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Microwave heated chemical looping ammonia synthesis over Fe and CoMo particles
Chemical looping ammonia synthesis (CLAS) materials were subjected to a three cycle ammonia synthesis test under both conventional thermal heating and microwave heating. Microwave heating was found to outperform conventional heating for the first cycle on both Fe and CoMo materials. Principles of microwave catalysis and the heating of metallic particles may be generalized from this study; the dielectric loss tangent for optimum heating must fall within a realtively small range, ~0.8–1.4, and the penetration depth of the microwave into the particle must be considered and optimized for efficient heating, penetration depth should be on the same order as the particle size. The active phases of both catalysts, Fe 4 N and Co 3 Mo 3 N, were found to be responsive to microwave irradiation. Lastly, the deactivation and regeneration of the materials was studied by examining the BET surface areas by reforming surfaces with a low concentration gas phase oxidation reaction. This study sheds light on more general principles of microwave catalysis and on the scale-up of CLAS reactions.
Oxidative ethane dehydrogenation under thermal vs. microwave heating over Ga/ZSM-5 and GaPt/ZSM-5
Conventional thermal heating versus microwave heating for the oxidative dehydrogenation of ethane with CO 2 as the oxidative co-reactant over 2%Ga/ZSM-5 and 1.5%Ga0.5%Pt/ZSM-5. The Ga/ZSM-5 and GaPt/ZSM-5 had a similar ethane conversion under microwave heating at 450 °C, compared to the thermally heated catalyst at 650 °C. The bimetallic GaPt/ZSM-5 performed better than the Ga/ZSM-5. Both the GaPtMWFB-450 °C and GaMWFB-450 °C resulted in a lower production rate to carbon monoxide and water than the TFB-650 °C, suggesting that the microwave heating is less favorable to the water gas shift reaction. In this study, microwave heating increased the catalytic conversion of ethane and selectivity to ethylene.
Temperature Homogeneity under Selective and Localized Microwave Heating in Structured Flow Reactors
Selective heating of different phases of multiphase systems via microwaves can result in energy savings and suppression of side reactions. However, materials properties and operating conditions that maximize temperature gradients are poorly understood. Here we utilize computational fluid dynamics (CFD) computations and temperature measurements in structured flow reactors (monoliths) in a monomodal microwave cavity to assess the temperature difference between the walls and the fluid and develop a simple lumped model to estimate when temperature gradients exist. We also explore the material’s thermal and electrical properties of structured reactors for isothermal catalyst conditions. We propose that CFD simulations can be used as a nonintrusive, predictive tool of temperature homogeneity. Importantly, we demonstrate that localized heating in the bed under several conditions rather than selective heating is responsible for the selectivity enhancement. Furthermore, our results indicate that structured beds made of high thermal conductivity materials avoid arcing and enable temperature homogeneity and low electrical conductivity materials allow microwaves to penetrate the domain.
Multiscale modeling of microwave-heated multiphase systems
Modeling of microwave heating of multiphase systems requires resolving the electromagnetic field from the single particle to the entire cavity. We introduce a multiscale methodology for computationally affordable simulations of microwave heating of multiphase systems consisting of one phase dispersed in a continuum phase. The methodology homogenizes the original multiphase system, by taking advantage of the large separation of length scales, to calculate the effective permittivity, effective thermal conductivity, and volumetric power absorbed in each phase. The methodology is rigorously assessed against particle-resolved detailed numerical simulations of model systems. We demonstrate a significant reduction in computational cost while retaining the accuracy of detailed simulations. Lastly, the present methodology enables high throughput exploration of novel multiphase system designs utilizing microwave heating.
Containerless synthesis of ceramic materials using microwave heating
It was demonstrated that microwave heating technique may be employed for the synthesis of a number of multicomponent ceramic oxide-based materials, e.g., YBa2Cu3O7 and CuFe2O4. A characteristic, and potentially extremely useful, feature of such synthesis is that they occur in significantly less time than that required using conventional furnace-based techniques. However, the information obtained to date is necessarily rather empirical, and systematic investigations of the use of microwave heating for the synthesis of ceramic materials are required. The synthesis of ceramic materials at high temperatures are often affected by unwanted, deleterious reactions of the reactants and/or products with the reaction container. Consequently, it is of interest to investigate the high temperature synthesis of ceramic materials using microwave heating in a containerless environment.
Modeling the Effects of Microwave Heating on Densification in Chemical Vapor Infiltration
Microwave heating has great potential to accelerate the synthesis of ceramic matrix composites (CMCs) by a process called Chemical Vapor Infiltration (CVI). In CVI, reactive gases ingress a porous preform and undergo chemical transformation to deposit solid ceramic phase within the pores at high temperature thus, densifying the preform. However, the competing effects of chemical kinetics and gas transport are known to result in non-uniform densification as the outer surfaces of the preform experience faster depositions compared to the core. Achieving spatial temperature control plays a key role improving the densification quality. Microwave heating can potentially create temperature inversion such that the core of the preform is hotter than the outer surface and subsequently, lead to improved densification while keeping the manufacturing times and costs low. In the present work, a computational modeling strategy has been developed that accounts for the key physical phenomena responsible for densification of porous preforms using microwave heating. Specifically, a chemical kinetics model has been formulated for Silicon Carbide (SiC) deposition from MTS/H2 precursor. The model is implemented in a pore-resolved reactive transport solver, Quilt. The CVI simulations are performed for several conditions. Initially, parameterized temperature control is imposed to identify optimum conditions for good densification quality at a fraction of processing time. Further, simulations of microwave heating of porous SiC preforms are performed using OpenFOAM. A strategy to achieve and enhance temperature inversion is identified. The resulting temperature profiles are used in the pore-resolved densification simulations to analyze the densification behavior. It is observed that the temperature inversion achieved by microwave heating leads to significant improvements in densification quality and at the same time, keeps the manufacturing time low.
Microwave heating of lunar materials. Appendix A
Microwave heating of nonmetallic inorganic material has been of interest for many years. Von Hippel in the late 1940's and early 1950's investigated how microwave radiation up to 10 GHz couples to various insulator materials. Perhaps the most work has been done by Wayne Tinga at the University of Edmonton. Most of the work to date has been done at the two frequency bands allowed in industrial use (0.915 GHz and 2.45 GHz). However some work has recently been carried out at 28 GHz and 60 GHz. Work done in this area at Los Alamos National Laboratory is discussed.
Reduced graphene oxide catalytically enhances the rate of cyanate ester curing under variable frequency microwave heating
Here, the curing of Lonza Primaset PT-30 novolac cyanate ester resin and EPON 826 bisphenol-A diglycidyl ether were investigated using convective thermal heating and variable frequency microwave (VFM) heating. The addition of 1 part per hundred reduced graphene oxide (r-GO) to PT-30 novolac cyanate ester increased the VFM cure rate compared to thermal heating. Curing it at 160°C for 240 min with VFM heating resulted in a 55% degree of cure compared to a 26% degree of cure with thermal heating. This observed VFM rate enhancement is due to selective microwave heating of the r-GO particles in the resin resulting in increased r-GO catalytic activity toward cyanate ester curing. It is both a thermal and catalytic effect, the latter of which is absent when r-GO is added to a bisphenol-A diglycidyl ether resin with o-phenylenediamine hardener. Impurities present in the PT-30 matrix do not appear to contribute to its overall cure kinetics, nor do they participate in the observed VFM rate enhancement.
Analysis of microwave-heated rocket engines for space propulsion
Microwave-heated plasmas in convergent nozzles are analyzed using a coupled Maxwell and Navier-Stokes solver to examine relevant issues associated with microwave thermal propulsion. Parametric studies are conducted to understand the effect of power, pressure, and plasma location with respect to the nozzle throat. For nozzles in the 0.5 to 3 N range with helium flow, results show that specific impulses up to 550-650 sec are possible, with further increases being limited by severe wall-heating. Coupling efficiencies of over 90 percent are consistently obtained, with overall efficiencies ranging from 40 percent to 80 percent. Size scale-up studies (done by scaling the frequency from 2.45 GHz to 0.91 GHz) indicate that plasma migration toward the walls occurs more frequently for the lower frequency. Increasing the cavity aspect ratio and detuning the cavity are found to be effective ways of keeping the plasma on-axis.
Carbon Nanotube Supported Amorphous MoS 2 via Microwave Heating Synthesis for Enhanced Performance of Hydrogen Evolution Reaction
Amorphous molybdenum disulfide (MoS 2 ) is a promising electrochemical catalyst for hydrogen evolution reaction (HER) due to more active sites exposed on the surface compared to its crystalline counterpart. In this study, a novel fast three-minute one-pot method is proposed to prepare the single-wall carbon nanotube- (SWCNT-) supported amorphous MoS 2 via a microwave heating process. Compared to traditional hydro- or solvent thermal methods to prepare MoS 2 which usually consume more than 10 hours, it is more promising for fast production. An overpotential at 10 mA/cm 2 of amorphous MoS 2 @SWCNT is 178 mV, which is 99 mV and 22 mV lower than crystalline MoS 2 @SWCNT and pure amorphous MoS 2 , respectively. After running 1000 cycles of polarization, ~2% increase in overpotential is observed, indicating its good stability. The enhanced performance results from the beneficial combination of the SWCNT substrate and the amorphous microstructures. The introduction of SWCNT increases catalyst conductivity and prevents MoS 2 aggregation. The amorphous microstructures of MoS 2 prepared by a microwave heating method lead to more Mo edges or active sites exposed.
Operation and Optimization of Microwave-Heated Continuous-Flow Microfluidics
Microwave (MW) technology can be powerful for electrification and process intensification but limited fundamental understanding of scalability and design principles hinders its effective use. In this work, we build a continuous-flow microreactor inside a commercial single-mode MW applicator and the corresponding computational fluid dynamics model to simulate the temperature profile. The model is in good agreement with experiments for various microreactor dimensions and operating conditions. The model indicates that MW heating is greatly influenced by reactor geometry as well as the operating parameters. We observe a strong correlation between parameters and develop a gradient boost regression tree model to predict the outlet temperature accurately. This model is then applied to optimize the dimensions and operating conditions to maximize the outlet temperature and energy efficiency, resulting in a Pareto optimal. We demonstrate computationally and experimentally that it is possible to surpass the Pareto optimal and achieve an energy efficiency of ~90% or greater at temperatures relevant for liquid-phase chemistry via salting of the solvent. The present methodology can be applied to other complex MW reactors. Lastly, the combined numerical and experimental approach provides insights into and a framework for scale-up and optimization.
Chemical recycling of polymer composites induced by selective variable frequency microwave heating
Abstract The application of variable frequency microwave (VFM) heating to achieve rapid thermal depolymerization of polymer composites is reported for the first time. The thermal and chemical influence of composite additives on polymer decomposition has been studied for a set of chemically recyclable polymers, including polyphthalaldehyde, polypropylene carbonate, two polyhydroxyalkanoates, and nylon 6. Carbon‐based additives, specifically nanocarbon particles, were used as effective microwave absorbers to controllably degrade the surrounding polymer matrix into valuable, monomeric compounds. Depolymerization and byproduct confirmation were quantified by gel permeation chromatography and nuclear magnetic resonance spectroscopy. Synergistic effects can be leveraged from pre‐treating composite samples to further reduce the total microwave energy required to depolymerize composite samples. This study establishes the use of VFM heating for chemical recycling of polymer composites that can be leveraged toward a plastic circular economy.
Microwave heating and joining of ceramic cylinders: A mathematical model
A thin cylindrical ceramic sample is placed in a single mode microwave applicator in such a way that the electric field strength is allowed to vary along its axis. The sample can either be a single rod or two rods butted together. We present a simple mathematical model which describes the microwave heating process. It is built on the assumption that the Biot number of the material is small, and that the electric field is known and uniform throughout the cylinder's cross-section. The model takes the form of a nonlinear parabolic equation of reaction-diffusion type, with a spatially varying reaction term that corresponds to the spatial variation of the electromagnetic field strength in the waveguide. The equation is analyzed and a solution is found which develops a hot spot near the center of the cylindrical sample and which then propagates outwards until it stabilizes. The propagation and stabilization phenomenon concentrates the microwave energy in a localized region about the center where elevated temperatures may be desirable.
Broadening of microwave heating beams in the DIII-D tokamak by edge turbulence
Abstract We have demonstrated for the first time that turbulent plasma density fluctuations in the edge of the DIII-D tokamak are responsible for substantial broadening of an injected microwave beam by successful quantitative comparison between experimental observations and first principles 2D full-wave simulations. The broadening of the beam has important implications for control of tokamak discharges through localized electron cyclotron deposition needed for eliminating magnetohydrodynamic instabilities. This new predictive capability is mandatory to design & operate present & future tokamaks in such a way that microwave heating schemes achieve their intended objectives.
Finite Element Analysis of Three Methods for Microwave Heating of Planetary Surfaces
In-Situ Resource Utilization will be Ground Breaking technology for sustained exploration of space. Volatiles are present in planetary regolith, but water by far has the most potential for effective utilization. The presence of water at the lunar poles and Mars opens the possibility of using the hydrogen for propellant on missions beyond Earth orbit. Likewise, the oxygen could be used for in-space propulsion for lunar ascent/descent and for space tugs from low lunar orbit to low Earth orbit. Water is also an effective radiation shielding material as well as a valuable expendable (water and oxygen) required for habitation in space. Because of the strong function of water vapor pressure with temperature, heating regolith effectively liberates water vapor by sublimation. Microwave energy will penetrate soil and heat from within, much more efficiently than heating from the surface with radiant heat. This is especially true under vacuum conditions since the heat transfer rate is very low. The depth of microwave penetration is a strong function of the microwave frequency and to a lesser extent on regolith dielectric properties. New methods for delivery of microwaves into lunar and planetary surfaces is being prototyped with laboratory experiments and modeled with COMSOL MultiPhysics. Recent results are discussed.
Insight into Enhanced Microwave Heating for Ammonia Synthesis: Effects of CNT on the Cs–Ru/CeO 2 Catalyst
Not Available
Design considerations for microwave heating of space food
Reliability, weight, size, and power supplies as factors in designing microwave ovens for spacecraft