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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 19 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2024

Shelf-life of ball-milled catalyst inks for the fabrication of fuel cell electrodes

A major factor driving fuel cell costs is the quantity of precious metal required. Therefore, it is important to understand a timeframe where inks can be reused. Here, in this work, we explore differences between a freshly prepared catalyst ink and one that has been stored for over a year – comparing ink properties, cathode catalyst layer microstructure, and their respective fuel cell performance. Ink studies revealed smaller agglomerate sizes and a decrease in shear viscosity for the aged ink. Longer storage time also results in fewer cracks and a more uniform ionomer distribution, as evidenced by microscopy characterization of rod-coated electrodes. Lastly, polarization curves show improved performance at higher current densities for the electrode prepared from the aged ink. We rationalize such effect in terms of enhanced ionomer adsorption onto the catalyst over time.

08 HYDROGEN↗
DOE OSTI2024

Medium-density amorphous ice unveils shear rate as a new dimension in water’s phase diagram

Recent experiments revealed a new amorphous ice phase, medium-density amorphous ice (MDA), formed by ball-milling ice I h at 77 K [Rosu-Finsen et al., Science 379, 474–478 (2023)]. MDA has density between that of low-density amorphous (LDA) and high-density amorphous (HDA) ices, adding to the complexity of water’s phase diagram, known for its glass polyamorphism and two-state thermodynamics. The nature of MDA and its relation to other amorphous ices and liquid water remain unsolved. Here, we use molecular simulations under controlled pressure and shear rate at 77 K to produce and investigate MDA. Here. we find that MDA formed at constant shear rate is a steady-state nonequilibrium shear-driven amorphous ice (SDA), that can be produced by shearing ice I h , LDA, or HDA. Our results suggest that MDA could be obtained by ball-milling water glasses without crystallization interference. Increasing the shear rate at ambient pressure produces SDAs with densities ranging from LDA to HDA, revealing shear rate as a new thermodynamic variable in the nonequilibrium phase diagram of water. Indeed, shearing provides access to amorphous states inaccessible by controlling pressure and temperature alone. SDAs produced with shearing rates as high as 10 6 s −1 sample the same region of the potential energy landscape than hyperquenched glasses with identical density, pressure, and temperature. Intriguingly, SDAs obtained by shearing at ~10 8 s −1 have density, enthalpy, and structure indistinguishable from those of water “instantaneously” quenched from room temperature to 77 K over 10 ps, making them good approximants for the “true glass” of ambient liquid water.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1983

Injection molding ceramics to high green densities

The injection molding behavior of a concentrated suspension of Si powder in wax was studied. It was found that the injection molding behavior was a function of the processing techniques used to generate the powder. Dry ball-milled powders had the best molding behavior, while air classified and impact-milled powders demonstrated poorer injection moldability. The relative viscosity of these molding batches was studied as a function of powder properties: distribution shape, surface area, packing density, and particle morphology. The experimental behavior, in all cases, followed existing theories. The relative viscosity of an injection molding composition composed of dry ball-milled powders could be expressed using Farris' relation.

Mangels, J. A.↗
DOE OSTI2026

Electrostatic‐Attraction‐Driven Self‐Assembled Graphene‐Disordered Rocksalt Composite Cathode for Lithium‐Ion Batteries

Disordered rocksalt cathodes hold promise for achieving high-capacity lithium-ion batteries while using low-cost, earth-abundant elements. However, their electrochemical performance remains critically limited by their poor electronic conductivity. Conventional strategies such as high-energy ball milling with excess carbon additives can improve conductivity but remain challenging to scale and often produce defects and increase surface area, thereby accelerating capacity degradation. Herein, we report an alternative approach of electrostatic-attraction-driven self-assembly to fabricate Li 1.2 Mn 0.6 Ti 0.2 O 1.8 F 0.2 (LMTOF) particles uniformly wrapped with electronically conductive graphene sheets without associated materials degradation. The graphene-wrapped LMTOF demonstrates significantly improved cycling stability (89% capacity retention after 100 cycles) and superior rate capability compared with an LMTOF-carbon composite electrode fabricated using the conventional high-energy ball-milling process. Post-cycling analysis reveals reduced oxygen evolution, suppressed unwanted side reactions, and improved structural integrity for the graphene-LMTOF composite. This work highlights the advantages of solution-based carbon wrapping and offers a scalable strategy to prepare high-performance DRX cathodes for lithium-ion batteries.

carbon composite↗
DOE OSTI2025

Densification, microstructure, and mechanical properties of Mo–30W alloys fabricated from conditioned powders

Refractory alloys, such as molybdenum-based systems, are attracting growing interest for applications in extreme environments, such as in the nuclear and aerospace industries. Recent advances in sintering technologies, coupled with mechanical alloying, have enabled the tailored design of these alloys by leveraging powder characteristics to control final microstructures and mechanical properties. In this study, Mo-30W alloys were fabricated using electric field-assisted sintering (EFAS) from ball-milled powders with and without hydrogen treatment to investigate the influence of surface oxides on material properties and sintering behavior. The results revealed that samples processed from as-ball-milled powder contained a high density of oxides within the microstructure, whereas oxide presence was significantly reduced in samples fabricated from hydrogen-treated powders. Interestingly, the two powder types led to opposite trends in grain size distribution: samples from untreated powders exhibited grain refinement from sample periphery to the center, while samples from hydrogen-treated powders showed grain coarsening toward the center. This behavior is attributed to temperature gradients present during sintering due to electrical percolation pathway differences during Joule heating. The powder surface oxides may have influenced the temperature distribution and grain evolution. Microhardness profiles measured along both axial and thickness directions were consistent with the grain size distribution. Furthermore, oxide films on powder surfaces have delayed densification by hindering particle necking and atomic diffusion during sintering.

36 - MATERIALS SCIENCE↗
DOE OSTI2025

Maximizing Calendering Effects Through the Mechanical Pulverization of Co-Free Nickel-Rich Cathodes in Lithium-Ion Cells

Calendering is a technique used to maximize the volumetric energy density of battery electrodes. However, higher amounts of calendering result in increased tortuosity and particle cracking. We propose a novel packing structure of electrode particles to maximize calendering benefits while minimizing particle fracture. Cobalt-free layered oxide cathode LiNi0.92Mn0.04Al0.04O2 (NMA) particles are pulverized through ball-milling and coated with lithium phosphate. Pulverized and pristine NMA are fabricated into “bimodal” electrodes, whereas “unimodal” electrodes consist of only pristine NMA. Each electrode type was made into 30% porosity, 40% porosity, and uncalendered coin cell samples. X-ray diffraction suggests that the unimodal samples suffer from more particle fracture than the bimodal samples when calendered to the same porosity of 30%. Electrochemical impedance spectroscopy suggests that the bimodal electrodes exhibit lower surface film resistance. This is supported by enhanced capacity retention for the bimodal samples after 100 cycles.

25 ENERGY STORAGE↗
DOE OSTI2025

Wafer-Free Crystalline Silicon Solar Cells (CRADA Final Report)

This CRADA project, based on the DOE Solar Energy Technologies Office (SETO) Solar Prize Voucher program, helped Leap Photovoltaics to develop methodologies to immobilize Si particles by permanently attaching them to an Al-coated substrate and thereby forming carrier-selective electrical contacts to the Si particles. The bigger goal was to help Leap Photovoltaics develop these immobilized and contacted particle arrays into relatively efficient, inexpensive, and industrially relevant solar cells. By using Si particles instead of wafers in a solar cell absorber layer, one can avoid costs associated with growing monocrystalline Si ingots, then diamond-sawing them into wafers, then processing wafers into cells – a mainstream practice in today's high-efficiency Si cell and module technology. Monocrystalline or polycrystalline Si particles can be obtained in various ways: for example, Si kerf from wafer sawing is monocrystalline; recycled Si cell wafers can be ball-milled into particles; particles can be grown using various gas-phase techniques (mostly from SiH4). These Si particles can be assembled onto a substrate and serve as an absorber layer for the solar cell, absorbing photons to generate photocarriers. The challenge with this technique is to collect photocarriers from individual Si particles, with separation of photogenerated electrons to the negative cell’s electrode and positive photogenerated holes to the positive electrode. Therefore, each particle must have two isolated, carrier-selective contacts: one for electrons and one for holes. Plus, particles need to be immobilized onto a solid substrate. The goal of this work was focused on the immobilization of Si particles and creating hole-selective contact to them at the same time, using industrially relevant Si photovoltaic (PV) cell technology: screen printing of Al back-surface field electrodes. This is used in the mainstream Propane Education and Research Council (PERC) technology for hole-collecting contacts at the back of the cell. The work performed at NREL consisted of screen printing of Al metal paste on substrates, spreading Si particles onto it, and thermally processing the structures to form hole-collecting contacts. The final structures were investigated by scanning electron microscopy (SEM) after focused ion beam (FIB) cross-sectioning and polishing. The work was done jointly by NREL staff and Leap Photovoltaics (Leap PV) employees stationed at NREL. The samples were then taken to Leap PV for further processing. Training the Leap PV employee on various NREL techniques (laser cutting, screen printing, thermal processing, characterization) was part of the scope.

14 SOLAR ENERGY↗
NASA NTRS1971

Development of a highly reliable composite board for printed circuitry for use in space environment

Materials, processes and fabrication techniques have been investigated for the development of a high-temperature circuit-board laminate. High quality, void-free copper-clad laminates have been made using 7628/HS-1 style fiberglas reinforcements with filled polyimide matrices. The fabricating characteristics of P13N resin appear suitable for use as a filled matrix in this circuit board development. High-fired, ball-milled alumina appears to be necessary to obtain the desired effects in the circuit board system. Nickel-clad copper foil bonding surfaces appear to be another requirement for retention of good bond strengths after art work and plating sequences. The fabrication cycle for this circuit board system is very dependent on the heating profile. Very rapid heating with quick loading is recommended. A stack approach to lamination was successfully used.

Bradbury, E. J.↗
NASA NTRS1978

Cleaning process for contaminated superalloy powders

A cleaning process for removing interstitial contaminants from superalloy powders after wet grinding is described. Typical analyses of oxygen, carbon, nitrogen, and hydrogen in ball-milled WAZ-20 superalloy samples after hydrogen plus vacuum cleaning are presented. The hydrogen cleaning step involves heating retorts containing superalloy powder twice under flowing hydrogen with a 24-hour hold at each temperature. The vacuum step involves heating cold-pressed billets two hours at an elevated temperature at a pressure of 10 microPa. It is suggested that the hydrogen plus vacuum cleaning procedure can be applied to superalloys contaminated by other substances in other industrial processes.

Anglin, A. E.↗
NASA NTRS1979

Modules of rupture and oxidation resistance of S12.55Al0.6O0.72N3.52 sialon

A Sialon of formula Si2.55Al0.6O0.72N3.52 was made from ball-milled alpha-Si3N4, AIN, and SiO2 by sintering the powder compacts at 1760 C for 4 hours in stagnant nitrogen. This Sialon had an average modulus of rupture ranging from 404 megapascals (58.6 ksi) at room temperature to 254 megapascals (36.8 ksi) at 1400 C. Oxidation tests at 1400 C in air showed it to have a parabolic oxidation rate constant less than or equal to 2.8x10 to the -10th power sq g/cm4 hr, which is smaller than that of any other Si3N4-base ceramic reported in the literature.

Arias, A.↗
NASA NTRS1981

"Densified" tiles form stronger bonds

Application of colloidal silica more than doubles bond strength of ceramic tile/substrate attachments. "Densification" process strengthens surface where tile attaches to felt strain-isolator pad, redistributing stresses and preventing failures at that point. First, isopropyl alcohol is applied to bottom tile surface. Second, aqueous mixture of cementing colloidal silica and reinforcing ball-milled silica particles is painted on tile. Finally, after drying, tile is rewaterproofed by exposure to vapors or methyltrimethoxysilane and acetic acid.

Dotts, R. L.↗
NASA NTRS1991

Fabrication Of Ceramic Mats

Process to make mats of fine zirconia filaments proposed. Ceramic mats formed by sintering mats of partially dried filaments extruded from slurry of ceramic powder, binder, and solvent. Mats of fine zirconia fibers easier to ball-mill than commercially available zirconia powder.

Collins, Earl R., Jr.↗
NASA NTRS1994

Ceramic fiber-reinforced monoclinic celsian phase glass-ceramic matrix composite material

A hyridopolysilazane-derived ceramic fiber reinforced monoclinic celsian phase barium aluminum silicate glass-ceramic matrix composite material is prepared by ball-milling an aqueous slurry of BAS glass powder and fine monoclinic celsian seeds. The fibers improve the mechanical strength and fracture toughness and with the matrix provide superior dielectric properties.

Bansal, Narottam P.↗
NASA NTRS1995

The effect of gravity on the combustion synthesis of Ni-Al and Ni3Al-TiB2 composites from elements

Previous studies on the combustion synthesis of advanced materials indicate that combustion and structure formation mechanisms involve several stages including melting of reactants and products, spreading of the melt, droplet coalescence, diffusion and convection, buoyancy of solid particles, and densification of the liquid product. Most of these processes are affected by gravity. Conducting the combustion synthesis under microgravity conditions is expected to help elucidate the reaction mechanisms. Two systems were examined. The first involves Ni/AI cladded particles, which is an ideal system to examine the individual particle and liquid flow before combustion occurs. For comparison, elemental Ni and Al powders with the same stoichiometry as that of the cladded particles were also used in some experiments. The second system was the Ni3AITiB2 composite in which the Ni3AI (-delta H(sub f) = 153.1 kJ/mol) phase melts during reaction enabling us to examine settling of the liquid phase. The amount of liquid phase was controlled by varying the TiB2 (-delta H(sub f) = 323.8 kJ/mol) content which generates the additional heat. The overall reactions for the two systems can be expressed as follows. System 1: 4Ni + 2AI yields Ni3AI + NiA and System 2: 3Ni + Al + x (Ti + 2B) yields Ni3Al + x(TiB2). For the first system, pellets were pressed directly from the cladded particles, at green densities about 77 +/- 3% of theoretical value. For the second, the pellets were prepared by mixing the elemental reactant powders in the required stoichiometry by ball-milling and then pressing uniaxially at green densities about 70 +/- 3 percent of theoretical. The pellets were cylindrical in shape, 10 mm in diameter and length typically 20-30 mm. The pellet samples were reacted in UHP Argon (1 atm) using the experimental setup and procedure described previously. After reaction, the samples were sectioned axially in order to conduct the microstructural analysis in the longitudinal direction. The phase composition of the reacted product was determined by X-ray diffraction (XRD) and the microstructure was analyzed using scanning electron microscopy (SEM) along with energy dispersive X-ray spectrometry (EDX).

Varma, Arvind↗
NASA NTRS2006

Incorporation of Multiwalled Carbon Nanotubes into High Temperature Resin Using Dry Mixing Techniques

As part of an ongoing effort to develop multifunctional advanced composites, blends of PETI330 and multiwalled carbon nanotubes (MWNTs) were prepared and characterized. Dry mixing techniques were employed and the maximum loading level of the MWNT chosen was based primarily on its effect on melt viscosity. The PETI330/ MWNT mixtures were prepared at concentrations ranging from 3 to 25 wt %. The resulting powders were characterized for homogeneity, thermal and rheological properties and extrudability as continuous fibers. Based on the characterization results, samples containing 10, 15 and 20 wt % MWNTs were chosen for more comprehensive evaluation. Samples were also prepared using in situ polymerization and solution mixing techniques and their properties were compared with the ball-mill prepared samples. The preparation and characterization of PETI330/ MWNT nanocomposites are discussed herein.

Ghose, Sayata↗