy with the lowest trace content showed the best creep performance – a result of the refined precipitate populations and the absence of large-scale inclusions and BN precipitates.

Antonov, Stoichko↗
NASA NTRS1979

Pulsed-electron-beam annealing of ion-implantation damage

Short-duration high-intensity pulsed electron beams have been used to anneal ion-implantation damage in silicon and to electrically activate the dopant species. Lattice regrowth and dopant activation were determined using He(+)-4 backscattering, SEM, TEM, and device performance characteristics as diagnostic techniques. The annealing mechanism is believed to be liquid-phase epitaxial regrowth initiating from the substrate. The high-temperature transient pulse produced by the electron beam causes the dopant to diffuse rapidly in the region where the liquid state is achieved.

Greenwald, A. C.↗
NASA NTRS1983

Toughening mechanism in elastometer-modified epoxy resins: Part 1

Several plaques of Epon 828, cured with piperidine, modified with hycar(r) CTBN 1300X8, Hycar(R) CTBN 1300X13, and Hycar(R) CTBN 1300x15, and in some cases modified with biphenol A (BPA), yielded properly toughened epoxies with rubber particle diameters ranging from 0.1 to 10 microns. Fracture toughness experiments indicate that toughness was more a function of rubber content than the rubber particle size. Tensile volumetric behavior of the near resin exhibits two regions: an initial region where the increase in volume strain was due to the Poisson's effect, and a second region where a slower rate of increase in volume strain was due to shear deformation. Tensile volumetric deformation of an elastomer-modified epoxy exhibits the same type of behavior to that of the neat resin at low rates ( 3.2x0.01 sec(-1)). But at very high strain rates, which correspond more closely to the strain rates at the crack tip, there exists an increase in volume strain beyond the Poisson's effect. TEM, SEM and OM studies indicate that the rubber particles had voided. When a thin section from the deformed region is viewed under crossed-polarized light, shear bands are seen connecting voided rubber particles. From this information cavitation and enhanced shear band formation is proposed as the toughening mechanism.

Yee, A. F.↗
NASA NTRS1982

Analytical electron microscope study of eight ataxites

Optical and electron optical (SEM, TEM, AEM) techniques were employed to investigate the fine structure of eight ataxite-iron meteorites. Structural studies indicated that the ataxites can be divided into two groups: a Widmanstaetten decomposition group and a martensite decomposition group. The Widmanstaetten decomposition group has a Type I plessite microstructure and the central taenite regions contain highly dislocated lath martensite. The steep M shaped Ni gradients in the taenite are consistent with the fast cooling rates, of not less than 500 C/my, observed for this group. The martensite decomposition group has a Type III plessite microstructure and contains all the chemical group IVB ataxites. The maximum taenite Ni contents vary from 47.5 to 52.7 wt % and are consistent with slow cooling to low temperatures of not greater than 350 C at cooling rates of not greater than 25 C/my.

Novotny, P. M.↗
NASA NTRS1985

Investigation of superlattice device structures

This report describes the investigation of growth properties, and the structure of epitaxial multilayer Si(Si(1x)Ge(x)) films grown on bulk Silicon Substrates. It also describes the fabrication and characterization of MOSFET and MESFET devices made on these epitaxial films. Films were grown in a CVD reactor using hydrides of Si and Ge with H2 and He as carrier gases. Growth temperatures were between 900 C and 1050 C with most films grown at 1000 C. Layer thickness was between 300A and 2000A and total film thickness was between 0.25 micro m and 7 micro m. The Ge content (X) in the alloy layers was between .05 and 0.2. N-type multilayer films grown on (100) p-type Si showed Hall mobility in the range 1000 to 1500 sq cm/v for an average carrier concentration of approx. 10 to the 16th power/cu cm. This is up to 50% higher than the Hall mobility observed in epitaxial Si films grown under the same conditions and with the same average carrier concentration. The mobility enhancement occurred in films with average carrier concentration (n) from 0.7 x 10 to the 16th power to 2 x 10 to the 17th power/cu cm, and total film thickness greater than 1.0 micro m. No mobility enhancement was seen in n-type multilayer films grown on (111) Si or in p-type multilayer films. The structure of the films was investigated was using SEM, TEM, AES, SIMS, and X-ray double crystal diffraction techniques. The film composition profile (AES, SIMS) showed that the transition region between layers is of the order of about 100A. The TEM examination revealed a well defined layered structure with fairly sharp interfaces and good crystalline quality. It also showed that the first few layers of the film (closest to the substrate) are uneven, most probably due to the initial growth pattern of the epitaxial film where growth occurs first in isolated islands that eventually growth and coalesce. The X-ray diffraction measurement determined the elastic strain and strain relief in the alloy layers of the film and the elastic strain in the intervening Si layers.

Gergis, I. S.↗
NASA NTRS1986

Toughening mechanisms in elastomer-modified epoxies. I - Mechanical studies. II - Microscopy studies

Tensile dilatometry at constant displacement rates is presently used to ascertain whether voiding, crazing or shear banding are the deformation mechanisms at work in the toughening of brittle epoxies through the addition of an elastomeric phase. The results obtained for epoxies toughened by various levels of several types of carbonyl-terminated butadiene nitrile liquid rubber indicate that, at low strain rates, the rubber particles simply enhance shear deformation; at sufficiently high strain rates, the particles cavitate and promote further shear deformation. Examinations of these materials are conducted by means of SEM, TEM, and optical microscopy in the second part of this study. Toughening is hypothesized to involve cavitation's relieving of triaxial tension at the crack tip, as well as shear band formation, which creates a plastic zone.

Yee, A. F.↗
NASA NTRS1987

Growth and characterization of cubic SiC single-crystal films on Si

Morphological and electrical characterization results are presented for cubic SiC films grown by chemical vapor deposition on single-crystal Si substrates. The films, up to 40 microns thick, were characterized by optical microscopy, (SEM), (TEM), electron channeling, surface profilometry, and Hall measurements. A variety of morphological features observed on the SiC films are described. Electrical measurements showed a decrease in the electron mobility with increasing electron carrier concentration, similar to that observed in Si. Room-temperature electron mobilities up to 520 sq cm/V-s (at an electron carrier concentration of 5 x 10 to the 16th/cu cm) were measured. Finally, a number of parameters believed to be important in the growth process were investigated, and some discussion is given of their possible effects on the film characteristics.

Powell, J. Anthony↗
NASA NTRS1987

Precipitation in a rapidly solidified and aged Ni-Al-Mo alloy

The early stages of decomposition of a highly supersaturated nickel-base alloy have been studied using TEM, SEM, and X-ray diffraction. The material was produced as a metastable solid solution by chill-block melt-spinning. On aging, the material exhibited a number of decomposition products appearing in series or concomitantly. Some of the decomposition products of this alloy, Ni4Mo, Ni3Mo, and Ni2Mo, are related to those found in Ni-Mo binary alloys. Alpha-Mo formed during solidification was distinguished from that formed by precipitation in the solid state by orientation relationships.

Nash, P.↗
NASA NTRS1987

The microstructure and tensile properties of extruded melt-spun ribbons of iron-rich B2 FeAl

The microstructure of extruded rods of iron-rich FeAl(B2-structure), as characterized by TEM, SEM, optical microscopy and x-ray diffractometry, consisted of elongated grains with a 111-line fibre texture containing a high dislocation density. Numerous oxide particles were found, mostly in lines which reflected the matrix flow during extrusion. In addition, some large inclusions were present. Tensile testing of annealed, relatively dislocation-free specimens as a function of increasing temperature found increasing ductility up to 900K, above which a ductility drop occurred accompanied by a change in fracture mode, from transgranular cleavage to intergranular fracture. The yield strength, which was independent of temperature up to 800K (at about 500MPa), also decreased rapidly as diffusion became more important. The predominant slip vector changed from 111-line to 100-line around 700K.

Baker, I.↗
NASA NTRS1988

Elevated temperature slow plastic deformation of NiAl/TiB2 particulate composites

The 'XD' process for production of discontinuously-reinforced metal-matrix composites has been used to enhance the high-temperature strength of NiAl-TiB2 composites with particulate densities of up to 30 vol pct. SEM, TEM, and optical characterizations of the resulting microstructures showed the average TiB2 particle size to be about 1 micron, while the average grain of the NiAl matrix was of the order of 10 microns. Elevated temperature compression tests conducted at 1200 and 1300 K indicated flow strengths to increase with TiB2 content, so that the 20 vol pct TiB2-reinforced composite was three times stronger than the unreinforced NiAl; this is ascribed to the very high density of microstructural tangled dislocations, loops, and subgrain boundaries connecting the particles.

Whittenberger, J. Daniel↗
NASA NTRS1991

The microstructure of SCS-6 SiC fiber

A thorough investigation of the microstructure of single SCS-6 SiC fibers widely used as reinforcements in metal-matrix and ceramic-matrix composites has been made. Various techniques of EM including SEM, TEM, HREM parallel electron energy loss spectroscopy (PEELS), and SAM have been used to analyze and characterize the microstructure. The fiber is a complicated composite consisting of many different layers of SiC deposited on a carbon core and different carbonaceous coatings covering the SiC layers. The structural and chemical aspects of each layer are characterized and discussed.

Ning, X. J.↗