A perfluorinated ionic liquid, 1-(perfluorohexyl)-3-methylimidazolium iodide, was synthesized via microwave reaction and compared to a non-fluorinated analog. Typically, the synthesis of fluorinated ionic liquids involves long reaction times and multiple steps. We have demonstrated a shortened synthesis and a more straightforward procedure, by using a microwave reactor for the microwave-assisted synthesis of 1-(perfluorohexyl)-3-methylimidazolium iodide. The addition of fluorinated alkyl chains on imidazolium ionic liquid cations increases the molecular free volume of the ionic liquid which is beneficial for increasing CO2 physisorption. Computational and experimental data shows an increased CO2 solubility and capacity for fluorinated ionic liquids. The perfluoroalkyl functionalized ionic liquid is characterized using 1H and 19F NMR spectroscopy, FTIR spectroscopy, and DSC. By DSC, a crystallization onset is near -31 °C and while the onset of the melting point between -30 and -17 °C.

Using ethanol adsorption calorimetry, the surface energetics of two carbon substrates and two products in microwave-assisted carbon nanotube (CNT) growth was studied. In this study, the ethanol adsorption enthalpies of the two graphene-based samples at 25 °C were measured successfully. Specifically, the near-zero differential enthalpies of ethanol adsorption are −75.7 kJ/mol for graphene and −63.4 kJ/mol for CNT-grafted graphene. Subsequently, the differential enthalpy curve of each sample becomes less exothermic until reaching a plateau, −55.8 kJ/mol for graphene and −49.7 kJ/mol for CNT-grafted graphene, suggesting favorable adsorbate–adsorbent binding. Moreover, the authors interpreted and discussed the partial molar entropy and chemical potential of adsorption as the ethanol surface coverage (loading) increases. Due to the low surface areas of carbon black–based samples, adsorption calorimetry could not be performed. This model study demonstrates that using adsorption calorimetry as a fundamental tool and ethanol as the molecular probe, the overall surface energetics of high–surface area carbon materials can be estimated.

Ultra-rapid microwave sintering of ceramics has been recently demonstrated by the authors. In the experiments with oxide ceramic samples carried out in a 24 GHz gyrotron system for microwave processing of materials, full density was achieved in the sintering processes with a duration of the high-temperature stage of one to several minutes and zero hold at the maximum temperature. The implementation of the ultra-rapid microwave sintering processes was made possible due to fast and efficient control over the temperature of the materials and the supplied microwave power. The absorbed microwave power density was typically in the range of 10–100 W/cm3, which is within the same order of magnitude as the power of Joule heat in the DC electric field–assisted flash sintering processes. At this power level, a thermal instability is triggered by the volumetric heating, which results in a drastic enhancement of mass transport. In addition, possibility of ultra-rapid microwave sintering of powder metals has been demonstrated within a model accounting for the effective electromagnetic properties and resonant absorption effects.

This study reports the fabrication of high mass loading (32 mg/cm2) electrodes of niobium pentoxide (Nb2O5) nanoparticles and carbon nanotubes (CNTs) using a facile procedure. The as-obtained Nb2O5 nanoparticles by microwave-assisted hydrothermal synthesis presented pseudohexagonal (TT) phase, and when exposed to the thermal treatment, the Nb2O5 nanoparticles changed to orthorhombic (T) phase. Distinct morphologies were obtained, which exhibited a specific surface area of 216 m2/g and 47 m2/g to pseudohexagonal and orthorhombic phases, respectively. Cyclic voltammetry and electrochemical impedance spectroscopy techniques were performed in a three-electrode system using 1 M Li2SO4 as electrolyte with a potential window of 0–0.9 V (versus standard calomel electrode). Both materials showed capacitive behavior with a specific capacitance of 0.11 F/cm2 and 0.09 F/cm2 to nanocomposites CNT + TT-Nb2O5 and CNT + T-Nb2O5 at 2 mV/s, respectively. Thus, an efficient, simple, and promising process to produce electrodes for supercapacitors was demonstrated.

The application of microwave radiation (MWR) during materials synthesis can generate a wide range of interesting phenomena, such as rapid, low-temperature phase transitions and the formation of nonequilibrium phases. However, the underlying mechanisms by which MWR can influence processes like nucleation, crystallization, sintering, and grain growth remain unknown. A critical need for studying these mechanisms is the ability to quantitatively characterize the effects of MWR exposure on atomic structure. In this regard, synchrotron X-ray sources provide an opportunity to shed new light on electromagnetic (EM) field–assisted synthesis due to the availability of high-energy X-rays that enable a wide range of experimental characterization techniques. Here, we review the use of synchrotron X-ray sources for both ex situ and in situ studies of MWR-assisted synthesis. While many synchrotron-based tools are available to characterize the structural effects of MWR from the micron down to the atomic scale, work in this field is ongoing, and no clear consensus exists regarding the underlying mechanisms of EM field–mediated phase transitions. We discuss the instrumentation available to study field–matter interaction mechanisms and identify future needs in synchrotron characterization to better understand how EM fields can engineer advanced materials.

Pt/Ce1-xRuxO2 and Ir/Ce1-xRuxO2 catalysts were prepared through the sol-gel technique, under microwave heating. In a first step, the Ce1-xRuxO2 solid solutions were prepared. Subsequently, an incipient wet impregnation process was carried out to homogeneously achieve the dispersion, either of platinum or iridium nanoparticles. The Pt/Ce1-xRuxO2 and Ir/Ce1-xRuxO2 catalysts were characterized by means of SEM, XRD, XPS, TEM, and specific surface area measurements. Crystal size and shifting into the CeO2 structure were detected after ruthenium doping producing the Ce1-xRuxO2 solid-solutions. Trough XPS technique Pt and Ir nanoparticles were found evenly dispersed in a metallic state. Those features allow us to foresee that, in the near future, these materials could be used efficiently as catalysts for oxidation process.

We examined the influence of the microwave power on the diagonal resistance in the GaAs/AlGaAs two dimensional electron system (2DES), in order to extract the electron temperature and determine microwave induced heating as a function of the microwave power. The study shows that microwaves produce a small discernable increase in the electron temperature both at null magnetic field and at finite magnetic fields in the GaAs/AlGaAs 2DES. The heating effect at null field appears greater in comparison to the examined finite field interval, although the increase in the electron temperature in the zero-field limit appears smaller than theoretical predictions.

This work presents the synthesis of selenium-based nanoparticles via microwave-assisted heating and their subsequent characterization using UV-vis Spectroscopy (UV-Vis), high-resolution transmission electron microscopy (HRTEM), and energy-dispersive X-ray spectroscopy (EDX), techniques. Ongoing research includes the study of the nanoparticles capacity to generate reactive oxygen species (ROS).

Herein, we report N, S co-doped carbon dots (NS CDs) as stabilizing and reducing agents for the synthesis of N, S doped carbon dots-Au nanocomposites (NS CDs-Au NCs) through the solution method and explore the catalytic property of the synthesized nanocomposites in the reduction of nitro aromatic compounds (NACs) such as 4-nitrophenol (4-NP), 4-nitroaniline (4-NA), and nitrobenzene (NB). The appraisal of the catalytic efficacy of the NS CDs-Au NCs was premised on real time monitoring of the reduction of NACs using UV-Visible absorption spectroscopy. The apparent rate constants (kapp) of reduction were found to follow the pseudo-first-order kinetics having values of 1.37 × 10−1, 8.9 × 10−2, and 5.35 × 10−2 s−1 for 4-NP, 4-NA, and NB, respectively. The apparent rate constant (1.37 × 10−1 s−1) observed for the reduction of 4-NP by NaBH4 using NS CDs-Au NCs has been found to be one of the highest values reported in the literature so far thereby validating their excellent efficacy as a catalyst.

A kaolin clay was activated with 1.0 M H2SO4 solution at minimum liquid to solid ratio (L/S) using microwave heating. The optimum experimental conditions for activation were L/S ratio 3.0 mL 1 M H2SO4 per gram kaolin, microwave input power 500–600 W, and heating time 5–10 min. Activation at L/S < 3.0 mL/g using 1.0 M H2SO4 was not efficient, indicating the influence of solvent for absorbing microwaves more intensively and thus improving activation. Significant physicochemical changes were observed by the proposed procedure with smaller volumes of activator compared to the conventional heating method. Microwave input power and heating time have a strong influence on the quality of the final material; activation at high input power (>700 W) and longer heating times (>10 min.) are not recommended since they cause dissolution of kaolinite structure. Microwave-heated kaolin manifested better adsorption for tartrazine dye due to improvements in textural and chemical properties of kaolinite. Moreover, irradiation of used kaolinite has significantly improved dye desorption, increasing the importance of microwaves in regeneration/recycling studies. Detailed dielectric measurements of kaolin-acid mixtures recorded at frequencies much lower than 2.45 GHz revealed that absorption of radiation is highly dependent on the activator solution in the mixture. For 3.0 mL/g mixtures, high dielectric constant ε’ 5223, dielectric loss factor ε” 5083, tangent loss tan d 1.30, penetration depth dp 0.57 cm at (103 Hz), and AC-conductivity σ 0.032 Om–1 were determined at 105 Hz. Filling the pores of kaolin by acid solution increased the microwave absorption and hence de-alumination of kaolinite.

Successful invasive plant eradication is rare, because the methods used target the adult stage, not taking into account the development capacity of a large seedbank. Heating by microwave was considered, because it offers a means to quickly reach the temperature required for loss of seed viability and inhibition of germination. Previous results were not encouraging, because homogeneous and deep-wave penetration was not achieved, and the various parameters that can affect treatment effectiveness were incompletely addressed. This study aimed to determine, under experimental conditions, the best microwave treatment to inhibit invasive species seed germination in terms of power (2, 4, 6 kW) and duration (2, 4, 8 min) of treatments and depending on soil moisture (10%, 13%, 20%, 30%) and seed burial depth (2, 12 cm). Three invasive species were tested: Bohemian knotweed, giant goldenrod, and jimsonweed. The most effective treatments required relatively high power and duration (2kW8min, 4kW4min, 6kW2min, and 6kW4min; 4kW8min and 6kW8min were not tested for technical reasons), and their effectiveness diminished with increasing soil moisture with germination percentage between 0% and 2% for the lowest soil moisture, 0% and 56% for intermediate soil moisture, and 27% and 68% in control treatments. For the highest soil moisture, only 2kW8min and 4kW4min reduced germination percentage between 2% and 19%. Occasionally, germination of seeds located at the 12-cm depth was more strongly affected. Giant goldenrod seeds were the most sensitive, probably due to their small size. Results are promising and justify further experiments before developing a field microwave device to treat large volumes of soil infested by invasive seed efficiently and with reasonable energy requirements. Other types of soil, in terms of texture and organic matter content, should be tested in future experiments, because these factors influence soil water content and, consequently, microwave heating.

A new rapid and energy saving method for the obtention of high performance nanoparticles and thin films of Nb2O5 by microwave-assisted hydrothermal synthesis is reported. The hydrothermal treatment of a sol–gel precursor solution in a microwave oven at 180 °C for 20 min was enough to obtain amorphous nanoparticles with average sizes of 40 nm. The calcination promotes the formation of different phases of Nb2O5 (TT and T) with pseudohexagonal and orthorhombic structure, respectively, that transform at higher temperatures in a mixture of orthorhombic and monoclinic phases. Crystalline phase composition was found to have a significant influence on the photocatalytic activity. The best photocatalytic performance was observed for the material mainly constituted by the TT-Nb2O5 phase. Thin films constituted by the TT phase were prepared by dip-coating. Photocatalytic experiments confirmed the high photocatalytic activity of this material, which showed a kinetic curve similar to that of a reference TiO2-P25 thin film.

This paper, for the first time, reports the results of microwave sintering of two emerging biomaterials, magnesium phosphate and amorphous magnesium calcium phosphate. Beneficial aspects of successful microwave sintering of calcium phosphate are well documented in the literature. The motivation for this work derives from the absence of any publication of similar nature on magnesium phosphates, which are becoming important with the rapid rise in interest in biodegradable Mg-alloys. Starting off with amorphous calcium magnesium phosphate and magnesium phosphate, the resulting microwave sintered product is a biphasic mixture of whitlockite substituted with magnesium and magnesium phosphate. The influence of the extent of Mg substitution on the mechanical properties, microstructure, and sintering behavior of tricalcium phosphate was evaluated. The results showed that the addition of Mg (up to the 50% wt/wt in relation to Ca mass) in the precursor compound of magnesium calcium phosphate improved the kinetics of the densification process and enhanced hardness values.

In this work, 3 simple, fast, labour and energy efficient methodologies were used to prepare carbon quantum dots (C-dots) using a red beetroot (Beta vulgaris subsp. vulgaris var. vulgaris) aqueous extract as the carbon source: alkali-assisted (AA), microwave-assisted (MA) and alkali-microwave-assisted (AMA) synthesis. TEM images shows nanoparticles with a nearly spherical morphology and diameters around 7.0 nm. FTIR spectra show characteristic peaks of C-H, C-O, O-H and C=C bonds for all the samples. The emission spectra show an interesting feature of the as-prepared samples: the emission band position can be tunable by changing the excitation wavelength. Comparing the 3 different methodologies in terms of photoluminescence properties, the one based only on the microwave-assisted heating has showed the most improved emission.

Microwave sintering is a novel and efficient technology for the rapid preparation of metallic materials. In this paper, an investigation has been performed on the distribution of microwave electromagnetic fields in a metallic particle system and its influence on sintering behavior. The results show that the microstructure of the “metallic-void” will induce a nonuniform distribution and focusing effect of electromagnetic fields during microwave processing, which may accelerate the sintering process. However, further study shows that the focusing effect will decline as the neck grows larger, and will also decline from outside to inside within the loosely packed powder system, which will result in the slowdown of the sintering rate. These results were supported by the synchrotron radiation computed tomography experimental observation of the microstructure evolution of metallic powders during an entire uninterrupted microwave sintering process.

Rare earth (e.g., Eu, Er, Yb, Tm) doped Y2O3 nanocrystals are promising fluorescent bioimaging agents which can overcome well known problems of currently used organic dyes like photobleaching, phototoxicity, and light scattering. Furthermore, the alternative quantum dots (QDs) composed of heavy metals (e.g., CdSe) possess inherently low biocompatibility due to the heavy metal content. In the present work, monodisperse spherical Y2O3:Eu3+ nanocrystals were successfully synthesized by microwave assisted urea precipitation method followed by thermochemical treatment. This is a green, fast and reproducible synthesis method, which is surfactant and hazardous precursors free. The as prepared particles were non-aggregated, spherical particles with a narrow size distribution. The calcined particles have a polycrystalline structure preserving the monodispersity and the spherical morphology of the as prepared particles. After calcination of Y(OH)CO3:Eu3+ precursors at 900°C for 2 hours, a highly crystalline cubic Y2O3 structure was obtained. The Y2O3:Eu3+ spherical particles showed a strong red emission peak at 613nm due to the 5D0–7F2 forced electric dipole transition of Eu3+ ions under UV excitation (235 nm) as revealed by the photoluminescence analysis (PL). The effect of reaction time on size and photoluminescence properties of calcined particles and also the effect of reaction temperature and pressure on the size and the yield of the precipitation process have been studied. The intense red fluorescent emission, excellent stability and potential low toxicity make these QDs promising for applications in bio-related areas such as fluorescence cell imaging or fluorescence bio labels.

In the present work, we report the synthesis and characterization of NaNbO3 particles obtained by microwave-assisted hydrothermal method from Nb2O5 and NaOH. The synthesis was made at different periods at 180 °C and 300W. The crystallization of NaNbO3 structures produced Na2Nb2O6.H2O in the intermediate phase with fiber-like morphology, and this is associated with the synthesis time. Pure orthorhombic NaNbO3 with cube-like morphology originates after synthesizing for 240 minutes. To verify the remnant polarization of particles, films were obtained by electrophoresis process and sintered at 800°C for 10 minutes in a microwave furnace. The films characterization indicated that films of niobate with fiber-like morphology present remaining polarization, and the morphology of cubes did not show remaining polarization. Considering these results, it can be concluded that the morphology implemented ferroelectric property of NaNbO3.

Calcium phosphates (CaPs) are major chemical constituents of mammalian bone. Their osteoconductivity in vitro and in vivo has encouraged their use in biomaterial applications such as implant materials and drug delivery. High aspect ratio nanoparticles are attractive for many biomedical applications; however, precise control of the phase and morphology is challenging. The impact of fuel-to-oxidant ratio, pH, and cation chemistry on morphology and phase was studied for CaP-based compositions by microwave-assisted solution combustion synthesis (MASCS) in a urea–nitrate (fuel–oxidant) system. An initial calcium to phosphate ratio of 1.5 was used. Highly crystalline hydroxyapatite (HA) and biphasic CaP nanoparticle compositions were produced as confirmed by x-ray diffraction, scanning electron microscopy, and transmission electron microscopy. MASCS was capable of synthesizing high aspect ratio (∼5 to 20) single and biphasic CaP nanoparticles with diameters ranging from 250 to 500 nm and lengths between 2 and 10 μm.

This work reports the preparation of iron-doped alumino-phosphate glass using microwave (MW) radiation at 1723 K in comparision with a conventional resistance heating furnace at the same temperature. X-ray diffraction analysis of the sample prepared in an MW furnace has confirmed glass formation which is similar to that of glass prepared in an electric furnace. Glass transition temperatures (Tg) for MW and conventional melted glass samples were observed to be 866 and 873 K, respectively. Higher Fe2+/(Fe3+ + Fe2+) ratio was reported in glass prepared in the MW furnace compared with the conventional furnace. The Fourier transform infrared spectra for both the samples indicate identical nature. It was observed that the maximum power required for melting glass in MW heating was 0.85 kW, which is around 25–30% of the power consumed by the conventional resistance heating furnace. In addition, the time needed to melt the glass in the MW furnace was found to be 3–4-fold lesser than the time required in the resistance heating furnace.

In this work, the morphology of BiFeO3 was successfully modulated from microsphere to microcube by using a polyanion, poly (methyl vinyl ether-alt-maleic acid) (PMVEMA), in a microwave assisted hydrothermal route. A simple ultrasonic purification method has been developed to obtain pure phase BiFeO3 from the crude products without using any chemicals. X-ray diffraction results confirmed the capability of this purification method. When increasing the amount of PMVEMA, the morphology of BiFeO3 gradually changed from microsphere to microcube as illustrated by scanning electron microscopy. A mechanism was suggested for the morphology evolution of BiFeO3. After the formation of the small BiFeO3 single crystal, PMVEMA preferentially absorbed on one side of the crystals through specific and/or noncovalent interactions, resulting in the preferential integration of these crystals to form microcubes. The magnetic properties of these microcrystals were also investigated and the magnetization of the microcubes increased with the decrease of temperature.