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In our review, we have presented a summary of the research accomplishments of nanostructured multimetal-based electrocatalysts synthesized by modified polyol methods, especially the special case of Pt-based nanoparticles associated with increasing potential applications for batteries, capacitors, and fuel cells. To address the problems raised in serious environmental pollution, disease, health, and energy shortages, we discuss and present an improved polyol process used to synthesize nanoparticles from Pt metal to Pt-based bimetal, and Pt-based multimetal catalysts in the various forms of alloy and shell core nanostructures by practical experience, experimental skills, and the evidences from the designed polyol processes. In their prospects, there are the micro/nanostructured variants of hybrid Pt/nanomaterials, typically such as Pt/ABO3-type perovskite, Pt/AB2O4-type ferrite, Pt/CoFe2O4, Pt/oxide, or Pt/ceramic by modified polyol processes for the development of electrocatalysis and energy technology. In the future, we suggest that both the polyol and the sol-gel processes of diversity and originality, and with the use of various kinds of water, alcohols, polyols, other solvents, reducing agents, long-term capping and stabilizing agents, and structure- and property-controlling agents, are very effectively used in the controlled synthesis of micro/nanoparticles and micro/nanomaterials. It is understood that at the levels of controlling and modifying molecules, ions, atoms, and nano/microscales, the polyol or sol-gel processes, and their technologies are effectively combined in bottom-up and top-down approaches, as are the simplest synthetic methods of physics, chemistry, and biology from the most common aqueous solutions as well as possible experimental conditions.

Synthesis routes of CoSb3 need a long reaction time, especially at high temperature and-/or high pressure. Although the modified polyol process assisted with microwave radiation can be used to solve these problems, it used the excess amount of Sb ion. Therefore, this study aimed to solve this drawback by retarding the rate of reduction. The different microwave times (0, 1, and 3 min) were investigated to find out the shortest heating duration for preparing CoSb3 nanoparticles. Te-doped and Sn-doped CoSb3 were synthesized to investigate the benefit of this synthesis method for increasing the solubility limit of Te and Sn in the CoSb3 structure. The phase and microstructure of the synthesized products were characterized by using x-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). The results showed that the high crystalline phase of CoSb3 (JCPDS: 78-0977) without any metallic impurity phases product was successfully synthesized in 3 minutes for a heating time at normal pressure, non-excessive addition of Sb ion precursor, and low temperature. The XRD results of Te-doped and Sn-doped CoSb3 products exhibited poor crystalline phase and hard to exactly identify. In SEM and TEM results, the CoSb3 powder consisted of very tiny spherical-like particles around 10 nanometers attaching together even at different microwave time similar to Te-doped/Sn-doped samples.

The tungsten-modified titanium dioxide, which prepared through the one-pot solvothermal process, exhibited the large specific surface area (~ 202 m2/g) and greater electrical conductivity (~ 0.022 S/cm). Furthermore, for the comparison purpose to find appropriate approach for the synthesis 20 wt. % Pt NPs/Ti0.7W0.3O2 catalyst, the modified chemical reduction utilizing NaBH4 and the rapid microwave-assisted polyol using ethylene glycol were employed without any surfactants or stabilizers. The characterization of Pt-based electrocatalyst was investigated through XRD, SEM-EDX, TEM measurements. As result, the platinum nanocatalyst formation with the face-centered cubic structure (fcc) and the amount loading on Ti0.7W0.3O2 support approximately 20 wt. % of two synthesized methods. However, the diameter size and distribution of Pt nanoforms have clearly classified in two reduction route. For example, the Pt nanocatalyst, which was created by the rapid microwave-assisted polyol at 160 °C for 2 min, exhibited the good distribution on support with ~3 nm diameter. This could be ascribed to the fast and uniform heating of microwave-assisted and moderate reducing possibility of ethylene glycol. These results indicate that the rapid microwave-assisted polyol was an appropriate approach not only for synthesizing 20 wt. % Pt NPs/Ti0.7W0.3O2 catalyst but also for preparing Pt-based electrocatalysts.