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DOE OSTI2024

Modeling Microwave-Enhanced Chemical Vapor Infiltration Process for Preventing Premature Pore Closure

The chemical vapor infiltration (CVI) process involves infiltrating a porous preform with reacting gases that undergo chemical transformation at high temperatures to deposit the ceramic phase within the pores, ultimately leading to a dense composite. The conventional CVI process in composite manufacturing needs to follow an isothermal approach to minimize temperature differences between the external and internal surfaces of the preform, ensuring that reactive gases infiltrate internal pores before external surfaces seal. This study addresses the challenge of premature pore closure in CVI processes through microwave heating. A frequency-domain microwave solver is developed in Open-FOAM to investigate volumetric heating mechanisms within the preform. Through numerical studies, we demonstrate the capability of microwave heating of creating an inside-out temperature inversion. This inversion accelerates reactions proximal to the preform center, effectively mitigating the risk of premature external pore closure and ensuring uniform densification. The results reveal a significant enhancement in temperature inversion when high-permittivity reflectors are incorporated to generate resonant waves. This microwave heating strategy is then coupled with high-fidelity direct numerical simulation (DNS) of reacting flow, enabling the analysis of resulting densification processes. The DNS simulation includes detailed chemistry and realistic diffusion coefficients. The numerical results can be used to estimate the impact of microwave-induced temperature inversion on densification in productions.

Ge, Wenjun↗

DOE OSTI2023

Controlling PET oligomers vs monomers via microwave-induced heating and swelling

The production of polyethylene terephthalate (PET) bottles and fibers, and their subsequent mismanagement, have created an urgent need to develop strategies to handle the resulting waste. Here, in this work, glycolysis of PET using manganese oxide catalysts under microwave-assisted heating is demonstrated to form oligomers and the monomer bis(2-hydroxyethyl) terephthalate (BHET) at moderate conditions. Higher surface area catalysts achieve faster overall rates of depolymerization to the monomer. Oligomers form homogeneously and depolymerize to monomers over manganese oxide. The polymer-to-solvent ratio and reaction temperature affect the overall oligomer yield. The swelling of PET, caused by the diffusion of ethylene glycol into the polymer matrix, causes the dissolution of the PET to form oligomers. Oligomers are characterized and show similar physical properties to the starting PET despite having 1/20th of the molecular weight.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS2006

Development of a Microwave Facility for Processing Lunar Regolith

This viewgraph presentation reviews in this Roadmap for Developing a Lunar Microwave Facility an approach to determine the source of the enhanced microwave heating of Lunar Regolith. A set of microwave heating studies were proposed for a specially designed realistic simulant to determine optimum processing parameters. Apollo lunar soil will be used to validate the heating features found for the simulant. We have also introduced several possible designs for a future lunar microwave processing facility. In the future when sufficient funds become available, a microwave facility for processing regolith on the lunar surface will be ready to be built

microwave processing↗

NASA NTRS1994

(abstract) Steady State Temperature Profile in a Cylinder Heated by Microwaves

We have developed a new theory to calculate the steady state temperature profile in a cylindrical sample positioned along the entire axis of a cylindrical microwave cavity. Temperature profiles were computed for alumina rods of various radii excited by one of the TM0n0 modes with n = 1, 2, or 3. Sample surface and center temperatures will be presented as a function of total sample absorbed power or electric field strength at the sample surface. An approach for attaining more uniform heating within the sample by reducing the magnitude of the inverted temperature profile using a concentric outer cylindrical tube will be discussed.

microwave↗

DOE OSTI2022

Microwave assisted heating of plastic waste: Effect of plastic/susceptor (SiC) contacting patterns

We discuss plastic accumulation as a growing sustainability challenge. Most plastics are thermally inert at room temperature, requiring high temperatures for depolymerization. In the quest for developing sustainable plastic upcycling, we investigate silicon carbide (SiC) as microwave absorbing susceptors for reaching depolymerization temperatures. We utilize three SiC topologies – particles, hot-pressed plastic films containing SiC particles, and monoliths. SiC particles of >0.5 mm in diameter can provide heating rates approaching ~200 °C/min at modest powers. Still, physically mixed plastic-susceptor beds suffer from density differences, causing non-uniform contact during plastic softening and melting. Hot-pressed plastic films containing SiC particles allow uniform plastic-susceptor contact but suffer from slow heating as only a single layer of susceptors exists between polymer layers. SiC monoliths mitigate these challenges by preferentially dissipating the microwaves and rapidly heating the plastics independently of polymeric properties.

36 MATERIALS SCIENCE↗

NASA NTRS2000

Uniform batch processing using microwaves

A microwave oven and microwave heating method generates microwaves within a cavity in a predetermined mode such that there is a known region of uniform microwave field. Samples placed in the region will then be heated in a relatively identical manner. Where perturbations induced by the samples are significant, samples are arranged in a symmetrical distribution so that the cumulative perturbation at each sample location is the same.

Barmatz, Martin B.↗

DOE OSTI2023

The selective heating effect of microwave irradiation on a binary mixture of water and polyethylene oxide: a molecular dynamics simulation approach

In this study, we investigate the molecular mechanisms of a microwave-driven selective heating process by performing molecular dynamics simulations for three different systems including pure water, pure polyethylene oxide (PEO), and water-PEO mixed systems in the presence of a microwave with two different intensities of electric field such as 0.001 V/Å -1 and 0.01 V/Å -1 at a frequency of 100 GHz. First, from performing molecular dynamics simulations of CO and CO 2 in the presence of the microwave, it is confirmed that the molecular dipole moment is responsible for the rotational motion induced by the oscillating electric field. Second, by analyzing the MD simulations of the pure water system, we discover that the dipole moment of water exhibits a time lag with respect to the microwave. During the heating process, however, the temperature, kinetic, and potential energies increase synchronously with the oscillating electric field of the microwave, showing that the heating of the water system is caused by the molecular reaction of water to the microwave. Comparing the water-PEO mixed system to the pure water and pure PEO systems, the water-PEO mixed system has a higher heating rate than the pure PEO system but a lower heating rate than the pure water system. Therefore, we conclude that heating the water-PEO mixed system is driven by water molecules selectively activated by microwave irradiation. Furthermore, we also calculate the diffusion coefficients of water molecules and PEO chains by describing their mean square displacements, demonstrating that the diffusion coefficients are increased in the presence of microwaves for both water and PEO in pure and mixed systems. Lastly, during the microwave heating process, the structures of the water-PEO mixed system are altered as a function of the intensity of electric field, which is mainly driven by the response of water molecules.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1979

Non-flammable polyimide materials for commercial application

Thermally-stable, fire-resistant polyimide foams developed for use as fire protection in aircraft, spacecraft and ground applications are presented. Polyimide precursors, synthesized by the reaction of 3, 3', 4, 4'-benzophenone tetracarboxylic acid dianhydride with a mixture of two diamines, can be processed into foams by indirect or direct heating techniques. Flexible resilient foams and thermal acoustical foams produced by the microwave heating of polyimide precursors are shown to conform to requirements for aircraft seating foams and thermal and acoustical insulation materials, respectively. Rigid polyimide foams reinforced by carbon mat, chopped carbon mat and chopped glass strand fillers and prepared by the microwave heating of a continuous mat, followed by its compression, or by filling a honeycomb structure with low density foam, are found to exhibit outstanding fire resistance and have mechanical properties approaching those desired for structural materials.

Gagliani, J.↗

DOE OSTI2024

Distributed Temperature Profiles of Silicon Carbide Catalyst Bed in a Microwave Reactor using Fiber-optic Sensor

Microwave heating is of great interest for reducing greenhouse gas emissions of catalytic chemical conversion processes because it can heat up the reactants rapidly and efficiently and accelerate reaction rates. In microwave-assisted catalytic thermochemical conversion processes, accurate internal temperature measurement would help facilitate effective process control. Metallic thermocouples interfere and spark in the microwave heating environment, so they are not an option. Infrared pyrometers typically provide a single temperature value by averaging over a finite surface area of the catalyst bed. In this work, we use fiber-optic sensors passing through the catalyst bed to provide more accurate temperatures along the height of the catalyst bed. The fiber optic sensors are immune to the electromagnetic microwave radiation and provide temperature profiles along their length. Here, custom fiber-optic sensors were coupled to the optical distributed temperature sensing devices to measure the temperature profiles along the height of the catalyst bed at high temperatures with ~1 mm spatial resolution. The sensing devices use optical frequency domain reflectometry (OFDR) technique for distributed temperature measurement. This work shows the temperature profiles along the height of the silicon carbide powder catalyst bed in the variable and fixed frequency microwave reactors.

Thapa, Juddha↗

NASA NTRS2007

Microwave Extraction of Water from Lunar Regolith Simulant

Nearly a decade ago the DOD Clementine lunar orbital mission obtained data indicating that the permanently shaded regions at the lunar poles may have permanently frozen water in the lunar soil. Currently NASA's Robotic Lunar Exploration Program, RLEP-2, is planned to land at the lunar pole to determine if water is present. The detection and extraction of water from the permanently frozen permafrost is an important goal for NASA. Extraction of water from lunar permafrost has a high priority in the In-Situ Resource Utilization, ISRU, community for human life support and as a fuel. The use of microwave processing would permit the extraction of water without the need to dig, drill, or excavate the lunar surface. Microwave heating of regolith is potentially faster and more efficient than any other heating methods due to the very low thermal conductivity of the lunar regolith. Also, microwaves can penetrate into the soil permitting water removal from deep below the lunar surface. A cryogenic vacuum test facility was developed for evaluating the use of microwave heating and water extraction from a lunar regolith permafrost simulant. Water is obtained in a cryogenic cold trap even with soil conditions below 0 C. The results of microwave extraction of water experiments will be presented.

Ethridge, Edwin C.↗

NASA NTRS2009

Continuous-Flow System Produces Medical-Grade Water

A continuous-flow system utilizes microwave heating to sterilize water and to thermally inactivate endotoxins produced in the sterilization process. The system is designed for use in converting potable water to medical-grade water. Systems like this one could be used for efficient, small-scale production of medical- grade water in laboratories, clinics, and hospitals. This system could be adapted to use in selective sterilization of connections in ultra-pure-water-producing equipment and other equipment into which intrusion by microorganisms cannot be tolerated. Lightweight, port - able systems based on the design of this system could be rapidly deployed to remote locations (e.g., military field hospitals) or in response to emergencies in which the normal infrastructure for providing medical-grade water is disrupted. Larger systems based on the design of this system could be useful for industrial production of medical-grade water. The basic microwave-heating principle of this system is the same as that of a microwave oven: An item to be heated, made of a lossy dielectric material (in this case, flowing water) is irradiated with microwaves in a multimode microwave cavity. The heating is rapid and efficient because it results from absorption of microwave power throughout the volume of the lossy dielectric material. In this system, a copper tube having a length of 49.5 cm and a diameter of 2.25 cm serves as both the microwave cavity and the sterilization chamber. Microwave power is fed via a coaxial cable to an antenna mounted inside the tube at mid-length (see figure). Efficient power transfer occurs due to the shift in wavelength associated with the high permittivity of water combined with the strong coupling of 2.45-GHz microwaves with rotational-vibrational transitions of the dipolar water molecule.

Akse, James R.↗

DOE OSTI2022

Methane Catalytic Pyrolysis by Microwave and Thermal Heating over Carbon Nanotube-Supported Catalysts: Productivity, Kinetics, and Energy Efficiency

Methane catalytic pyrolysis, which is the reaction to produce hydrogen and carbon without emitting CO 2 , represents an approach for decarbonization using natural gas as an energy resource. In this work, the endothermic pyrolysis reaction was carried out under two heating scenarios: convective thermal heating and microwave-driven irradiative heating. The pyrolysis reaction was conducted at 550-600 °C over carbon nanotube-supported Ni-Pd and Ni-Cu catalysts. On both catalysts, an enhanced methane conversion rate was observed under microwave irradiation. The enhanced catalytic activity was hypothetically caused by the presence of free electrons in the carbon atoms within CNT that enabled the CNT support to absorb microwave energy effectively and to be heated efficiently by microwave. The microwave catalytic pyrolysis has shown improvement in kinetics, where the apparent activation energy dropped from 45.5 kJ/mol under conventional convective heating to 24.8 kJ/mol under microwave irradiation. When the methane conversion rate is increased by 37 %, the microwave power consumption only changed by 10.8 %. The research demonstrated the potential of transforming natural gas to clean hydrogen and value-added carbon in a more energy-efficient way. Process simulation and techno-economic analysis showed that potentially hydrogen minimum selling price of about $1 /kg H 2 could be achieved.

03 NATURAL GAS↗

DOE OSTI2020

p-type conductivity and damage recovery in implanted GaN annealed by rapid gyrotron microwave annealing

We demonstrate p-type activation of GaN doped by Mg ion implantation, and in situ during metalorganic chemical vapor deposition through sequential short-duration gyrotron microwave heating cycles at temperatures of 1200–1350 °C. GaN is implanted with 1019 cm−3 Mg ions, capped with AlN, and annealed under 3 MPa N2 overpressure in 5 s heating cycles for less than 60 s total using a high-power gyrotron microwave heating source. Through I–V characterization, photoluminescence spectroscopy, and Raman spectroscopy, we study the evolution of electrical properties, optically active point defects, and material strain in response to implantation and annealing. For Mg-implanted samples, increasing annealing temperature is characterized by an increase in the PL substitutional Mg-related peak (UVL) relative to the shallow-donor vacancy-related peak (GL2). Through comparison of implanted and in situ doped samples, it is demonstrated that the origin of compensating VN lies primarily in implantation rather than degradation from the annealing process. Transmission line measurements and diode I–V measurements show a sheet resistance of 1083 kΩ/□ and a hole concentration of 1.23 × 1015 cm−3, respectively, in the Mg-implanted material annealed at 1350 °C. We conclude that temperature-cycled gyrotron annealing at 1350 °C decreases implant-induced compensating point defects and activates Mg to obtain selective p-type conduction.

Meyers, V. (ORCID:0000000176731553)↗

NASA NTRS1982

Evaluation of waveguide coating materials

Waveguide coating materials were tested at 8470 MHz for insertion loss. Samples of these coatings on waveguide pieces without flanges were tested in an environmental chamber to simulate the effects of high power microwave heating. Test results indicated that three types of coating materials are acceptable with regard to insertion loss. However, simulated microwave heating caused debonding of Metcot 7 and BD-991 coatings, resulting in peelings in the waveguide. The higher cost Chemglaze R104 does not exhibit this problem.

Chen, W. C. J.↗

DOE OSTI2020

Effect of magnetic field ripple on parallel electron transport during microwave plasma heating in the Proto-MPEX linear plasma device

The Prototype Material Plasma Exposure eXperiment (Proto-MPEX) is a linear plasma device located at Oak Ridge National Laboratory to develop the plasma source concept for the Materials Plasma Exposure eXperiment (MPEX). Recent experiments have demonstrated the heating of electrons in a high-density deuterium plasma (n e ~ 5 × 10 19 m -3 ) via electron Bernstein waves and source plasma production via helicon waves in this linear configuration. Moreover, experimental observations suggest that the magnetic ripple adversely affects the parallel transport of the heated electrons toward the target where material samples are to be exposed to the plasma. In order to understand the transport process during microwave application, a test-particle Monte-Carlo (MC) code has been developed that incorporates the effects of Coulomb collisions, magnetic mirror adiabatic trapping and electron cyclotron interaction via a quasilinear RF heating operator. MC calculations indicate that the absence of 2nd turning points along the trajectory of cyclotron heated electrons significantly reduces adiabatic trapping and maximizes power transport to the Target surface. Thermalization of cyclotron heating electrons is analyzed with the MC code and it is found that for conditions relevant to ProtoMPEX, a significant fraction of the absorbed heating power is coupled to the Target surface via ballistic fast electrons; however, under certain conditions, up to 60% of the absorbed RF power can be dissipated via thermalization of the fast electrons on the background plasma. Results are compared with experimental measurements. Finally, the implications of the results are discussed in the context of the upcoming MPEX device.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

A Step toward Process Electrification: Microwave-Assisted Co-Gasification of Waste Plastics and Biomass to Produce Clean Energy

Barely 9% of the 353 million metric tons of plastic waste produced worldwide over the last two decades has been recycled, with the majority of it being either landfilled or incinerated. Recycling and upcycling plastic waste is thus essential in mitigating environmental pollution. Gasification is the thermochemical conversion of solid carbon feedstock at high temperatures using a gasifying agent to produce hydrogen-rich syngas. Existing gasification technologies are energy-intensive and require high operating temperatures (>1000 °C), leaving them uncommercial. Microwave heating has sparked attention in a variety of chemical processes due to its specific advantages over traditional heating technologies, such as rapid and selective heating to improve process efficiency. NETL’s research team recently investigated the synergistic advantages of corn stover and mixed plastics in producing hydrogen-rich syngas via microwave heating. As a continuation of the research, this study provides an outlook over the non-catalytic versus catalytic effects of plastic-corn stover gasification via process electrification to enhance H2 production, minimize undesired tar, and improve process efficiency. Our aim is to provide complete electrification of the existing gasification process by using waste plastics as a starting block to produce valuable fuel and support the nation’s net zero goals.

Abedin, Ashraf↗

DOE OSTI2025

Exploring Catalyst Compositions for Microwave-Assisted Methane Dehydroaromatization

The flaring of natural gas in U.S. shale regions remains a challenge for producers. One alternative to flaring is converting the wasted gas into valuable chemicals. Microwave-based processes offer a promising solution, potentially enabling the development of compact, modular systems for on-site production of chemicals, such as aromatics, from natural gas. This is due to the advantages of microwave heating, including efficient heating of compact volumes, accelerated reaction rates, and electrification of heating. However, developing effective catalysts for microwave-based processes is challenging, as conventional materials often require modification to be effectively heated by microwaves. This study provides an overview of a catalyst development project focused on a molybdenum-supported zeolite catalyst, optimized for the direct conversion of methane into aromatics under microwave irradiation. It details the synthesis, characterization, and the effects of promoters, as well as computational efforts undertaken to understand and enhance the catalyst's performance.

flare gas↗

NASA NTRS1995

Steady State Temperature Profile in a Cylinder Heated by Microwaves

A new theory has been developed to calculate the steady state temperature profile in a cylindrical sample positioned along the entire axis of a cylindrical microwave cavity. Temperature profiles where computed for- alumina rods of various radii contained in a cavity excite in one of the TM(sub OnO) modes with n = 1, 2 or 3. Calculations where also performed with a concentric outer cylindrical tube surrounding the rod to investigate hybrid heating. The parameters studies of the sample center and surface temperature where performed as a function of the total power transmitted into the cavity. Also, the total hemispherical emissivity was varied at boundaries of the rod, surrounding tube, and cavity walls. The result are discussed in the context of controlling the average rod temperature and the temperature distribution in the rod during microwave processing.

Jackson, H. W.↗