Low Pressure and Low Temperature Hermetic Wafer Bonding Using Microwave Heating
We bonded gold on silicon substrates (Au/Si) for a MEMS application by using microwave radiation in a single-mode cavity.
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We bonded gold on silicon substrates (Au/Si) for a MEMS application by using microwave radiation in a single-mode cavity.
Changes in the properties of the lower ionosphere due to ohmic heating of the plasma by the solar power satellite (SPS) microwave power beam are considered. The development of a predictive model of the underdense interaction of an electromagnetic beam and the lower ionosphere is described. The extent to which the Platteville and Arecibo experiments simulate SPS conditions is considered.
The use of intermetallic Pt–Co nanocrystals (NCs) for the electrocatalytic oxygen reduction reaction is quickly gaining interest thanks to the higher electrochemical stability of the intermetallic L1 o phase compared to a random alloy A1 phase. However, the thermal treatment that enables the intermetallic phase transformation also causes considerable NC aggregation, resulting in a significant loss of electrochemically active surface area. Herein, we report the use of microwave radiation to induce the intermetallic phase transformation in Cu-doped Pt–Co NCs. We demonstrate that microwave radiation reduces NC aggregation while allowing for a complete phase transformation in only 30 s. Furthermore, these microwave-treated NCs demonstrate higher mass activity for the oxygen reduction reaction while maintaining electrochemical stability similar to the thermally annealed samples.
We have developed a model for microwave heating of a sphere in a rectangular resonant cavity. The model calculates transient temperature distributions within a sphere during the approach to steady state conditions or on the path to thermal runaway.
Securing domestic sources of critical minerals (CM) is paramount to ensuring a robust and self-sustaining technology infrastructure. Utilizing untapped non-conventional sources, like acid mine drainage, coal ash, bauxite residue/red mud, and more is an emerging approach that addresses this national concern while identifying new value-added pathways originating from waste streams. Red mud is a byproduct of the Bayer process that produces alumina and contains a wealth of CM – 50 µg/g Ga, 2.9 mg/g total rare earth elements plus yttrium, 12 mg/g Mn, 58 mg/g Al, and others. About 170 MM tonnes of red mud are co-produced annually alongside the 142 MM tonnes of alumina generated, highlighting the abundancy of this feedstock. In this work, different strategies were explored for extracting CM from authentic bauxite residue that involve thermal heating, microwave heating, and sonication all with different acids and buffers. CM recovery was then explored one step further by testing the adsorption of the extracted metals onto NETL’s Multi-functional Sorbent Technology (MUST). Microwave treatment of red mud proved the most effective CM extraction, whereas sonication was less desirable due to scale-up concerns. Successful recovery of CM from this leachate with MUST supports further studies toward optimizing the overall process.
This review article focuses on the latest advances in the synthesis of inorganic nano-catalysts using microwave heating, which has progressed significantly since its initial implementation in the mid-1980s. Over the years, nanoparticles (NPs), which inherently offer better surface accessibility for heterogeneous catalysis, have been synthesized using a wide array of heating methods. Microwave heating is one such method and employs a unique heating mechanism that can have several benefits for catalysis. When compared to conventional form of heating which relies on inter-layer mixing via convection, microwave heating operates through the chemical polarity in the target chemicals leading to an “inside-out” mode of heating. This heating mechanism is more targeted and therefore results in rapid synthesis of catalytically active NPs. Platinum group metals (PGM) have classically been the focus of nano-catalysis; however, recent efforts have also applied non-PGM group metals with the goals of lower costs, and ideally, improved catalytic reactivity and durability. This is especially of interest with respect to Pd because of its current historically high cost. Investigations into these new materials have primarily focused on new/improved synthetic methods and catalytic compositions, but it is important to note that these approaches must also be economic and scalable to attain practical relevance. With this overarching goal in mind, this review summarizes notable recent findings with a focus on Pd-dilution and microwave heating in a chronological fashion.
Compared to traditional heating, microwave-assisted heating enhances catalyst activity, selectivity and stability. These features are essential in gasification to improve the process outcome while mitigating the generation undesirable by-products such as char. To study the effect of microwaves on fluidized bed reactors, the electromagnetics module of COMSOL and MFiX are coupled using file input/output wherein external calls are made to COMSOL from MFiX. The particle bed heating rates and temperature distributions are investigateed in the case of a monodisperse bed of magnetite particles subjected to single mode transverse electric and magnetic fields in reacting and non-reacting conditions. The effect of inlet gas velocity on the heating rate of particle is also explored in this work.
Microwaves (MWs) can enable the electrification and intensification of chemical manufacturing. They have been applied to various unit separations, such as drying, distillation, and extraction, entailing gas–liquid and solid–liquid systems. However, a limited quantitative understanding of MW-heated liquid–liquid biphasic systems related to extraction exists. This work measures the temporal and spatial temperature difference between an aqueous and an organic phase in batch and continuous microfluidic modes. We demonstrate permanent temperature differences between phases over 35 °C and spatiotemporal periodic and quasiperiodic oscillations modulated by the flow patterns. The temperature differences are primarily driven by the faster absorption rate of MW irradiation by the aqueous phase versus the slower heat transfer from the aqueous phase to the organic phase. These are amplified by low specific interfacial area and modifications of the electromagnetic field. We employ a multiphysics model to predict the temperature difference in a batch system. The model is in good agreement with the experiments. We demonstrate a strong effect of input power, dielectric properties of organic solvents, the volume of solvents, and the volume ratio between phases on the temperature difference. A simple analytical model describes the temperature difference and provides design principles. Furthermore, the combined approach offers new insights into the design and optimization of the MW-heated biphasic systems.
Agglomerates of polar molecules in nonpolar solvents are selectively heated by microwave radiation. The magnitude of the selective heating was directly measured by using the temperature dependence of the intensities of the Stokes and anti-Stokes bands in the Raman spectra of p-nitroanisole (pNA) and mesitylene. Under dynamic heating conditions, a large apparent temperature difference (ΔT) of over 100 °C was observed between the polar pNA solute and the nonpolar mesitylene solvent. This represents the first direct measurement of the selective microwave heating process. The magnitude of the selective microwave heating was affected by the properties of the agglomerated pNA. As the concentration of the pNA increases, the magnitude of the selective heating of the pNA was observed to decrease. This is explained by the tendency of the pNA dipoles to orient in an antiparallel fashion in the aggregates as measured by the Kirkwood g value, which decreased with increasing concentration. This effect reduces the net dipole moment of the agglomerates, which decreases the microwave absorption. After the radiation was terminated, the effective temperature of the dipolar molecules returned slowly to that of the medium. The slow heat transfer was modeled successfully by treating the solutions as a biphasic solvent/solute system. Based on modeling and the fact that the agglomerate can be heated above the boiling temperature of the solvent, an insulating layer of solvent vapor is suggested to form around the heated agglomerate, slowing convective heat transfer out of the agglomerate. Furthermore, this is an effect unique to microwave heating.
Utilizing liquid amines for air revitalization applications has been of continued interest for many decades. They have the advantage of being regenerable sorbents with long lifetimes and a high acuteness for carbon dioxide. While their usage on Earth for flue gas and submarines has been explored for some time now, they are still being researched for use in microgravity environments. To succeed in a microgravity environment, such as usage on the International Space Station, an air revitalization system that is reliant on liquid amines as its sorbent must have a low Equivalent System Mass (ESM), among many other performance parameters. One way of optimizing this ESM number is through bringing down the systems power consumption with the use of microwave heating of the liquid sorbent. Microwave heating allows the liquid sorbent to be heated in a much more efficient way when compared to conventional types of heating techniques, such as convection or conduction. This paper will explore the physical mechanisms behind microwave heating, and how it could potentially be applied to a liquid amine carbon capture system, laying out any concerns and future constraints that a system designer may encounter.
Microwave heating has many potential lunar applications including sintering regolith for lunar surface stabilization and heating regolith for various oxygen production reactors. The microwave properties of lunar simulants must be understood so this technology can be applied to lunar operations. Dielectric properties at microwave frequencies for a common lunar simulant, JSC-1AC, were measured up to 1100 C, which is approximately the melting point. The experimentally determined dielectric properties included real and imaginary permittivity (epsilon', epsilon"), loss tangent (tan delta), and half-power depth, the di stance at which a material absorbs 50% of incident microwave energy. Measurements at 2.45 GHz revealed tan delta of JSC-1A increases from 0.02 at 25 C to 0.31 at 110 C. The corresponding half-power depth decreases from a peak of 286 mm at 110 C, to 13 mm at 1100 C. These data indicate that JSC-1AC becomes more absorbing, and thus a better microwave heater as temperature increases. A half-power depth maximum at 100-200 C presents a barrier to direct microwave heating at low temperatures. Microwave heating experiments confirm the sluggish heating effect of weak absorption below 200 C, and increasingly strong absorption above 200 C, leading to rapid heating and melting of JSC-1AC.
The objective is to develop a better understanding of the thermal shock properties of lunar regolith sintered using 2.45 GHz electromagnetic radiation and to do a preliminary study into the recovery of bound hydrogen in lunar soil heated using 2.45 GHz radiation. During the first phase of this work, lunar simulant material was used to test whether or not microhardness data could be used to infer thermal shock resistance and later actual lunar regolith was used. Results are included on the lunar regolith since this is of primary concern and not the simulant results. They were similar, however. The second phase investigated the recovery of hydrogen from lunar regolith and results indicate that microwave heating of lunar regolith may be a good method for recovery of bound gases in the regolith.
This slide presentation reviews the use of microwaves to heat lunar soil in order to obtain water. There appears to be large amounts of water in the lunar poles, in Martian areas in lower latitudes and some of the Moons of Jupiter. The presence of water in the south lunar polar region was demonstrated by the Lunar CRater Observation and Sensing Satellite (LCROSS) mission. Microwaves can be used to extract water from lunar soil without excavation. Using microwaves on a lunar soil simulant at least 95% of the water from the regolith permafrost simulant was extracted (2 minutes). The process is modeled using COMSOL Multiphysics Finite Element analysis microwave physics module and demonstrated usingan experiment of an microwave apparatus on a rover.
Microwave-assisted hydrogen generation from hydrocarbon-bearing reservoir rocks is strongly influenced by mineralogy, methane activation, carbonate reactions, and thermal runaway behavior. This study investigates a new approach in which carbonate phases are generated in-situ through the reaction of internally produced CO2 with Ca(OH)2 under microwave heating conditions. The objective is to evaluate how rock mineralogy, methane injection, and Ca(OH)2 addition influence hydrogen generation, carbon redistribution, and stage-dependent reaction pathways during microwave exposure. Microwave heating experiments were conducted using Permian Basin reservoir rocks under three experimental conditions: rock-only experiments under Ar atmosphere, CH4–Ar experiments without additive, and CH4–Ar experiments containing 5 wt% Ca(OH)2. Methane-assisted experiments were performed under continuous injection of 30 standard cubic centimeters per minute (sccm) CH4 and 30 sccm Ar. Based on thermal runaway behavior, each experiment was divided into three operational stages: Before Thermal Runaway (BR), After Thermal Runaway–Decrease in Microwave Power (ARD), and After Thermal Runaway– Increase in Microwave Power (ARI). Temperature and gas composition were continuously monitored throughout the experiments. The rock-only experiments demonstrated that hydrogen generation can occur intrinsically from hydrocarbon-bearing rocks under microwave heating, even without externally injected methane. However, hydrogen production did not correlate solely with kerogen content, indicating that mineralogy strongly influences hydrogen-generation pathways. Correlation analyses suggested that kerogen decomposition initially generated CH4, CO, and CO2, followed by secondary hydrocarbon reactions associated with H2 and C2 hydrocarbon formation. Methane-assisted experiments substantially increased hydrogen production; however, identical methane injection rates produced significantly different hydrogen yields among the rock samples, confirming that mineralogical composition controls methaneconversion behavior under microwave heating conditions. The addition of Ca(OH)2 significantly altered carbon evolution behavior in a stage-dependent manner. During the BR stage, Ca(OH)2 reduced gas-phase CO2 production, particularly in carbonate-rich rocks, indicating favorable conditions for in-situ carbonation and carbonate deposition prior to extensive thermal decomposition. The suppression of CO2 during BR became more pronounced with increasing carbonate content of the rock system. After thermal runaway, carbonate-containing systems exhibited enhanced hydrogen generation behavior, suggesting that carbonatederived mineral transformations and carbonate-mediated reactions contribute to high-temperature hydrogen-generation pathways. In carbonate-poor rocks, Ca(OH)2 addition enabled simultaneous URTeC 4493775 2 enhancement of hydrogen production and partial suppression of CO2 release during the post-runaway stages. Overall, the results demonstrate that microwave-assisted hydrogen generation is governed by dynamically evolving interactions among kerogen decomposition, methane activation, mineral transformations, carbonate formation/decomposition, and thermal runaway behavior. This work introduces in-situ carbonate engineering with Ca(OH)2 as a strategy for coupling hydrogen generation with partial insitu carbon management under microwave heating conditions.
Two processing techniques considered suitable for producing bricks from lunar regolith are examined: direct solar heating and microwave heating. An analysis was performed to compare the two processes in terms of the amount of power and time required to fabricate bricks of various sizes. Microwave heating was shown to be significantly faster than solar heating for rapid production of realistic-size bricks. However, the relative simplicity of the solar collector(s) used for the solar furnace compared to the equipment necessary for microwave generation may present an economic tradeoff.
The production of construction materials on the lunar surface will require an appropriate fabrication technique. Two processing methods considered as being suitable for producing dense, consolidated products such as bricks are direct solar heating and microwave heating. An analysis was performed to compare the two processes in terms of the amount of power and time required to fabricate bricks of various size. The regolith was considered to be a mare basalt with an overall density of 60 pct. of theoretical. Densification was assumed to take place by vitrification since this process requires moderate amounts of energy and time while still producing dense products. Microwave heating was shown to be significantly faster compared to solar furnace heating for rapid production of realistic-size bricks.
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. Here, this study addresses the challenge of premature pore closure in CVI processes through microwave heating. A frequency-domain microwave solver is developed in OpenFOAM 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 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.
The Material Plasma Exposure eXperiment (MPEX) at Oak Ridge National Laboratory is in the final design phase. MPEX will be capable of exposing neutron-irradiated materials to plasmas for the study of plasma-material interaction. This facility will provide information about the complex effects of plasmas on materials and contribute to examining new materials that can withstand high heat fluxes and high ion fluences for future fusion devices. MPEX plasma is heated by 70-GHz or 105-GHz electron Bernstein wave/electron cyclotron heating (ECH), and the high-frequency microwaves are prone to scattering microwave power, which can have detrimental effects, especially on diagnostic components. A large portion of the injected ECH power is expected to be absorbed by plasma, but the remainder requires that microwave absorbers be placed immediately upstream and downstream of the ECH launcher to minimize stray microwaves leaving the ECH region. These microwaves can inadvertently heat components that cannot be shielded or otherwise protected. The microwave absorber design is based on an array of pyramid-shaped ceramic tiles brazed to a water-cooled explosion-bonded heat sink and a stainless steel plate to produce one tile module. Computational fluid dynamics and structural analyses were performed to optimize and validate the design. Multiple test coupons were produced to validate the process for brazing the two different tile materials to the Glidcop AL-15 baseplate. The articles were tested to evaluate the reliability and thermal performance through exposure to an electron beam with a heat flux of up to 1.5 MW/m2. Nondestructive testing was performed before and after testing to identify voids or separations that may have been introduced by the high heat flux. This paper discusses the details of high heat flux microwave absorber design, manufacturing details and associated challenges, and test results, demonstrating the effectiveness of the proposed design.