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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 91 records · Page 5
All sourcesNASA NTRSDOE OSTI
DOE OSTI2022

Microwave catalytic conversion of acetylene for co-production of hydrogen and carbon nanotubes

Natural gas conversion to hydrogen and solid carbon can drastically reduce the carbon footprint. Microwave plasma pyrolysis is an emerging process for chemical industries to directly convert methane (CH 4 ), the major component of natural gas, to hydrogen and carbon, which offers benefits such as fast process dynamics, flexibility, and high product yield. However, the formation of unwanted by-products, like acetylene (C 2 H 2 ), will require extra cost for gas separation. Plasma pyrolysis of CH 4 produces large amount of acetylene at downstream, which is currently used mainly for welding. Here, to avoid gas separation and upgrade acetylene from the downstream of methane plasma reactor, a novel approach toward its transformation to carbon nanotubes (CNT) and pure hydrogen (H 2 ) over Ni-based bimetallic catalyst driven by microwave irradiation has been reported in this work. The dominant gas product was hydrogen. Low concentrations of methane, ethane, and ethylene were observed in the product stream. Catalytic acetylene decomposition was carried out at 400 °C over Al 2 O 3 supported Ni catalyst. The results showed that, at 400 °C, acetylene was dehydrogenated to CNT and hydrogen was the dominant gas in product stream over 10Ni-1Pd-Al 2 O 3 catalyst. Characterizations of spent catalysts was conducted using Raman spectroscopy and transmission electron microscopy (TEM) to investigate the properties of carbon deposited over the catalyst during the catalytic acetylene decomposition. The results highlight that methane can be efficiently converted to hydrogen and CNT through 2-step process, microwave plasma and microwave catalytic conversion of intermediate acetylene, operated in a single reactor system driven by microwave.

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

Revealing Molecular Mechanisms in Hierarchical Nanoporous Carbon via Nuclear Magnetic Resonance

Hierarchical nanoporous carbons (HNC) have been proven to be an effective adsorbent for the adsorption of volatile organic compounds (VOCs) and CO 2 . However, questions remain regarding the hierarchical structure regulation, the adsorption mechanisms of adsorbate uptake, and interactions within the HNC. Here, we synthesize HNC from wood, using a microwave-induced heating method incorporating K 2 CO 3 activation. Our HNC exhibit Murray's law multiscale structures, prompting a molecular-scale study of adsorbate adsorption via nuclear magnetic resonance (NMR). NMR chemical shifts are consistent with ring-current effects from the adsorbent. Our NMR technique provides a convenient way to quantitate adsorption of adsorbate in HNC. VOC vapor adsorption results show NMR chemical-shift changes with time, suggesting initial adsorption into mesopores, followed by diffusion into micropores. Schroeder's paradox is demonstrated by differences in observed shifts for adsorbed liquid vis-à-vis vapor phase in these HNC. These HNC show high CO 2 adsorption capacity, portending applications to carbon capture.

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

Experimental Investigation of the Effects of Magnetic Mirrors on Plasma Transport in the Prototype Material Plasma Exposure Experiment

The Prototype Material Plasma Exposure eXperiment (Proto-MPEX) at Oak Ridge National Laboratory is developing a helicon radio frequency (RF) source for plasma production along with microwave electron heating and RF ion heating. Proto-MPEX has several magnetic mirrors that affect plasma transport. The magnetic field near the helicon source is ~ 0.05 T, and the peak magnetic field in Proto-MPEX is ~ 1.8 T, which results in a large magnetic well for particles sourced at the helicon transporting toward the target region. Keeping the helicon source field and the target field constant, experiments have been conducted by methodically changing the magnetic field, at a local axial location, within the source and the target. Plasma flow measurements using Mach probes have shown a decrease in the flow as a function of the magnetic mirror ratio. Plasma flows were further investigated with ion cyclotron resonant heating (ICH). Results with the addition of ICH measured upstream of the antenna have shown a decrease in Mach number as a function of mirror ratio when compared to helicon discharges. Such flow behavior demonstrated slowing down of the plasma due to the increased reverse plasma flow toward the helicon plasma source. However, in high magnetic fields, when the resonant magnetic field moved away from the ICH antenna, no effects on the plasma flow due to ICH were observed.

Kafle, Nischal↗
DOE OSTI2023

Microwave-assisted, performance-advantaged electrification of propane dehydrogenation

Nonoxidative propane dehydrogenation (PDH) produces on-site propylene for value-added chemicals. While commercial, its modest selectivity and catalyst deactivation hamper the process efficiency and limit operation to lower temperatures. We demonstrate PDH in a microwave (MW)–heated reactor over PtSn/SiO 2 catalyst pellets loaded in a SiC monolith acting as MW susceptor and a heat distributor while ensuring comparable conditions with conventional reactors. Time-on-stream experiments show active and stable operation at 500°C without hydrogen addition. Upon increasing temperature or feed partial pressure at high space velocity, catalysts under MWs show resistance in coking and sintering, high activity, and selectivity, starkly contrasting conventional reactors whose catalyst undergoes deactivation. Mechanistic differences in coke formation are exposed. Gas-solid temperature gradients are computationally investigated, and nanoscale temperature inhomogeneities are proposed to rationalize the different performances of the heating modes. The approach highlights the great potential of electrification of endothermic catalytic reactions.

42 ENGINEERING↗
DOE OSTI2025

Microwave-assisted delignification for improved cellulose production

This study aims to develop microwave (MW) technologies to improve the paper pulping process, decreasing both chemical and thermal energy requirements. The overall objective is to explore an efficient process that aids in the delignification of paper pulp, reducing energy needs and chemical intensity. The experimental variables evaluated during the MW-assisted digestion process include formic acid concentration, time, temperature, digestion cycles, and the formic acid to paper ratio. This research investigates the potential of MW technology to create a more sustainable and efficient cellulose production method.

microwave heating↗
DOE OSTI2026

Recycling of Printed Circuit Boards to Recover Critical Materials

The printed circuit board (PCB), a central component of most electronic devices, represents a significant fraction of the electronic product waste stream. The complex composition of PCBs, consisting of metals, polymers, and fiberglass, requires specialized recovery steps to reclaim valuable and critical materials and the safe disposal of brominated compounds. In this review paper, we describe the current state of critical material recovery and traditional recycling technologies and identify key obstacles to large-scale implementation. Metals present at high concentrations, such as copper, lead, and iron, are conventionally recovered from PCBs using hydrometallurgical, pyrometallurgical, or electrometallurgical processes. Hydrometallurgical methods achieve high selectivity through chemical leaching but pose significant challenges for effluent and reagent recovery. Pyrometallurgical methods facilitate rapid metal separation through smelting but require substantial energy and may release harmful gases. Electrometallurgical techniques produce high-purity metals but are constrained by pretreatment requirements and the consumption of energy. The non-metallic fraction of PCB waste is recycled using thermochemical conversion, microwave-aided heating, and direct recycling of epoxy–fiberglass composites, enabling material or energy recovery. The recovered polymer from direct recycling may have reduced mechanical strength and poor compatibility with new polymer matrices, and the resulting products from the thermal conversion suffer from incomplete conversion, degradation of quality, and residual contamination, as compared to synthetic polymers. Recent process developments have focused on extracting rare earth and supply-critical materials present at lower concentrations in the waste stream. The literature on existing and emerging approaches for recycling PCB wastes is reviewed to identify sustainable, economically viable, and environmentally responsible strategies for the recovery and reuse of critical materials from waste streams.

36 MATERIALS SCIENCE↗
DOE OSTI2021

Microwave-Assisted Preparation of Luminescent Inorganic Materials: A Fast Route to Light Conversion and Storage Phosphors

Luminescent inorganic materials are used in several technological applications such as light-emitting displays, white LEDs for illumination, bioimaging, and photodynamic therapy. Usually, inorganic phosphors (e.g., complex oxides, silicates) need high temperatures and, in some cases, specific atmospheres to be formed or to obtain a homogeneous composition. Low ionic diffusion and high melting points of the precursors lead to long processing times in these solid-state syntheses with a cost in energy consumption when conventional heating methods are applied. Microwave-assisted synthesis relies on selective, volumetric heating attributed to the electromagnetic radiation interaction with the matter. The microwave heating allows for rapid heating rates and small temperature gradients yielding homogeneous, well-formed materials swiftly. Luminescent inorganic materials can benefit significantly from the microwave-assisted synthesis for high homogeneity, diverse morphology, and rapid screening of different compositions. The rapid screening allows for fast material investigation, whereas the benefits of enhanced homogeneity include improvement in the optical properties such as quantum yields and storage capacity.

59 BASIC BIOLOGICAL SCIENCES↗
DOE OSTI2022

Material Plasma Exposure eXperiment (MPEX) High Heat Flux Bellows for Component Alignment in High Microwave Environment

The Material Plasma Exposure eXperiment (MPEX) device is a linear plasma device developed to perform plasma material interaction experiments under the conditions prototypic of a fusion reactor divertor. MPEX has multiple systems that must be precisely aligned to the plasma axis, including an electron cyclotron heating system that emits up to 400 kW of microwave power into the vacuum vessel. Five distinct systems require precise alignment on the MPEX device, thus requiring four bellows, all of which are adjacent to the plasma at a relatively high heat flux of approximately 47 kW/m2 and microwave power regions. The MPEX high heat flux bellows (HHFB) is designed to deliver 6 degrees of freedom positioning. The HHFB includes titanium–zirconium–molybdenum (TZM) inserts that are brazed into a Glidcop AL-15 body using a high-temperature braze alloy, thus blocking direct line of sight to an edge-welded bellows from the plasma and microwave screen to block microwaves from the bellows. Further, a custom ConFlat knife edge is machined into the Glidcop AL-15, so the vacuum flanges do not need a braze or weld joint on the vacuum interface. Fingerstock or copper mesh is used to restrict microwave power from entering the interstitial space between the water-cooled Glidcop AL-15 body and edge-welded bellows. Glidcop AL-15 was selected as the material of choice for the water-cooled body because it can maintain mechanical integrity at elevated temperatures, and it also allows for a high-temperature braze. TZM was selected for its machinability and compatibility with vacuum and plasma requirements. A test article is also being considered for a similarly shaped component, the MPEX limiter, that will demonstrate the integrity of the braze joint under high thermal load. Results from this testing will be extrapolated to deduce the lifetime and integrity of the HHFB design.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2020

Catalytic direct conversion of ethane to value-added chemicals under microwave irradiation

The reaction mechanism of ethane conversion over 4 % Mo-0.5 % Fe/ZSM-5 catalyst was investigated using two different reactors with different heating modes. A microwave fixed-bed reactor (MWFB) was used and its performance was compared to a conventional thermal fixed-bed reactor (CTFB). Over 80 % ethane conversion was achieved under microwave irradiation mode at 375 °C. Here, to achieve the same ethane conversion conventionally, the reaction temperature had to be elevated to 660 °C in the CTFB. The formation rates and selectivity of the products were compared under these two heating methods. The CTFB products had a higher selectivity towards aromatic compounds; whereas, the MWFB products had a higher selectivity towards ethylene; 26.5 % higher than the CTFB. Carbon analysis over spent catalysts of CTFB showed three distinct types of coke, whereas the microwave resulted in a single higher temperature coke type.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Accelerated Synthesis of Ordered Mesoporous Carbons Using Plasma

Conventional ordered mesoporous carbon (OMC) production usually requires long processing times in the carbonization step to achieve desired temperatures through controlled ramps. To enable expedited materials discovery, developing advanced manufacturing capability with significantly improved throughput is highly desired. Current approaches for accelerating the synthesis of OMCs include using microwave and Joule heating. However, both methods rely on the introduction of additional components, such as microwave absorbers and electrically conductive agents, within the bulk materials to impart the ability to reach high carbonization temperatures. This work demonstrates accelerated synthesis and functionalization of OMCs through the use of a dielectric barrier discharge plasma, where carbonization can be accomplished within 15 min using 30 W plasma sources, representing more than an order of magnitude increase in polymer-to-carbon conversion kinetics compared to that of a traditionally pyrolyzed analogue. Particularly, the ability of performing rapid carbonization without the use of additional substrates within the OMC precursor systems is advantageous. A systematic investigation of how plasma power, time, and gas atmosphere impact the resulting OMC pore textures and properties is performed, demonstrating the broad applicability of plasma-enabled carbonization methods. Furthermore, we demonstrate that the plasma treatment strategy can be extended to incorporate heteroatoms into the carbon framework by introducing ammonia gas, resulting in OMCs with a nitrogen content up to 4.7 at %, as well as non-Pluronic templating systems for synthesizing OMC with pore sizes larger than 10 nm. As employing a plasma source for materials pyrolysis is an industrially relevant approach, our system can be extended toward scaled synthesis of OMCs with much faster production rates.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2024

Relithiation process for direct regeneration of cathode materials from spent lithium-ion batteries

A method for the regeneration of cathode material from spent lithium-ion batteries is provided. The method includes dissolving a lithium precursor in a polyhydric alcohol to form a solution. Degraded cathode material containing lithium metal oxides are dispersed into the solution under mechanical stirring, forming a mixture. The mixture is heat treated within a reactor vessel or microwave oven. During this heat treatment, lithium is intercalated into the degraded cathode material. The relithiated electrode material is collected by filtration, washing with solvents, and drying. The relithiated electrode material is then ground with a lithium precursor and thermally treated at a relatively low temperature for a predetermined time period to obtain regenerated cathode material.

Belharouak, Ilias↗
DOE OSTI2024

Microwave-assisted catalytic gasification of mixed plastics and corn stover for low tar, hydrogen-rich syngas production

The challenge for efficient management of post-consumer plastic and biomass waste has grown over the past few decades due to their dramatic increases. In comparison to conventional gasification, microwave-assisted co-gasification of plastics and corn stover offers many benefits, including increased H 2 yield and gas components compared to unfavorable char/tar. Nonetheless, for future commercialization of the process and ease of product separation, further reduction of the undesirable tar is necessary, which can be achieved over the catalytic route. Here, in this work, we studied the catalytic effect of magnetite for microwave-assisted co-gasification of corn stover and plastic to make syngas with higher H 2 and lower tar selectivity over non-catalytic conditions. A 1:1:1 ratio of plastic-corn stover-magnetite was used to evaluate the reaction parameters such as temperature, space velocity, heating media, and catalytic cycles under gasification conditions. In comparison with the microwave non-catalytic route, a 100% increase in the total H 2 yield with 76% higher H 2 production efficiency (mmol/kWh) was achieved in the presence of the magnetite catalyst, while reducing the overall tar formation from 9% to 2%. When magnetite was reduced in situ during the reaction, it coupled with microwave and delivered oxygen radicals that cracked down plastic and corn stover intermediates generated from the synergistic effect under microwave heating. Soon after the oxygen transfer process initiated, magnetite reached its final oxidation state consisting of microwave-active Fe and Fe 3 C phases that continued coupling with microwaves along with the generated graphitic carbon to maintain the heat necessary to further reduce the generated tar and make additional gaseous products, as confirmed by XRD, Raman, and TGA analyses.

08 HYDROGEN↗
DOE OSTI2020

Electron cyclotron resonance (ECR) magnetometry with a plasma reservoir

The local magnetic field in a Penning–Malmberg trap is found by measuring the temperatures that result when electron plasmas are illuminated by microwave pulses. Multiple heating resonances are observed as the pulse frequencies are swept. The many resonances are due to electron bounce and plasma rotation sidebands. The heating peak corresponding to the cyclotron frequency resonance is identified to determine the magnetic field. A new method for quickly preparing low density electron plasmas for destructive temperature measurements enables a rapid and automated scan of microwave frequencies. This technique can determine the magnetic field to high precision, obtaining an absolute accuracy better than 1 ppm and a relative precision of 26 ppb. One important application is in situ magnetometry for antihydrogen-based tests of charge-parity-time symmetry and of the weak equivalence principle.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗
DOE OSTI2023

Microwave resonance enhanced CO 2 reduction using biochar

The conventional process for CO 2 conversion requires high energy and expensive catalysts, and shows poor product selectivity. Here, in this study, we address these challenges by investigating an environmentally friendly method for CO production through the variable frequency microwave-driven CO 2 Boudouard reaction over biochar. We hypothesized that tuning the microwave frequency to align with the dielectric properties of biochar, and thereby induce a resonance effect, could significantly enhance reaction efficiency. Experiments were conducted to explore the effect of microwave frequency on CO 2 conversion efficiency in the variable frequency microwave reactor operating within a frequency range of 2430–6000 MHz. Results reveal a significant resonance effect at 4225 MHz resulting in an outstanding CO 2 conversion of 96.3%, in sharp contrast to the complete absence of conversion observed at the conventional 2450 MHz. The resonance frequency not only facilitated exceptional conversion but also remarkably improved energy efficiency, yielding a productivity of 1427.5 µmol/kJ of CO. This represents a remarkable 474-fold increase compared to electrical heating. Furthermore, continuous microwave irradiation at this optimized frequency demonstrated remarkable stability and induced substantial enhancements in the pore structure and surface area of biochar. This innovative approach provides promising insights into sustainable and efficient CO production processes.

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

Microwave-Assisted Activation of Mo/HZSM5 in Methane Dehydroaromatization

Natural gas flaring is a significant challenge for oil and gas producers. One viable option to mitigate flaring is the conversion of natural gas into valuable chemicals. Applying microwave energy to heterogenous catalyst materials offers advantages in terms of higher rates and product selectivities in comparison to traditional thermal systems which can be designed for on-demand chemical production in modular reactor systems. Methane dehydroaromatization (MDHA) produces transportable, liquid aromatic products directly from natural gas, which is ideal for remote production but is hindered by low thermodynamic yields and rapid deactivation. The stability and performance of the Mo/ZSM5 catalyst is often determined by the state and nature of Mo in the catalyst, which in turn is dictated by the temperature and gaseous environment during catalyst activation. In this study, the Mo/HZSM5 catalyst was activated under three different heating modes (thermal, microwave E-field, and microwave H-field) and four different gas environments (CO, He, CH4+H2, and H2). All the activated catalysts were characterized using different tools and performance evaluated in MDHA.

methane dehydroaromatization↗
DOE OSTI2024

Insights into Designing an Efficient and Reliable Microwave-Assisted Methane Dehydroaromatization Process: Effect of Microwave Absorber on Catalyst Performance

Microwave-assisted methane dehydroaromatization has the potential to address challenges of traditional dehydroaromatization reactions. However, catalysts for microwave-enhanced reaction systems require effective coupling of fields with the catalyst to produce heat and reach reaction temperatures. Here, this work presents an in-depth understanding of the effect of the addition of silicon carbide as a microwave absorber on catalyst performance among other variables, the viability of the microwave reactor configuration, and insights into designing an effective and reliable microwave-based methane dehydroaromatization process. The effect of other parameters including temperature, weight hourly space velocity, role of microwave absorber, and methane concentration during microwave-assisted methane dehydroaromatization reaction are studied. Mo/ZSM-5 was found to suffer from low permittivity and nonuniform heating under microwave conditions. Mixing silicon carbide powder as a microwave absorber with the catalyst was found to provide more uniform heating. When assessing the catalytic performance of the mixture, it was found that higher methane partial pressures at 2000 cc/g cat .h and a temperature range of 500-600°C produced the highest amount of benzene. The formation of graphitic carbon on the spent catalyst increased with temperature, gas-solid contact period, and methane concentration, which resulted in higher methane conversion and benzene selectivity. The study indicates that under microwave heating the presence of localized carbon enhanced catalyst life by coupling with microwave energy, leading to localized heating, and improving benzene selectivity.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗
DOE OSTI2023

Study of unripe and inferior banana flours pre-gelatinized by four different physical methods

This study aimed to prepare the pre-gelatinized banana flours and compare the effects of four physical treatment methods (autoclaving, microwave, ultrasound, and heat-moisture) on the digestive and structural characteristics of unripe and inferior banana flours. After the four physical treatments, the resistant starch (RS) content values of unripe and inferior banana flours were decreased from 96.85% (RS2) to 28.99–48.37% (RS2 + RS3), while C∞ and k values were increased from 5.90% and 0.039 min −1 to 56.22–74.58% and 0.040–0.059 min −1 , respectively. The gelatinization enthalpy (ΔHg) and I 1047/1022 ratio (short-range ordered crystalline structures) were decreased from 15.19 J/g and 1.0139 to 12.01–13.72 J/g, 0.9275–0.9811, respectively. The relative crystallinity decreased from 36.25% to 21.69–26.30%, and the XRD patterns of ultrasound (UT) and heat-moisture (HMT) treatment flours maintained the C-type, but those samples pre-gelatinized by autoclave (AT) and microwave (MT) treatment were changed to C + V-type, and heat-moisture (HMT) treatment was changed to A-type. The surface of pre-gelatinized samples was rough, and MT and HMT showed large amorphous holes. The above changes in structure further confirmed the results of digestibility. According to the experimental results, UT was more suitable for processing unripe and inferior banana flours as UT had a higher RS content and thermal gelatinization temperatures, a lower degree and rate of hydrolysis, and a more crystalline structure. The study can provide a theoretical basis for developing and utilizing unripe and inferior banana flours.

Zhang, Siwei↗
DOE OSTI2024

Microwave-Assisted Gasification of Biochar: Effect of Operational Parameters and Biochar Composition on Syngas Production

The utilization of microwave-assisted gasification for biomass/plastic is a promising route toward clean energy production, contributing to a reduction in carbon footprint. This method facilitates the conversion of biomass into syngas with enhanced hydrogen (H2) yield, surpassing conventional heating approaches. However, the gasification of biochar, a byproduct resulting from the initial rapid pyrolysis of biomass, appears as a rate-determining step in biomass gasification. To ensure high conversion efficiency, particularly in pilot or larger scales, the maintenance of high biochar reactivity is essential, which can be achieved by introducing catalysts to minimize biochar formation. Furthermore, given the susceptibility of biochar to microwave heating, gaining a comprehensive understanding of its behavior in the presence of microwave-active catalysts under microwave conditions is crucial to obtain valuable insights into the underlying mechanisms, thereby improving overall biomass gasification efficiency. In the previous study, magnetite (Fe3O4) was selected for microwave-assisted gasification for biomass/plastic due to its dual role as a catalyst and microwave absorber and demonstrated considerably enhanced hydrogen production. Herein, Fe3O4 is rationally modified with metal promoters and their synergistic effect toward biochar gasification performance is investigated. The data shows that metal promoted Fe3O4 shows a higher syngas yield than that of pristine Fe3O4 in biochar.

Mai, Duy Hien↗