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Microwave heating was used to join Silicon Carbide rods using a thin TiC /Si tape interlayer . Microwaves quickly heated the rods and tape to temperatures where solid-state displacement reactions between TiC and Si occurred.
A fire occurred in a CEM MARS 6 analytical microwave during microwave-assisted, acid digestion of a soil sample in a Research and Development (R&D) laboratory. The soil sample had been pretreated at 550°C for approximately 4 hours in a furnace prior to digesting in the microwave. Less than 1-gram aliquots of the pretreated soil sample were placed into separate microwave reaction vessels along with an acid mixture used for digestion. The microwave was used to facilitate digestion of the samples. Microwave reaction vessels were loaded with acid and soil samples, sealed in cassettes, and the cassettes placed onto a microwave carousel. A temperature probe that senses the reaction temperature during the run was inserted into the Reference Cell thermowell. The contents of the Reference Cell were identical to the contents of the other reaction cells. The researcher initiated the run and then left the laboratory to perform other work. Upon returning to check the digestion run, flames and smoke were observed originating from the microwave. The researcher exited the lab, immediate emergency actions were taken, and the local fire department responded and extinguished the fire. No personnel were injured, and no facility structural damage occurred. The affected microwave is a total loss. The fire investigation revealed the most credible cause of the fire is an incompatible temperature probe that did not accurately measure temperature of the liquid phase of the Reference sample.
For presentation at the 28th North American Catalysis Society Meeting in Providence, RI, June 18-23, 2023.
Microwave-assisted gasification is an energy-efficient alternative to conventional gasification in which known feedstocks can be converted into syngas, char, and other byproducts to produce clean hydrogen at lower temperatures (~550 °C) through selective heating. Fe oxides are well-known gasification catalysts that can reduce in-situ to activate the methyl radicals by supplying surface oxygen and promoting H2 formation. This study introduces Fe2O3 as a microwave-active catalyst to enhance H2 production and tar reduction for plastic-corn stover co-gasification. The results found that the microwave reaction at 800 °C produced 24 times more mmol of hydrogen per kWh energy as compared to the conventional run at 900 °C. The X-ray diffraction results show the presence of Fe3O4 and FeO peaks indicating reduction of Fe2O3 to help devolatize reaction intermediates; while the appearance of metallic Fe in the microwave run at 800 °C indicates that Fe2O3 achieves full reduction at the microwave gasification temperature yielding maximum hydrogen production.
The conversion of carbon dioxide into higher value chemicals is a viable way to support sustainability and net-zero economy goals. Of the different CO2 conversion routes, direct conversion offers a simplified process, lower reaction temperatures, and thus low energy input. Alcohols can be directly combined with CO2 to produce polycarbonates, e.g., DMC (dimethyl carbonate) formation from methanol and CO2. Recently CO2 and 1,6-hexanediol were shown to convert into poly(hexamethylene carbonate)diol using an atmospheric flow based process in single step. For these conversions, CeO2-based catalysts are widely used due to the abundance of oxygen vacancies that are believed to be the active sites for this reaction. Microwave (MW) heating is a unique approach that can provide selective volume-based heating and enhanced reaction rates and/or selectivities. For the current work, CO2 and diol conversion into polymers were investigated on different CeO2 catalysts under microwave heating and the performance was compared against conventional heating. The reaction products were analyzed using infrared spectroscopy (IR) and nuclear magnetic resonance (NMR) spectroscopy. Preliminary results showed microwaves irradiation produced faster rates of polycarbonate production as evidenced by IR data.
Deterioration of concrete due to the alkali–silica reaction (ASR) involves a reaction between alkaline ions in the cement pore solution and non-crystalline silica found in many aggregates. The product of reaction is a porous hydrophilic ASR gel, which causes expansion and cracking of concrete structure. Currently, there is no reliable method for non-destructive evaluation of ASR. We have investigated the feasibility of using relative dielectric permittivity obtained from X-band microwave backscattering of concrete. Advantages of this method of concrete evaluation are that measurements are non-contact and one-sided, and the approach is scalable to arbitrary-size concrete structures. The exploratory study was performed using an unrestrained set of accelerated ASR concrete prism specimens developed according to the ASTM1293 standard. One set of specimens contained no entrained air, while another set was contained entrained air. The specimens were removed from the environmental chamber at different times during a year-long study to create a set of different ASR maturity specimens. Strain measurements were performed on all specimens. Strain data both air entrained and non-air entrained sets were shown to be in close agreement with Larive model of isothermal unrestrained ASR expansion with similar fitting parameters. Furthermore, relative dielectric permittivity of concrete specimens was correlated with strain data. Both sets show correlation between dielectric permittivity and strain, with stronger linear correlation observed for the air-entrained specimens. Development of such correlation would enable estimating expansion of actual concrete structures from microwave backscattering measurements, which could be used for risk stratification to guide and minimize coring.
This paper presents an innovative approach to producing energy-dense, carbon–neutral liquid ammonia as a means for carrying energy. This approach synergistically integrates microwave reaction chemistry with novel heterogeneous catalysis that decouples dinitrogen activation from high-temperature and high-pressure reactions, altering reaction pathways and increasing ammonia formation rate. Results presented here demonstrate that ammonia synthesis can be conducted at 280 ? and ambient pressure to achieve ~1 mmol ammonia/g cat/h over supported ruthenium catalyst systems utilizing microwave irradiation. It is further shown that adding promoter ions such as potassium, cerium, and barium significantly improves the ammonia production rate over undoped ruthenium-based catalysts. This effect could be attributed to enhanced dielectric loss processes that lead to stronger microwave absorption by the catalyst. Measurement of the equilibrium constant under microwave conditions showed a higher ammonia yield than under thermal equilibrium conditions for both the iron- and ruthenium-based catalysts. Finally, this study also illustrates the advantages of using a variable-frequency microwave reactor for ambient-pressure ammonia synthesis. Mechanistically, investigators believed that the oscillating electric fields of the radiation can couple with adsorbed nitrogen on the surface and accelerate its dissociation. Since dinitrogen dissociation on the surface is rate limiting, this effectively accelerates the reaction.
Lunar simulant material was fabricated to simulate Apollo 11, Apollo 15, and Apollo 16 soils. The approximate compositions which these soils simulate are given. Samples of each soil simulate were fabricated into right circular cylinders, placed into a microwave reaction cavity, and heated using 2.45 GHz radiation to a particular processing temperature at which it was held for a prescribed length of time. Examples are given of two microwave heating programs for these simulant samples. Upon completion of thermal processing, each sample had its top and bottom surfaces polished. A technique was employed which looks at hardness data to determine the fracture toughness of a material and then relates this to thermal shock resistance. Some advantages of this technique are its low cost for analysis and thermal shock resistance as a function of initial sample orientation in the microwave field can be determined. Samples were prepared for testing and results are expected. At the same time, other samples are currently being investigated using scanning electron microscopy to determine their microstructures.
This document summarizes NETL's microwave catalysis work.
A spectroscopic study is presented of the matrix-isolated products of the direct combination reaction of chlorine atoms with ozone and of the microwave discharge reaction of chlorine and oxygen. Infrared spectra in the wavenumber range 2000 to 200 per cm were recorded for reaction products trapped by the condensation of a matrix of solid argon. Evidence for the formation of the ClO radical as well as the ClOO and ClClO radicals during the direct chlorine-ozone reaction is obtained, however no evidence is found for the presence of asymmetric ClO3 under conditions thought favorable for its formation. The ClO molecule is also observed following the microwave discharge reaction of chlorine and oxygen in argon in the isotopic forms (Cl-35)(O-16), (Cl-37)(O-16), (Cl-35)(O-18), and (Cl-37)(O-18). It is noted that the vibrational frequency for the (Cl-35)(O-16) radical at 849.2 per cm is blue-shifted 5 per cm above its gas-phase fundamental.
A keynote presentation delivered at 26th Canadian Catalysis Symposium virtually on microwave work at NETL.
In chemical reactions, the breaking and formation of chemical bonds usually need external energy to overcome the activation barriers. Conventional energy delivery transfers energy from heating sources via various media, hence losing efficiency and inducing side reactions. In contrast, microwave (MW) heating is known to be highly energy efficient through dipole interaction with polar media, but how exactly it transmits energy to initiate chemical reactions has been unknown. Here, we report a rigorous determination of energy delivery mechanisms underlying MW-enabled rapid hydrothermal synthesis, by monitoring the structure and temperature of all the involved components as solid-liquid intercalation reaction occurs using in situ synchrotron techniques. We reveal a hitherto unknown direct energy transmission between MW irradiation source and the targeted reactants, leading to greatly reduced energy waste, and so the ultrafast kinetics at low temperature. These findings open up new horizons for designing material synthesis reactions of high efficiency and precision.
The state-of-the-art Carbon Dioxide Reduction Assembly (CRA) was delivered to the International Space Station (ISS) in April 2010. The system is designed to accept carbon dioxide from the Carbon Dioxide Removal Assembly and hydrogen from the Oxygen Generation Assembly. The two gases are reacted in the CRA in a Sabatier reactor to produce water and methane. Venting of methane results in an oxygen resupply requirement of about 378 lbs per crew member per year. If the oxygen is supplied as water, the total weight for resupply is about 476 lb per crew member per year. For long-term missions beyond low Earth orbit, during which resupply capabilities will be further limited, recovery of hydrogen from methane is highly desirable. For this purpose, NASA is pursuing development of a Plasma Pyrolysis Assembly (PPA) capable of recovering hydrogen from methane. Under certain conditions, water vapor and carbon dioxide (nominally intended to be separated from the CRA outlet stream) may be present in the PPA feed stream. Thus, testing was conducted in 2010 to determine the effect of these "oxygenated" compounds on PPA performance, particularly the effect of inlet carbon dioxide and water variations on the PPA product stream. This paper discusses the test set-up, analysis, and results of this testing
The state-of-the-art Carbon Dioxide Reduction Assembly (CRA) was delivered to the International Space Station (ISS) in April 2010. The system is designed to accept carbon dioxide from the Carbon Dioxide Removal Assembly and hydrogen from the Oxygen Generation Assembly. The two gases are reacted in the CRA in a Sabatier reactor to produce water and methane. Venting of methane results in an oxygen resupply requirement of about 378 lbs per crew member per year. If the oxygen is supplied as water, the total weight for resupply is about 476 lb per crew member per year. For long-term missions beyond low Earth orbit, during which resupply capabilities will be further limited, recovery of hydrogen from methane is highly desirable. For this purpose, NASA is pursuing development of a Plasma Pyrolysis Assembly (PPA) capable of recovering hydrogen from methane. Under certain conditions, water vapor and carbon dioxide (nominally intended to be separated from the CRA outlet stream) may be present in the PPA feed stream. Thus, testing was conducted in 2010 to determine the effect of these oxygenated compounds on PPA performance, particularly the effect of inlet carbon dioxide and water variations on the PPA product stream. This paper discusses the test set-up, analysis, and results of this testing.
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.
A microwave-assisted HNO3-H2SO4-HF digestion system was explored/optimized for the total dissolution of Boron Carbide samples followed by multi-elemental determination using ICP-MS and ICP OES, in order to improve the methods used in a previous try using a microwave-assisted H2O2-HNO3-HF digestion system. The samples were microwave digested to accomplish complete dissolution needed to perform quantitative analysis of their metal content. Two Boron Carbide samples were provided to us: JM10 and JM11. The Boron Carbide samples were completely dissolved at the end of the optimized microwave digestion procedure that was developed. The digested samples were analyzed for metals mostly by ICP MS; few elements were analyzed by ICP-OES. Microwave digestion reactions were performed in a Titan MPS instrument (Perkin Elmer, USA). Titan MPS instrument is equipped with Temperature and Pressure regulations and controlled by software. Each microwave digestion batch contained the samples of interest along with a reagent blank and one certified standard (1632e) in order to (i) compensate for the contaminations present in the reagents, (ii) ensure that the digestion was complete and (iii) that there was a good recovery of all the constituents. The certified standard used (1632e) was provided with USGS certificates of analysis.
The use of microwave irradiation for the synthesis of inorganic nanomaterials has recently become a widespread area of research that continues to expand in scope and specialization. The growing demand for nanoscale materials with composition and morphology tailored to specific applications requires the development of facile, repeatable, and scalable synthetic routes that offer a high degree of control over the reaction environment. Microwave irradiation provides unique advantages for developing such routes through its direct interaction with active reaction species, which promotes homogeneous heat distribution, increased reaction rates, greater product quality and yield, and use of mild reaction conditions. Many catalytic nanomaterials such as noble metal nanoparticles and intricate nanocomposites have very limited synthetic routes due to their extreme temperature sensitivity and difficulty achieving homogeneous growth. This work presents recent advances in the use of MW irradiation methods to produce high-quality nanoscale composites with controlled size, morphology, and architecture.
Gasification of waste feedstock such as biomass, waste plastics suffers from high tar yields during hydrogen-rich syngas production. The presence of tars result in lower quality syngas, lower syngas yields, reactor blockage, reactor down time, and costly maintenance. Therefore, removal of tar from syngas during gasification is essential. Catalytic reforming of tars via in-situ syngas cleanup is an effective way of mitigating tars. This work explores the possibility of microwave-assisted catalytic dry reforming of tars for syngas production. Further, due to its chemical complexity, toluene, which is one of the main tar constituents, could be used as a model tar compound. Toluene dry reforming was studied using the Fe/Al 2 O 3 catalyst under CO 2 under the temperature range of 400–700 °C. The toluene reforming reaction was conducted using microwave and conventional thermal reactors. Under microwave irradiation, CO 2 and toluene conversions are boosted to 80% at 500 °C. Hydrogen and carbon monoxide yields were approximately five times and ten times higher in the microwave reactor at 500 °C, respectively, compared to the productions obtained in the conventional fixed-bed reactor at 700 °C. Filamentous carbon was also produced as a valuable side product to improve the economy of this process and such value-added carbon was only observed in the microwave reactor. Three reaction pathways were observed during microwave reaction: the toluene decomposition produces an initial hydrogen and carbon deposit on the catalyst; the formation of methane and benzene suggests toluene hydrodemethylation as a secondary reaction; and toluene hydrogenolysis forms light alkanes such as methane, and through reforming reaction under CO 2 to syngas.