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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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17 records
All sourcesNASA NTRSDOE OSTI
DOE OSTI2023

Effect of Magnesium Dopant on the Grain Boundary Stability of Nanocrystalline Aluminum Powders during Cryomilling

In this investigation, pure aluminum (Al) powders were cryomilled with and without magnesium dopants to study (a) the effect of cryomilling time on the crystallite size and (b) the effect of magnesium dopant on Al to achieve grain boundary stability. The cryomilling process was carried out using liquid nitrogen for different durations. The characterization of the cryomilled powders was carried out using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and X-ray diffraction (XRD) to understand the particle morphology, crystallite size, and elemental composition. The results demonstrated that the size of the crystallites in both Al and Mg-doped Al powders reduces as the cryomilling duration increases. The results also indicated that the preferential segregation of Mg dopant at the grain boundaries of Al provides stability to the cryomilled powders at elevated temperatures. This article discusses the mechanism for the changes in crystallite size and the effect of the Mg dopant on the grain boundary stability in Al powders.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Influence of Cryomilling on Crystallite Size of Aluminum Powder and Spark Plasma Sintered Component

The present investigation aims to develop nanocrystalline (NC) pure aluminum powders using cryomilling technique and manufacture bulk components using spark plasma sintering (SPS). The cryomilling was performed on pure Al powders for 2, 6, and 8 h. The cryomilled powders were then consolidated using SPS to produce bulk components. The particle morphology and crystallite size of the powders and the bulk SPS components were analyzed using scanning electron microscopy (SEM), X-ray diffraction (XRD), and transmission electron microscopy (TEM). The results showed that the crystallite size of pure Al powders decreases with increased cryomilling time. The results also showed that the SPS at elevated temperatures resulted in a slight increase in crystallite size, however, the changes were insignificant. The mechanical properties of the bulk components were determined using a Vickers microhardness tester. The hardness of the cryomilled SPS component was determined to be three times higher than that of the unmilled SPS component. The mechanism for the reduction in crystallite size with increasing cryomilling time is discussed. This fundamental study provides an insight into the development of bulk nanomaterials with superior mechanical properties for automotive, aerospace, marine, and nuclear applications.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Mechanical and Tribological Performance of Additively Manufactured Nanocrystalline Aluminum via Cryomilling and Cold Spray

In this study, nanocrystalline (NC) aluminum (Al) and magnesium (Mg)-doped Al bulk components were fabricated using a hybrid manufacturing process that combines cryomilling and high-pressure cold spray (HPCS) additive deposition techniques. Yttria-stabilized zirconia (YSZ) was also added during the HPCS process to improve deposition efficiency and build-up thickness via peening. The evolution of morphology, crystallite size, and elemental composition of both cryomilled powders and cold-sprayed (CS’ed) components was systematically characterized using X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM), and Transmission Electron Microscopy (TEM). Mechanical characterization was performed using Vickers microhardness and uniaxial tensile testing, while the tribological behavior was assessed using sliding wear tests under dry/lubricated conditions. XRD analysis revealed that increased cryomilling duration led to significant crystallite refinement, which directly correlated with enhanced hardness and strength. This mechanical strengthening was accompanied by an increase in coefficient of friction (COF) and lower wear rates. The results also showed that the Mg-doped Al exhibited superior hardness, tensile strength, and tribological performance compared to pure Al. The study further explores the underlying mechanisms responsible for these enhancements, highlighting the potential of solute-assisted grain boundary stabilization in tailoring high-performance NC Al alloys.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Manufacturing Bulk Nanocrystalline Al-3Mg Components Using Cryomilling and Spark Plasma Sintering

In the current study, pure aluminum (Al) powders were cryomilled with and without 3 wt.% pure magnesium (Mg) dopant for varying durations followed by spark plasma sintering (SPS) of powders to prepare bulk components with superior mechanical properties. The crystallite sizes were determined for powders and the bulk components by analyzing the X-ray diffraction (XRD) spectrum. The calculations indicated a reduction in crystallite size with the increase in the cryomilling duration. The results also showed a more significant decrease in the crystallite sizes for Al-3Mg samples than that of pure Al. The changes in the surface morphology of powders were characterized using scanning electron microscopy (SEM). The elemental mapping analysis at nanoscale was carried out using Energy-dispersive X-ray spectroscopy (EDX) in Scanning transmission electron microscopy (STEM). The mechanical properties of the bulk components were assessed using a Vickers Microhardness tester. The test results demonstrated an improvement in the hardness of Mg-doped components. Higher hardness values were also reported with an increase in the cryomilling duration. This article discusses the mechanisms for the reduction in crystallite size for pure Al and Al-3Mg and its subsequent impact on improving mechanical properties.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Promoting Reversibility of Multielectron Redox in Alkali-Rich Sulfide Cathodes through Cryomilling

We report conventional cathodes for Li-ion batteries (LIBs) are reaching their theoretical capacity limits. One way to meet the growing demands for high-capacity LIBs is by developing so-called Li-rich cathode materials that greatly benefit from additional capacities from anionic moieties in the structure. Li-rich materials are intrinsically subject to higher degrees of (de)intercalation, leaving the particles more prone to fractures and thus rapid capacity fade. Alkali-rich LiNaFeS 2 reversibly cycles with capacities exceeding 300 mAh g -1 , but its capacity fades faster than an isostructural material Li 2 FeS 2 . Using synchrotron-based transmission X-ray microscopy (TXM), we demonstrate that the capacity fade of LiNaFeS 2 stems from particle fractures in the first charge cycle. We improve the cycling performance of LiNaFeS 2 by means of cryomilling, which enhances capacity retention at cycle 50 by 76%. Through crystallographic and morphological characterization techniques, we confirm that cryomilling not only decreases particle and crystallite size while increasing microstrain but also prevents particles from fracturing. Cryomilling is a powerful tool to engineer nanoscale battery materials, and TXM allows the direct observation of morphological changes of the particles, which can be leveraged to develop next-generation cathode materials for LIBs.

25 ENERGY STORAGE↗
DOE OSTI2024

Recycling of additively printed anisotropic Nd-Fe-B bonded magnets

A high potential cost-effective and environmentally friendly method has been applied for recycling anisotropic Nd-Fe-B bonded magnets. Waste additively printed Hydrogenation-Disproportionation-Desorption-Recombination (HDDR) Nd-Fe-B anisotropic bonded magnet was pulverized into composite powder containing Nd-Fe-B particles and nylon binder through cryomilling at a liquid nitrogen temperature (~77 K) under Ar inert atmosphere. Then, the cryomilled composite powder was warm compacted into a bonded magnet. Further, the magnetic particles were aligned during post-compaction annealing under a magnetic field of 30 kOe. The recycled bonded magnets have a higher density (3% enhancement), but slightly inferior magnetic properties compared to the original magnets, i.e., the magnetic remanence, coercivity and maximum energy product are reduced by 2%, 3% and 8%, respectively. The scanning electron microscopy revealed that some HDDR Nd-Fe-B powder crumbled into fine particles during cryomilling. Powder X-ray diffraction showed a small amount of Nd-oxide impurity in the cryomilled powder. The slightly deteriorated magnetic properties are ascribed to the oxidation of Nd-Fe-B particles due to formation of fresh fracture surface during cryomilling. The approach enables the direct reuse of end-of-life bonded magnets in an economical and environmentally friendly way.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Smart manufacturing approach to manufacture bulk nanocrystalline aluminum for lightweight applications

In this research, a smart manufacturing approach was used to enhance the mechanical properties of aluminum (Al) for lightweight applications. The smart manufacturing involved cryomilling of Al powders with and without 5 wt.% magnesium (Mg) powders for varying durations followed by a high-pressure cold spray (HPCS) additive manufacturing process to prepare bulk components. The morphological changes, crystallite size, and composition of the cryomilled powders and cold sprayed (CS’ed) components were examined using scanning electron microscopy (SEM), x-ray diffraction (XRD), and transmission electron microscopy (TEM) techniques. The results showed that the crystallite size reduces with an increase in cryomilling time and the addition of Mg dopant. To test the mechanical properties of the bulk CS’ed components, microhardness tests were performed using a Vickers microhardness tester. Uniaxial tensile tests were also carried out to ascertain the material’s tensile properties. The mechanical testing results showed great improvement in the hardness and tensile strength of CS’ed Al–Mg samples as compared to pure Al samples. Subsequently, fractography analysis of the tensile failed samples was carried out to determine the nature of the failure. Here, the research article also discusses the inherent mechanisms for the improvement in mechanical properties of smart manufactured components as a result of Mg doping and cryomilling.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Enhancement in Mechanical Properties of Bulk Nanocrystalline Aluminum by Grain Boundary Strengthening Mechanism

In the present work, commercially pure aluminum (Al) powders were milled at cryogenic temperatures (a) without magnesium (Mg) and (b) with 5 wt.% Mg powders for different durations. The cryomilled powders were analyzed using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and x-ray diffraction (XRD) to determine the changes in particle morphology, elemental composition, and crystallite size. The results showed a reduction in crystallite size with the increase in cryomilling duration. Thereafter, the spark plasma sintering (SPS) process was carried out to manufacture bulk samples. The mechanical properties of the bulk SPS samples were assessed by conducting microhardness, tensile, and fatigue tests. The Vickers microhardness tests showed improved hardness for the Al-Mg bulk samples as compared to pure Al. The Al-Mg samples also showed an increase in tensile strength with increasing cryomilling time. Fatigue test results showed an improvement in Al-Mg components' high-cycle fatigue response. Furthermore, the mechanism for the enhancement in mechanical properties as a result of crystallite size reduction and grain boundary strengthening by the addition of Mg dopant is also discussed.

36 MATERIALS SCIENCE↗
DOE OSTI2024

The Grain Boundary Relaxation (GBR) Approach for Manufacturing High Strength Nanocrystalline Lightweight Metals

The overarching goal of the project was to conduct research and development work as proposed in the Statement of Project Objective (SOPO) of the award document DE-FE-0009116. The project had 4 tasks and 12 milestones. All the milestone deliverables were completed. The accomplishments of the project objectives and technical discussions are described in Sections 3 and 4, respectively. The modeling and simulation work indicated that to increase the strength and stability of nanocrystalline aluminum (Al), selection of dopants, such as Mg, is necessary. It was predicted that the crystallite size should be less than 50 nm to give high strength. On the basis of modeling, cryo-milling of Al was conducted with the addition of Mg as a function of different times. The crystallite size of the cryo-milled powders was determined by XRD and TEM. Both measurements showed that the actual crystallite size of the grain was <40 nm. The thermal stability of the grain size was established as a function of temperature. It was established that the grain size was < 50 nm up to 500C. The crystallite size of the bulk sample prepared by spark plasma sintering (SPS) and cold spray (CS) additive manufacturing was less than <40 nm. The mechanical properties of the bulk samples prepared by SPS and CS, showed excellent microhardness, good tensile properties (>200 MPa) with moderate ductility and improved fatigue performance. Adding yttria stabilized zirconia (YSZ) improved the build thick of the CS sample, however the YSZ was getting embedded into the sample. A highly dense SPS samples sent for 3rd party testing to the Innovation Testing Services showed a minimum hardness of 180 HV with an average tensile strength of 512.5 MPa. The high cycle fatigue tests also showed an endurance limit of 179.5 MPa. The Energy cost evaluations showed an overall energy cost of around $\$$17.05 for the cryomilling and SPS processes and the total manufacturing cost calculations of $\$$78.14 for 1 kg of sample. The energy cost to prepare a Kg of CS sample is $\$$17.60 and the overall manufacturing cost is $\$$86.85.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Nanocrystalline Materials: Synthesis, Characterization, Properties, and Applications

Nanostructuring is a commonly employed method of obtaining superior mechanical properties in metals and alloys. Compared to conventional polycrystalline counterparts, nanostructuring can provide remarkable improvements in yield strength, toughness, fatigue life, corrosion resistance, and hardness, which is attributed to the nano grain size. In this review paper, the current state-of-the-art of synthesis methods of nanocrystalline (NC) materials such as rapid solidification, chemical precipitation, chemical vapor deposition, and mechanical alloying, including high-energy ball milling (HEBM) and cryomilling was elucidated. More specifically, the effect of various process parameters on mechanical properties and microstructural features were explained for a broad range of engineering materials. This study also explains the mechanism of grain strengthening using the Hall-Petch relation and illustrates the effects of post-processing on the grain size and subsequently their properties. This review also reports the applications, challenges, and future scope for the NC materials.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Cold spray manufacturing of oxide-dispersion strengthened (ODS) steels using gas-atomized and ball-milled 14YWT powders

The cold spray deposition process has been investigated for the manufacture of 14YWT oxide-dispersion strengthened (ODS) steel, a nanostructured ferritic alloy (NFA), using gas-atomized and ball-milled feedstock powders. Cold spraying of the gas-atomized powder resulted in a thick dense deposit, but annealing them above 900 °C induced grain growth and heterogeneous precipitation of nanoparticles, thus resulting in lower hardness (~ 170 HV) compared to 14YWT ODS steel manufactured by the conventional method. The ball-milled powder (Fe-14Cr-3W-0.4Ti-0.2Y-0.125O) was cryomilled in liquid N 2 to achieve small particle sizes followed by annealing in a H 2 /Ar environment at 1000 °C and 1100 °C to reduce the hardness from ~ 8 GPa to ~ 5 GPa. Both smaller particle sizes and lower hardness of annealed powders made them amenable to the cold spray deposition process, resulting in thick and dense deposits, while retaining the favorable fully solutionized microstructure of the ball-milled powders. The microstructure of the as-deposited ODS exhibited very fine grain sizes (50–250 nm) with a uniform dispersion of Y-Ti-O nanoprecipitates in the ferritic steel matrix. The hardness values of the cold spray deposits using the powders annealed at 1000 °C and 1100 °C was 770 HV and 496 HV, respectively. Post-heat treatment of the as-deposited material up to 1100 °C showed a high-density microstructure with uniformly dispersed nanoscale oxide particles. The hardness of the annealed deposits up to 1000 °C had a notably higher hardness than bulk 14YWT ODS steel manufactured by conventional methods. The study demonstrates that cold spray deposition of the microstructurally-tailored feedstock powders can be used to successfully manufacture ODS steel with microstructure and properties comparable to those produced by the conventional methods, while providing for an attractive option for the more rapid and cost-effective manufacturing of ODS steel cladding tubes.

14YWT↗
DOE OSTI2020

Thermoelectric properties of BiSbTe-type alloys prepared by chill-casting and cryo-milling

The thermoelectric properties of Bi x Sb 1-x Te 3 processed through milling have been extensively studied with varied results that needs to be rationalized. Since cryo-milling is a relatively cleaner milling process compared to other milling processes, in this study we explore this technique to reduce the particle size prior to compaction to get an insight into the thermoelectric properties. We first report the results of cryomilled BiSbTe 3 compacted by spark plasmas sintering (SPS) process and show that milling leads to a change in transport behavior from ‘p’ to ‘n’ type similar to that reported for Bi 2 Te 3 . It is shown that the defects induced by milling is responsible for this change in materials behavior. We further study the effect of change in Bi to Sb ratio and excess tellurium on the thermoelectric properties when processed through cryo-milling as well as casting using a chilled copper block. Excess tellurium leads to a microstructure containing a fraction of layered eutectic that gets further fragmented during cryo-milling. Although the Seebeck coefficient does not change significantly, reflecting the cleanliness of the process, the thermal conductivity changes during hot compaction leading to an improvement of ZT. However, a comparison of all the reported results does not reveal any systematics in thermoelectric properties reflecting the difficulties with these materials.

36 MATERIALS SCIENCE↗
DOE OSTI2020

High-Energy All-Solid-State Organic–Lithium Batteries Based on Ceramic Electrolytes

Recent studies have identified unique properties of organic battery electrode materials such as moderate redox potentials and mechanical softness which are uniquely beneficial for all-solid-state batteries based on ceramic electrolytes. Here, we further explore the promise of organic materials and demonstrate a sulfide electrolyte- based organic-lithium battery with a specific energy of 828 Wh kg –1 , rivaling the state-of- the-art of all-solid-state batteries. Two innovation steps are responsible for the accomplishment. First, the combination of lithium anode and the high-capacity cathode material pyrene-4,5,9,10-tetraone ensures a high theoretical specific energy. Second, the microstructure of the organic cathode is optimized with the introduction of cryomilling, a technique common to processing soft materials but not familiar to electrode fabrication. The cathode material utilization increases to 99.5% as a result, up from the 55–89% previously reported for ceramic electrolyte-based solid-state organic batteries. In conclusion, the improvement highlights the special requirements of solid-state organic electrodes for microstructural engineering while preserving the chemical integrity of components.

25 ENERGY STORAGE↗
DOE OSTI2024

Not Cutting Corners: Bioderived Triggers Driving Oxidative Main Chain Scission of Poly(ethylene terephthalate)

About 20–34 billion poly(ethylene terephthalate) (PET) bottles from the beverage industry leak into aquatic ecosystems annually, necessitating the development of urgent strategies to treat waterborne plastic pollution. Inspired by the scalability of water disinfection infrastructure and protocols, we present a dual depolymerization approach relying on oxidation, followed by hydrolysis. Incorporating bioderived monounsaturated C18 diacid (C18:1-DA) counits at low dosages (2–5%) in the PET backbone overcomes the diffusional limitations of depolymerizing PET in the solid state by suppressing the glass transition temperature of the copolymer by 20 °C. Cryomilled C18:1-PET powder suspended in an oxidant-loaded alkaline slurry underwent bulk depolymerization to oligomers at 80–100 °C via oxidative scissions at the internally located unsaturations. In contrast, conventional PET undergoes only minor end-chain scission under mild alkaline conditions. These oligomers are suitable for low-energy repolymerization or facile solvolysis to monomers. A permanganate-periodate oxidant couple demonstrated successful oxidation through the bulk of the polymer, which subsequently was hydrolyzed to monomers. Furthermore, this model system serves as a proxy for ozonolysis, followed by mild hydrolysis to reduce the energetics of alkaline hydrolysis. This integrated oxidation–hydrolysis strategy paves the way for the industrial adoption of cleaner, advanced oxidation processes, such as ozonolysis for plastic pretreatment, further enabling commercialized chemical recycling of unsaturation-containing polyesters.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2026

Effects of Polymer Morphology on Solvent and Catalyst Accessibility during Polyethylene and Polystyrene Autoxidation

Efficient catalytic deconstruction of plastics requires facile solvent and catalyst access to polymer substrates to minimize mass transfer effects. Autoxidation using Co(II) acetate, Mn(II) acetate, and a radical carrier in acetic acid is a promising strategy to deconstruct mixed plastic waste, yet the role of polymer morphology in governing solvent and catalyst accessibility remains poorly understood. Here, in situ simultaneous small- and wide-angle X-ray scattering (SAXS/WAXS), complemented by X-ray fluorescence (XRF) imaging and high-pressure differential scanning calorimetry (DSC), were used to elucidate interactions between acetic acid, a Co/Mn catalyst solution, and semicrystalline polyethylene (PE) and amorphous polystyrene (PS) from room temperature to 160 °C. In PE, acetic acid and catalyst access were confined to amorphous regions and cryomilled particle interfaces at room temperature, while crystalline lamellae remained intact after soaking for up to 34 h. Increasing temperature enabled solvent uptake into PE, followed by solvent-assisted softening above 100 °C, and a modest melting-point depression that removed lamellar transport barriers upon melting. Conversely for PS, acetic acid penetrated the glassy polymer without inducing chain mobility until the glass transition was reached, above which the observed structural changes were consistent with enhanced segmental mobility which enabled bulk penetration. These results suggest that polymer morphology and thermally activated physical transitions arising from diffusion and polymer–solvent interactions can influence whether autoxidation of plastics is transport-limited or kinetically controlled, providing a framework for aligning reaction conditions with reaction outcomes.

09 BIOMASS FUELS↗
DOE OSTI2026

Pyrolysis Molecular Beam Mass Spectrometry_Analysis_of_Natural_Variants_of_Poplulus_Trichocarpa_Leaves

Select leaves from natural variants of Poplar (Populus Trichocarpa) grown in a greenhouse at Oak Ridge National Laboratory were analyzed by Pyrolysis-Molecular Beam Mass Spectrometry (Py-MBMS). Leaves were harvested, cryomilled and kept frozen until analysis. Py-MBMS analysis was conducted using approximately 4 mg of biomass and each sample was analyzed in duplicate. A Frontier PY2020 unit pyrolyzed samples at 500°C for 30 s in 80 µL deactivated stainless steel cups. An Extrel Super-Sonic MBMS Model Max 1000 was used to collect mass spectral data fromm/z30 to 450 at 17 eV and processed using Merlin Automation software (V3). Spectral ion intensities were normalized to the total ion chromatogram signal for each sample for analysis of spectral variance. Lignin content (wt %) was estimated based on relative responses from standards of known Klason lignin content using mean-normalized ion intensities ofm/z120, 124 (G), 137 (G), 138 (G), 150 (G), 152, 154 (S), 164 (G), 167 (S), 168 (S), 178 (G), 180, 181, 182 (S), 194 (S), 208 (S) and 210 (S) where G indicates guaiacyl-derived ions, S indicates syringyl-derived ions, and other ions either derive from other lignin monomers or multiple sources. Ratios of S and G lignin monomer units (S/G) were obtained by dividing the sum of S-based ions by the sum of G-based ions using mean-normalized ion intensities.

CBI↗