Inorganic syntheses assisted by microwave heating

This Special Issue on “Inorganic Syntheses Assisted by Microwave Heating” represents one of the few fully dedicated issues on inorganic microwave synthesis published by any international scientific journal and it features five papers and one review article. [...

Morphology and Photoluminescence of HfO2Obtained by Microwave-Hydrothermal

In this letter, we report on the obtention of hafnium oxide (HfO2) nanostructures by the microwave-hydrothermal method. These nanostructures were analyzed by X-ray diffraction (XRD), field-emission gum scanning electron microscopy (FEG-SEM), transmission electron microscopy (TEM), energy dispersive X-ray spectrometry (EDXS), ultraviolet–visible (UV–vis) spectroscopy, and photoluminescence (PL) measurements. XRD patterns confirmed that this material crystallizes in a monoclinic structure. FEG-SEM and TEM micrographs indicated that the rice-like morphologies were formed due to an increase in the effective collisions between the nanoparticles during the MH processing. The EDXS spectrum was used to verify the chemical compositional of this oxide. UV–vis spectrum revealed that this material have an indirect optical band gap. When excited with 488 nm wavelength at room temperature, the HfO2nanostructures exhibited only one broad PL band with a maximum at around 548 nm (green emission)

Perovskite oxides rpepared by hydrothermal and solvothermal synthesis : a review of crystallisation, chemistry, and compositions

Perovskite oxides with general composition ABO3 are a large group of inorganic materials that can contain a variety of cations from all parts of the Periodic Table and that have diverse properties of application in fields ranging from electronics, energy storage to photocatalysis. Solvothermal synthesis routes to these materials have become increasingly investigated in the past decade as a means of direct crystallisation of the solids from solution. These methods have significant advantages leading to adjustment of crystal form from the nanoscale to the micron‐scale, the isolation of compositions not possible using conventional solid‐state synthesis and in addition may lead to scalable processes for producing materials at moderate temperatures. These aspects are reviewed, with examples taken from the past decade’s literature on the solvothermal synthesis of perovskites with a systematic survey of B‐site cations, from transition metals in Groups 4‐8 and main group elements in Groups 13, 14 and 15, to solid solutions and heterostructures. As well as hydrothermal reactions, the use of various solvents and solution additives are discussed and some trends identified, along with prospects for developing control and predictability in the crystallisation of complex oxide materials

Rapid continuous microwave-assisted synthesis of silver nanoparticles to achieve very high productivity and full yield: from mechanistic study to optimal fabrication strategy

Systematic studies of silver nanoparticle synthesis in a continuous-flow single-mode microwave reactor using polyol process were performed, revealing that the synthesis is exceptionally effective to give very small metal particles at full reaction yield and very high productivity. Inlet concentration of silver nitrate or silver acetate, applied as metal precursors, varied between 10 and 50 mM, and flow rates ranged from 0.635 to 2.5 dm3/h, to give 3–24 s reaction time. Owing to its much higher reactivity, silver acetate was shown to be far superior substrate for the synthesis of small (10–20 nm) spherical silver nanoparticles within a few seconds. Its restricted solubility in ethylene glycol, applied as the solvent and reducing agent, appeared to be vital for effective separation of the stage of particle growth from its nucleation to enable rapid synthesis of small particles in a highly loaded system. This was not possible to obtain using silver nitrate. All the observations could perfectly be explained by a classical LaMer–Dinegar model of NPs’ formation, but taking into account also nonisothermal character of the continuous-flow process and acetate dissolution in the reaction system. The performed studies indicate an optimal strategy for the high-yield fabrication of metal particles using polyol method