In this study, real-time and in-situ permittivity measurements under intense microwave electromagnetic fields are proposed as a powerful technique for the study of microwave-enhanced thermal ...processes in materials. In order to draw reliable conclusions about the temperatures at which transformations occur, we address how to accurately measure the bulk temperature of the samples under microwave irradiation. A new temperature calibration method merging data from four independent techniques is developed to obtain the bulk temperature as a function of the surface temperature in thermal processes under microwave conditions. Additionally, other analysis techniques such as Differential Thermal Analysis (DTA) or Raman spectroscopy are correlated to dielectric permittivity measurements and the temperatures of thermal transitions observed using each technique are compared. Our findings reveal that the combination of all these procedures could help prove the existence of specific non-thermal microwave effects in a scientifically meaningful way.
A microwave cavity and heating system for microwave processing and in situ dynamic measurements of the complex permittivity of dielectric materials at high temperatures ( ~ 1000 ° C) has been ...developed. The method is based on a dual-mode cylindrical cavity where heating and testing are performed by two different swept frequency microwave sources. A cross-coupling filter isolates the signals coming from both sources. By adjusting the frequency bandwidth of the heating source and the level of coupling to the cavity, an automatic procedure allows for the establishment of a desirable level of heating rate to the dielectric sample to reach high temperatures in short cycles. Dielectric properties of materials as a function of temperature are calculated by an improved cavity perturbation method during heating. Accuracy of complex permittivity results has been evaluated and an error lower than 5% with respect to a rigorous analysis of the cavity has been achieved. The functionality of the microwave dielectric measurement system has been demonstrated by heating and measuring glass and ceramic samples up to 1000 ° C. The correlation of the complex permittivity with the heating rate, temperature, absorbed power, and other processing parameters can help to better understand the interactions that take place during microwave heating of materials at high temperatures compared to conventional heating.
Abstract
Microwaves (MWs) are an emerging technology for intensified and electrified chemical manufacturing. MW heating is intimately linked to a material’s dielectric permittivity. These properties ...are highly dependent on temperature and pressure, but such datasets are not readily available due to the limited accessibility of the current methodologies to process-oriented laboratories. We introduce a simple, benchtop approach for producing these datasets near the 2.45 GHz industrial, medical, and scientific (ISM) frequency for liquid samples. By building upon a previously-demonstrated bireentrant microwave measurement cavity, we introduce larger pressure- and temperature-capable vials to deduce temperature-dependent permittivity quickly and accurately for vapor pressures up to 7 bar. Our methodology is validated using literature data, demonstrating broad applicability for materials with dielectric constant ε' ranging from 1 to 100. We provide new permittivity data for water, organic solvents, and hydrochloric acid solutions. Finally, we provide simple fits to our data for easy use.
Commercially, 3 mol% Y2O3‐stabilized tetragonal zirconia (70–90 nm) compacts were fabricated using a conventional and a nonconventional sintering technique; microwave heating in a resonant mono‐mode ...cavity at 2.45 GHz, at temperatures in the 1100–1400°C range. A considerable difference in the densification behavior between conventional (CS) and microwave (MW) sintered materials was observed. The MW materials attain a full density of 99.9% of the theoretical density (t.d.) at 1400°C/10 min, whereas the CS reach only 98.0% t.d. at the same temperature and 1 h of dwelling time. Therefore, the MW materials exhibit superior Vickers hardness values (16.0 GPa) when compared with CS (13.4 GPa).
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•Electromagnetic, heat transfer and fluid dynamics coupled for MW heating simulation.•Dielectric properties of NaY zeolite measured as a function of temperature 298–623 K.•Temperature ...evolution and distribution results validated with experimental data.•Model predicts thermal runaway of zeolite under MW heating.
Three-dimensional mathematical model was developed for a rectangular TE10n microwave heating cavity system, working at 2.45 GHz. Energy/heat, momentum equations were solved together with Maxwell’s electromagnetic field equations using Comsol Multiphysics® simulation environment. The dielectric properties, ε' and ε'', of NaY zeolite (Si/Al = 2.5) were evaluated as a function of temperature. Considering these values, the microwave heating of a porous fixed-bed made of dry NaY zeolite was simulated. Electric field distribution, axial and radial temperature profiles and temperature evolution with time were obtained. The zeolite fixed bed was heated up to 180 °C in 5 min, with 30 W power. The fixed-bed temperature evolution under non-steady state conditions showed the same trend as the one observed experimentally with only an average deviation of 10.3%. The model was used to predict microwave heating of other materials improving energy efficiency of the microwave cavity. Furthermore, the developed model was able to predict thermal runaway for zeolites.
Optical measurements from high‐speed, high‐definition video recordings can be used to define the full‐field dynamics of a structure. By comparing the dynamic responses resulting from both damaged and ...undamaged elements, structural health monitoring can be carried out, similarly as with mounted transducers. Unlike the physical sensors, which provide point‐wise measurements and a limited number of output channels, high‐quality video recording allows very spatially dense information. Moreover, video acquisition is a noncontact technique. This guarantees that any anomaly in the dynamic behaviour can be more easily correlated to damage and not to added mass or stiffness due to the installed sensors.
However, in real‐life scenarios, the vibrations due to environmental input are often so small that they are indistinguishable from measurement noise if conventional image‐based techniques are applied. In order to improve the signal‐to‐noise ratio in low‐amplitude measurements, phase‐based motion magnification has been recently proposed.
This study intends to show that model‐based structural health monitoring can be performed on modal data and time histories processed with phase‐based motion magnification, whereas unamplified vibrations would be too small for being successfully exploited. All the experiments were performed on a multidamaged box beam with different damage sizes and angles.
The application of microwave technology for efficient and environmentally friendly synthesis of ceramic pigments is a successful and rapidly evolving area of research. However, a clear understanding ...of the reactions and their relationship with the material absorbance has not been fully achieved. The present study introduces an in situ permittivity characterization technique, which serves as an innovative and precise tool for assessing the microwave synthesis of ceramic pigments. Several processing parameters (atmosphere, the heating rate, raw mixture composition and particle size) were evaluated by studying the permittivity curves as a function of temperature to elucidate their effect on the synthesis temperature and the final pigment quality. The validity of the proposed approach was verified through correlation with other well-known analysis techniques, such as DSC or XRD, providing valuable information about the reaction mechanisms and the optimum conditions for the synthesis process. In particular, changes in permittivity curves were linked, for the first time, to undesired metal oxide reduction at too-high heating rates and could be used to detect pigment synthesis failures and ensure product quality. The proposed dielectric analysis was also found to be a useful tool for optimizing raw material composition for the microwave process, including the use of chromium with lower specific surface area and flux removal.
The identification of the minerals composing rocks and their dielectric characterization is essential for the utilization of microwave energy in the rock industry. This paper describes the use of a ...near-field scanning microwave microscope with enhanced sensitivity for non-invasive measurements of permittivity maps of rock specimens at the micrometer scale in non-contact mode. The microwave system comprises a near-field probe, an in-house single-port vectorial reflectometer, and all circuitry and software needed to make a stand-alone, portable instrument. The relationship between the resonance parameters of the near-field probe and the dielectric properties of materials was determined by a combination of classical cavity perturbation theory and an image charge model. The accuracy of this approach was validated by a comparison study with reference materials. The device was employed to determine the permittivity maps of a couple of igneous rock specimens with low-loss and high-loss minerals. The dielectric results were correlated with the minerals comprising the samples and compared with the dielectric results reported in the literature, with excellent agreements.
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