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(NH4)2RuCl6is an important precursor in the synthesis of Ru powder with high-purity requirement. In this study, high-purity (>99.999 wt%) micro-sized (NH4)2RuCl6pieces were synthesized by distillation and precipitation from crude Ru powder. Then, the thermal decomposition behavior of the (NH4)2RuCl6pieces was investigated. The decomposition process included two stages. First, (NH4)2RuCl6was decomposed from 255.0°C to 314.0°C, with the endothermic peak located at 309.4°C. At this stage, HCl and NH3were released, while the dense micro-pieces were transformed to loosened micro-pieces due to the thermal decomposition. Then, the solid phase [(NH3)4Ru3Cl12] kept decomposing from 314.0°C to 352.7°C, HCl and N2were released, and agglomerated Ru particles were achieved. Thermogravimetric analysis-differential thermal analysis-mass spectrum coupling (TG-DTA-MS) was used to monitor the thermal decomposition process and identify the released gaseous phases, respectively. The solid phases in different stages were characterized by high-temperature X-ray diffraction (HTXRD). A good understanding of the processing and thermal decomposition of (NH4)2RuCl6is crucial in the creation of Ru products.

Pt-based high-entropy-alloy nanoparticles (HEA-NPs) have excellent physical and chemical properties due to the diversity of composition, complexity of surface structure, high mixing entropy, and properties of nanoscale, and they are used in a wide range of catalytic applications such as catalytic ammoxidation, the electrolysis of water to produce hydrogen, CO2/CO reduction, and ethanol/methanol oxidation reaction. However, offering a facile, low-cost, and large-scale method for preparing Pt-based HEA-NPs still faces great challenges. In this study, we employed a spray drying technique combined with thermal decomposition reduction (SD-TDR) method to synthesize a single-phase solid solution from binary nanoparticles to denary Pt-based HEA-NPs containing 10 dissimilar elements loaded on carbon supports in an H2atmosphere with a moderate heating rate (3 °C/min), thermal decomposition temperature (300–850 °C), duration time (30 min), and low cooling rate (5–10 °C/min). The Pt autocatalytic behavior was found and investigated, confirming that Pt element could decrease the reduction temperature of other metals via autocatalytic behavior. Therefore, using the feature of Pt autocatalytic behavior, we have achieved Pt-based HEA-NPs at a minimum temperature of 300 °C. We not only prepared a series of Pt-based HEA-NPs with targetable ingredient, size, and phase using the SD-TDR method but also proved the expandability of the SD-TDR technique by synthesizing Pt-based HEA-NPs loaded on different supports. Moreover, we investigated methanol oxidation reaction (MOR) on as-synthesized senary PtCoCuRuFeNi HEA-NPs, which presented superior electrocatalytic performance over commercial Pt/C catalyst.