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.

The surface of ordered mesoporous (MCM‐48) silica has been subjected to covalent grafting with silane molecules containing one to three amino groups. The dielectric properties of the materials were studied in detail, and the functionalized materials were used for CO₂ adsorption at room temperature, followed by regeneration under either conventional heating or microwave irradiation. It has been found that, as the intensity of functionalization with amino groups increases (from mono‐ to tri‐amino silanes) both the CO₂ load and the dielectric response at microwave frequencies increase. In particular, functionalization with a tri‐amino silane derivative gave the highest CO₂ adsorption and the fastest microwave heating, resulting in a fourfold acceleration of adsorbent regeneration. The grafted material was fully stable for at least 20 adsorption‐regeneration cycles, making it an ideal candidate for microwave‐swing adsorption (MWSA) processes. © 2015 American Institute of Chemical Engineers AIChE J, 62: 547–555, 2016

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.

This paper reports the development of a stand-alone and portable instrument designed to measure the complex permittivity of dielectric materials at microwave frequencies. The equipment consists of an in-house single-port vectorial reflectometer and a resonant coaxial bi-reentrant microwave cavity where the material under test is placed inside a Pyrex vial, making the device appropriate for measuring liquids, semi-solids, powders and granular materials. The relation between the dielectric properties of the involved materials and the cavity resonance has been solved by numerical methods based on mode-matching and circuit analysis. In order to increase the measurement range, so that low to high loss materials can be characterized in the same cavity, the effect of the coupling network is de-embedded from the resonance measurements. The performance of the newly devised instrument is evaluated by error/uncertainty analysis and comparative studies with other well-established instruments and methods. Errors lower than 2% in the dielectric constant, and 5% in the loss factor, are found. This simple, portable, affordable and robust device could help non-specialized personnel to accurately measure dielectric properties of materials used in a wide range of microwave applications.

Microwave-assisted processes have recognized advantages over more conventional heating techniques. However, the effects on the materials’ microstructure are still a matter of study, due to the complexity of the interaction between microwaves and matter, especially at high temperatures. Recently developed advanced microwave instrumentation allows the study of high temperature microwave heating processes in a way that was not possible before. In this paper, different materials and thermal processes induced by microwaves have been studied through the in situ characterization of their dielectric properties with temperature. This knowledge is crucial in several aspects: to analyze the effects of the microwave field on the reaction pathways; to design and optimize microwave-assisted processes, and to predict the behavior of materials leading to repeatable and reliable heating processes, etc.