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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 379 records · Page 21
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Early reactivity of sodium silicate-activated slag pastes and its impact on rheological properties

The fast loss of fluidity of sodium silicate-activated slag (SS-AAS) systems have been widely studied in the literature. In this study, the rheology of these cements has been correlated with the evolution of the reaction products formed over time. For this purpose, a combination of experimental characterization techniques, to study the pore solution composition and microstructure of SS-AAS pastes and thermodynamic calculations have been applied. The initial precipitation of ill-defined N-A-S-H and C-N-A-S-H producta leads to a fast increase of the storage modulus after 40 min of reaction. These products are formed from the reaction of the Na{sup +} ions and silicate ions of the activator with the Ca{sup 2+} and aluminate species dissolved from the slag. However, when a shear is applied, the structure breaks down and fluidity is recovered, that infers that the attractive forces between the particles are low at the early stages of hydration.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Accelerated carbonation and structural transformation of blast furnace slag by mechanochemical alkali-activation

Alternative cements and production routes are necessary to offset the considerable global CO 2 emissions of Portland cement production. The combination of alkali-activation and mechanochemical milling in a CO 2 rich atmosphere is a promising green direction for synthesizing cementitious material as it upcycles hazardous material (slag) while capturing wt% of CO 2 during synthesis. We investigate the resulting structural transformations incurred during synthesis and hydration using a suite of characterization techniques including solid-state 27 Al, 29 Si, and 13 C NMR. The local aluminosilicate network structure of the processed clinker is best described by a melilite-type structure. Upon hydration, the network polymerizes to form a calcium, sodium aluminosilicate hydrate gel. The synthesis route also creates various metastable carbonates and bicarbonates from captured CO 2 and alkali-additives that transform into stable carbonate phases like calcite, aragonite, and gaylussite, after hydration. These findings indicate accelerated carbonation reactions occur during clinker production and demonstrates novelty as a green cement technology.

36 MATERIALS SCIENCE↗
DOE OSTI2022

Novel processing route for design and manufacturing of metal toughened nanoceramics: Al–Al 2 O 3 nanocermets

Monolithic alumina is a highly brittle ceramic with a very low fracture toughness, making it an unreliable material for mechanical and structural applications. Ceramic-metal composites (cermets) are the subject of intensive interest to obtain materials which can address the intrinsic brittleness of ceramics without compromising their high strength and light weight. In the present investigation, aluminium-alumina (Al–Al 2 O 3 ) nanocermets were developed. The nanocermets possessed the toughness of Al phase and the strength of reinforced nano Al 2 O 3 particles. Here, the nanocermets green bodies were prepared such that upon sintering each adjacent Al 2 O 3 grain was conformally coated with a continuous Al film. Mechanical milling via a combination of cryo-milling and ball-milling was used to prepare Al–Al 2 O 3 nano-powder mixture. Spark plasma sintering was used to consolidate the green nanocermets. Results show that specimens prepared from 35 h milled powders exhibited superior mechanical properties as compared to other nanocermets, with an improvement in microhardness, elastic modulus, compressive strength, and flexural strength by 88%, 78%, 69% and 40% with respect to sintered pure Al. The indentation toughness of 35 h milled nanocermet showed an increment of 12.5% with respect to sintered pure Al 2 O 3 . Characterization techniques such as XRD, SEM, HR-TEM, X-ray tomography were employed to investigate the phase evolution and structural morphology, while FEM simulations were performed for understanding the crack propagation mechanisms in nanocermets.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Metal-organic-framework and walnut shell biochar composites for lead and hexavalent chromium removal from aqueous environments

Extensive research in recent years has explored the realm of porous carbon composites for various applications, including electrochemistry, structural materials, environmental remediation, and more. In particular, the fabrication of porous carbon composites using a metal-organic framework (MOF) and biochar (BC) for aqueous remediation is a fairly new avenue of research. In this study, a MOF-BC composite was synthesized with unmodified and chemically modified BCs using solvothermal synthesis. The composites were used as adsorbents to remediate heavy metals, such as lead (II) and chromium (VI), from aqueous environments. Here, it was verified that the MOF was homogeneously deposited onto the BC's surface using various material characterization techniques. Lead and chromium adsorption studies revealed a high adsorption capacity with greater than 99% removal for lead and ∼65% for chromium, respectively. Impressively, for lead, the highest observed experimental adsorption capacity of the MOF-chemically modified BC composite was 535 mg/g, compared to 240 mg/g for pristine BC. Meanwhile, the adsorption capacity of the same MOF-BC composite for chromium ions was low at 18 mg/g, compared to 80 mg/g for the chemically modified BC. The MOF-BC had a rapid adsorption rate, achieving equilibrium at only 150 min of reaction time for lead ions. MOF-BCs have higher adsorption for cationic lead through physisorption and ion-exchange mechanisms, whereas, for anionic chromium, removal is dominated only by physisorption mechanisms. The outcomes and methodological developments attained in this study offer a novel and compelling approach for synthesizing MOF-BC composites for aqueous remediation applications.

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

Oxidation kinetics and microstructure evolution of high Mn stainless-steel alloy in CO 2 at 700 °C

Oxidation kinetics and scale formation were examined in 21–2N Stainless Steel alloys in a CO 2 environment at 700 °C. Several characterization techniques were used to identify the morphology, crystallographic structure, and chemical composition of the oxide scale formation during exposures up to 1925 h. High manganese content played an important role in homogenous oxide scale formation of Mn 3 O 4 and MnCr 2 O 4 at the scale/gas and scale/alloy interfaces and as an FCC stabilizer in the alloy. Depletion of Mn resulted in an FCC to BCC phase transformation at the scale/alloy interface. No carburization was observed, indicating that the oxide layer is preventing carbon uptake.

36 MATERIALS SCIENCE↗
DOE OSTI2023

Probing individual single atom electrocatalyst sites by advanced analytical scanning transmission electron microscopy

Single atom electrocatalysts (SAEs) are promising next-generation materials for promoting a variety of important reactions, such as the oxygen reduction, nitrogen reduction, and CO 2 reduction reactions. While bulk characterization techniques such as X-ray absorption spectroscopy and Mössbauer spectroscopy have significantly enhanced our understanding of these catalysts, direct probing of individual single metal atom sites at the atomic scale is necessary to understand local variations in the properties of these sites and accelerate design and synthesis of improved SAEs. Aberration-corrected scanning transmission electron microscopy (STEM) has become a powerful tool for providing this type of atomic-scale information about SAE metal sites. These sites are typically unstable under the electron beam, however, which, in combination with conventional acquisition methods and detectors, has limited the type and quantity of information obtainable by spectroscopic STEM techniques. Here, we map multiple individual SAE metal sites in a nitrogen-doped carbon containing atomically dispersed Fe and Re (FeReNC) at the atomic scale by direct electron detection electron energy-loss spectroscopy (EELS). Direct electron detection provides an improved signal-to-noise ratio over conventional scintillator-based detectors and enables detection and real space localization of weak signals. In addition, we demonstrate an automated method for identification of metal atom positions, placement of the probe on these sites, and simultaneous EELS and energy dispersive X-ray spectroscopic (EDS) signal acquisition. This simultaneous acquisition of EELS and EDS provides access to the composition and bonding of a wide range of SAE metal sites. In this study, focusing the probe directly on the metal sites also increases the relevant data acquisition rate by more than an order of magnitude over two-dimensional mapping, enabling improved statistical measurements of site properties. The versatility, sensitivity, and speed that these techniques provide enhances our ability to probe the local elemental and chemical environment of a large number of individual SAE metal site structures at the atomic scale, enabling an improved understanding of the variations in the local properties of these electrocatalysts to be gained. As a result, significantly increased information about individual metal sites will be available to future electrochemical studies through these techniques, accelerating the development of advanced SAEs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Cross-scale modeling and experimental integration for advancing cathode electrolyte interphase studies in high energy density lithium-ion batteries

Electrochemical interfaces are critical to the performance and durability of lithium-ion batteries (LIBs). The solid electrode-electrolyte interphase (SEI and CEI) structures that form during cycling can passivate reactive surfaces, ensuring safe operation, but also may contribute to performance degradation. Understanding the microscopic factors influencing interphase formation, growth, and evolution is essential for balanced battery design. While significant research has focused on the anode-electrolyte interphase (SEI), the cathode-electrolyte interphase (CEI) remains less explored, despite its importance in high-voltage and advanced battery technologies. Challenges in conducting in-situ or operando experiments arise from the occluded nature of these interfaces and the long timescales involved, often leading to biased interpretations. A validated multi-scale, multi-physics modeling approach, integrated with advanced characterization techniques, can effectively elucidate the intrinsic stability of electrolyte and cathode surfaces, the impact of chemical heterogeneity, and the role of microstructural features on CEI performance. In conclusion, this article reviews current modeling and simulation strategies for studying CEI in advanced LIBs and highlights opportunities for future methodological advancements and experimental integration.

Cathode-electrolyte interphase↗
DOE OSTI2020

Synthesis of porous organic cage CC3 via solvent modulated evaporation

We demonstrate a Humidity Modulated Solvent Evaporation (HMSE) approach to promote the nucleation and growth of CC3 crystals. This approach relies on the gradual evaporation of dichloromethane (solvent) from a diluted concentration of CC3 precursors deposited on aluminum foil. The slow solvent evaporation allowed enough time for the organization and formation of CC3 porous organic cage. The solvent diffusion rate was modulated by the relative humidity in the system. The slow kinetics implied during the development of CC3 phase, allowed the formation of CC3 crystals. HRTEM, SAED, SEM, and XRD patterns were used as pivotal characterization techniques to follow and confirm the formation of CC3 crystals.

porous organic cages, modulated evaporation, cryst↗
DOE OSTI2024

Iron-sandstone synergy: Advancing in-situ hydrogen production from natural gas via electromagnetic heating

Here, to address the escalating demands for decarbonization in the petroleum industry, a carbon-zero technology, known as in-situ hydrogen (H 2 ) production via electromagnetic (EM)-assisted catalytic heating, has recently been proposed for generating and extracting clean H 2 directly from petroleum reservoirs. Although preliminary techno-economic analyses show significant potential of this emerging technology for clean and affordable hydrogen, the fundamentals of natural gas conversion to H 2 in the presence of reservoir rocks are poorly understood. In this study, we explore the synergy between sandstone and artificial iron-based catalysts in enhancing in-situ H 2 production from methane (CH 4 ) cracking under EM irradiation. The dynamic behaviors of sandstone under EM heating are comprehensively investigated, including its thermal behaviors, thermal runaway (TR) phenomenon, gas generation during TR, and energy consumption. We found that sandstone demonstrates an evident natural catalytic effect for promoting CH 4 conversion to H 2 , enabling H 2 production starting at about 394 °C. The natural catalytic role of iron minerals in sandstone is elucidated using various advanced characterization techniques. Remarkably, when adding iron catalysts into the sandstone, the highest H 2 concentration and CH 4 conversion reaches 91 mol.% and 80%, respectively, at a temperature of 666 °C, while they are 50 mol.% and 35%, respectively, for the sample consisting of iron catalysts and quartz at the same level of temperature. This result indicates a strong iron-sandstone synergy and a potential to stimulate H 2 production by leveraging this synergy. Throughout the experimental process, the generation of carbon oxides (CO and CO 2 ) is negligible. These findings pave a pathway towards future pilot for carbon-zero in-situ H 2 production from sandstone gas reservoirs.

03 NATURAL GAS↗
DOE OSTI2024

Trace Fe activates perovskite nickelate OER catalysts in alkaline media via redox-active surface Ni species formed during electrocatalysis

The accurate description of activity trends among perovskite-oxide oxygen-evolution-reaction (OER) catalysts using electronic-structure descriptors requires that the bulk structure of the catalyst is comparable to that of the surface. Few studies have addressed the dynamic nature of the catalyst's structure during the OER and the consequential implications for understanding activity. Here, we use a combination of electrochemical and materials-characterization techniques to study the surface reconstruction and the associated formation of a new redox-active phase on LaNiO 3 particles, LaNiO 3 epitaxial films, and an analogous Ruddlesden-Popper phase, La 2 NiO 4 . Small, but characteristic, redox features corresponding to Ni redox in nominally amorphous NiO x H y are observed during cyclic voltammetry of these initially fully crystalline materials. The size of these redox features grows with prolonged cycling and contributes to an increased surface area as determined from electrochemical impedance spectroscopy (EIS). Here we find the OER activity is strongly dependent on soluble Fe species in the electrolyte, common impurities in alkaline media. These observations are consistent with the reconstruction of the crystalline surface to form NiO x H y species and subsequent activation by adsorption of Fe forming the well-known and extremely active NiFeO x H y OER catalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2025

Enhancement of oxidative dehydrogenation over cerium-doped nickel niobium catalysts and analysis of batch-to-batch variability

Nickel based catalysts are inexpensive and efficient for use in the oxidative dehydrogenation of ethane. NiO doped with niobium and cerium shows increased ethylene production. Small amounts of Ce doped onto a NiNb catalyst led to increased Ni activity. The catalyst that had the highest ethylene production rate per g of catalyst had 1 atom% Ce, 86 at% Ni, and 13 at% Nb (1CeNiNb) while, if surface area is incorporated into the calculation, the catalyst that had the highest ethylene production rate per m 2 was the 0.5CeNiNb catalyst. The ethylene production rates of these Ce-containing catalysts are 27 %-127 % higher than those with NiNb alone previously reported in the literature. Here, to fully understand how cerium affects the NiNb catalyst, the Ce content and effect on active sites has been fully characterized over multiple batches. In doing this, light has been shed on batch-to-batch variability. Characterization techniques such as powder X-ray diffraction, hydrogen temperature programmed reduction, X-ray photoelectron spectroscopy, synchrotron X-ray absorption spectroscopy, and methanol adsorption were used.

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

Elucidating the role of surface species in CO oxidation catalyzed by boron nitride nanotube supported transition metal oxides

Boron nitride nanotube (BNNT) is considered a highly promising catalyst support due to its outstanding thermal stability and chemical inertness. These characteristics make BNNT an attractive alternative for high-temperature applications. However, most studies to date have focused on incorporating platinum group metals (PGMs) to achieve high activity. Although BNNT-supported PGM catalysts are highly effective, their scarcity and high cost hinder widespread use in industrial processes. In this study, BNNT-supported transition metal oxides (TMO x /BNNT; TM = Fe, Co, Ni, and Cu) catalysts were investigated, and CO oxidation was applied as a model reaction to evaluate their catalytic performance. Several characterization techniques, including SEM-EDX, TEM, SXRD, H 2 -TPR, and XPS, were employed to examine their physicochemical properties. Notably, the particle size of the metal oxides differed significantly depending on the metal type. This variation is primarily attributed to the inherent metal–support interactions and the thermodynamic stability of each oxide during synthesis. These properties also affected catalytic activity, and various parameters, such as oxygen mobility and redox behavior, played important roles in determining performance. Finally, in situ DRIFTS, CO-TPSR, reaction-order analysis, and 18 O 2 isotope-labeling experiment were used to investigate the reaction mechanism. In conclusion, the findings provide insights into the design of cost-effective BNNT-supported catalysts and highlight their potential applicability in oxidation reactions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Probing the Self-Assembly dynamics of cellulose nanocrystals by X-ray photon correlation spectroscopy

Charge-stabilized colloidal cellulose nanocrystals (CNCs) can self-assemble into higher-ordered chiral nematic structures by varying the volume fraction. The assembly process exhibits distinct dynamics during the isotropic to liquid crystal phase transition, which can be elucidated using X-ray photon correlation spectroscopy (XPCS). Anionic CNCs were dispersed in propylene glycol (PG) and water spanning a range of volume fractions, encompassing several phase transitions. Coupled with traditional characterization techniques, XPCS was conducted to monitor the dynamic evolution of the different phases. Additionally, simulated XPCS results were obtained using colloidal rods and compared with the experimental data, offering additional insights into the dynamic behavior of the system. The results indicate that the particle dynamics of CNCs undergo a stepped decay in three stages during the self-assembly process in PG, coinciding with the observed phases. The phase transitions are associated with a total drop of Brownian diffusion rates by four orders of magnitude, a decrease of more than a thousand times slower than expected in an ideal system of repulsive Brownian rods. Given the similarity in the phase behaviors in CNCs dispersed in PG and in water, we hypothesize that these dynamic behaviors can be extrapolated to other polar solvent environments. Importantly, these findings represent the direct measurement of CNC dynamics using XPCS, underscoring the feasibility of directly assessing the dynamic behavior of other rod-like colloidal suspensions.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Enhanced grindability of bastnaesite ore by ex-situ CO 2 treatment under the partial pressure of 0-100 psi

High grinding energy consumption has long constrained the sustainable development of mineral processing. This study introduces an innovative technology that employs ex-situ CO 2 treatment to enhance the grindability of bastnaesite ore. The grinding aid effect was evaluated under CO 2 partial pressures ranging from 0 psi to 100 psi using particle size distribution and the Bond work index (BWI), while the underlying mechanism was elucidated with various characterization techniques including inductively coupled plasma (ICP), scanning electron microscopy (SEM), thermogravimetric analysis (TGA), and Brunauer-Emmett-Teller (BET). The optimal grinding aid effect was achieved at 100 psi partial pressure, 50% slurry concentration, and 3 h reaction duration. Correspondingly, the P80 of the grinding product decreased from 81.76 μm to 72.73 μm and the BWI of bastnaesite ore decreased from 6.96 kW·h/t to 6.30 kW·h/t, a reduction of 9.48%. The grinding aid effect primarily resulted from the transformation of sparingly soluble carbonates like calcite and dolomite into more soluble bicarbonates, which created substantial cracks and pores, thereby reducing the ore's hardness and improving its grindability. By significantly saving grinding energy consumption while delivering environmental benefits, this technology exhibits great promise for further optimization and widespread adoption.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2020

Effects of charging rates on LiNi 0.6 Mn 0.2 Co 0.2 O 2 (NMC622)/graphite Li-ion cells

Enabling fast charging capability of lithium-ion battery is of great importance to widespread adoption of electric vehicles. Increasing the charging rates from state-of-the-art 2C (30 min) to 6C (10 min) requires deep understanding on the cell aging mechanism. Here, 400 mAh pouch cells are cycled at 1C, 4C and 6C charging rates with 1C discharging rate. Capacity fading, cathode structural changes, Li inventory loss, electrolyte composition changes and Li plating on graphite electrodes are thoroughly studied by various characterization techniques. The rapid capacity fading in cells at 6C charging rate is mainly due to Li inventory loss from cathode structure and metallic Li plating on graphite electrode at higher charging rate. Post-mortem analysis also revealed changes in electrolyte such as increased salt molarity and transesterification during fast charging.

25 ENERGY STORAGE↗
DOE OSTI2022

Revisiting the capacity-fading mechanism of P2-type sodium layered oxide cathode materials during high-voltage cycling

We report P2-type sodium layered oxide cathode (Na 2/3 Ni 1/3 Mn 2/3 O 2 , P2-NNMO) has attracted great attention as a promising cathode material for sodium ion batteries because of its high specific capacity. However, this material suffers from a rapid capacity fade during high-voltage cycling. Several mechanisms have been proposed to explain the capacity fade, including intragranular fracture caused by the P2-O2 phase transion, surface structural change, and irreversible lattice oxygen release. Here we systematically investigated the morphological, structural, and chemical changes of P2-NNMO during high-voltage cycling using a variety of characterization techniques. It was found that the lattice distortion and crystal-plane buckling induced by the P2-O2 phase transition slowed down the Na-ion transport in the bulk and hindered the extraction of the Na ions. The sluggish kinetics was the main reason in reducing the accessible capacity while other interfacial degradation mechanisms played minor roles. Our results not only enabled a more complete understanding of the capacity-fading mechanism of P2-NNMO but also revealed the underlying correlations between lattice doping and the moderately improved cycle performance.

25 ENERGY STORAGE↗
DOE OSTI2023

Challenges and opportunities in plasma-activated reactions of CO 2 with light alkanes

We present upgrading CO 2 with surplus light alkanes to value-added chemicals using one-step plasma-activated processes under mild conditions, where opportunities and challenges for improving product selectivity focus on understanding reaction pathways, decoupling and benchmarking plasma and catalyst roles in reactions, tuning catalyst structural and electronic properties under plasma activation, and developing in situ characterization techniques.

03 NATURAL GAS↗
DOE OSTI2020

Impact of Cr and Co on 99Tc retention in magnetite: A combined study of ab initio molecular dynamics and experiments

This work explores the effect of co-mingled dopants, Co(II) and Cr(III), on Tc(IV) incorporation and retention in magnetite when heat treated to 625 or 700 °C. Key trends in Tc retention in the high temperature regime were identified using a combination of density-functional-theory based ab initio molecular dynamics (AIMD) simulations, and batch experiments including solid phase characterization techniques, e.g. X-ray absorption spectroscopy. A stabilizing effect on Tc(IV) was observed when the number of Tc and Cr atoms are equal or when the magnetite surface is oversaturated with Tc and Cr inclusions. Here, oversaturation is hypothesized to force Cr from the magnetite surface to form a Cr2O3 phase, which may act as a protective layer that prevents Tc release. With the addition of Co, Tc(IV) is stabilized via redox processes. The presence of Cr in low concentrations interferes with this redox stabilization and Cr is preferentially stabilized as opposed to Tc. As a result, using Co as a stabilizing dopant for Tc may be compromised in the presence of Cr. When the relative concentration of Tc, Cr and Co is the same, or more Co atoms are added to high Cr incorporated systems, the formation of the Cr2O3 phase may be suppressed. Although waste streams with co-mingled Tc and Cr potentially may benefit from a Co dopant, since the formation of a Cr2O3 passivation layer may protect incorporated Tc from being released, the relative concentration of the three elements will be a critical parameter for maximizing effectiveness of this strategy.

Lee, Mal Soon↗