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Abstract High temperature synthesis and treatments are ubiquitous in chemical reactions and material manufacturing. However, conventional sintering furnaces are bulky and inefficient with a narrow temperature range (<1500 K) and slow heating rates (<100 K min⁻¹), which are undesirable for many applications that require transient heating to produce ideal nanostructures. Herein, a 3D‐printed, miniaturized reactor featuring a dense micro‐grid design is developed to maximize the material contact and therefore acheive highly efficient and controllable heating. By 3D printing, a versatile, miniaturized reactor with microscale features can be constructed, which can reach a much wider temperature range (up to ≈3000 K) with ultrafast heating/cooling rates of ≈10⁴K s⁻¹. To demonstrate the utility of the design, rapid and batch synthesis of Ru nanoparticles supported in ordered mesoporous carbon is performed by transient heating (1500 K, 500 ms). The resulting ultrafine and uniform Ru nanoparticles (≈2 nm) can serve as a cathode in Li‐CO₂batteries with good cycling stability. The miniaturized reactor, with versatile shape design and highly controllable heating capabilities, provides a platform for nanocatalyst synthesis with localized and ultrafast heating toward high temperatures that is otherwise challenging to achieve. 

Abstract Efficient electrocatalysts are critical in various clean energy conversion and storage systems. Polyelemental nanomaterials are attractive as multifunctional catalysts due to their wide compositions and synergistic properties. However, controlled synthesis of polyelemental nanomaterials is difficult due to their complex composition. Herein, a one‐step synthetic strategy is presented to fabricate a hierarchical polyelemental nanomaterial, which contains ultrasmall precious metal nanoparticles (IrPt, ≈5 nm) anchored on spinel‐structure transition metal oxide nanoparticles. The polyelemental nanoparticles serve as excellent bifunctional catalysts for the oxygen evolution reaction (OER) and oxygen reduction reaction (ORR). The mass catalytic activity of the polyelemental nanoparticles is 7‐times higher than that of Pt in ORR and 28‐times that of Ir in OER at the same overpotentials, demonstrating the high activity of the bifunctional electrocatalyst. This outstanding performance is attributed to the controlled multiple elemental composition, mixed chemical states, and large electroactive surface area. The hierarchical nanostructure and polyelemental design of these nanoparticles offer a general and powerful alternative material for catalysis, solar cells, and more. 

Abstract Mixing multimetallic elements in hollow‐structured nanoparticles is a promising strategy for the synthesis of highly efficient and cost‐effective catalysts. However, the synthesis of multimetallic hollow nanoparticles is limited to two or three elements due to the difficulties in morphology control under the harsh alloying conditions. Herein, the rapid and continuous synthesis of hollow high‐entropy‐alloy (HEA) nanoparticles using a continuous “droplet‐to‐particle” method is reported. The formation of these hollow HEA nanoparticles is enabled through the decomposition of a gas‐blowing agent in which a large amount of gas is produced in situ to “puff” the droplet during heating, followed by decomposition of the metal salt precursors and nucleation/growth of multimetallic particles. The high active sites per mass ratio of such hollow HEA nanoparticles makes them promising candidates for energy and electrocatalysis applications. As a proof‐of‐concept, it is demonstrated that these materials can be applied as the cathode catalyst for Li–O₂battery operations with a record‐high current density per catalyst mass loading of 2000 mA g_cat.⁻¹, as well as good stability and durable catalytic activity. This work offers a viable strategy for the continuous manufacturing of hollow HEA nanomaterials that can find broad applications in energy and catalysis.