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Supported bimetallic alloy nanoparticles are of great interest in various catalytic applications due to the synergistic effects between different metals for improved catalytic performance. However, it still remains a challenge to efficiently synthesize atomically mixed alloy nanoparticles with uniform dispersion onto a desired substrate. Here, in situ, rapid synthesis of atomically mixed bimetallic nanoparticles well‐dispersed on a conductive carbon network via a 1 s high‐temperature pulse (HTP, ≈1550 K, duration 1 s, the rate of 10⁴K s⁻¹) is reported. The high temperature facilitates the total (atomic) mixing of different metals, while the rapid quenching ensures the uniform dispersion of nanoparticles with fine features such as twin boundaries and stacking faults, which are potentially beneficial to their catalytic performance. By varying the ratio of the precursor salts and parameters in the HTP process, the composition, size, and morphology of the resultant nanoparticles can easily be tuned. Moreover, the synthesized bimetallic (PdNi) nanoparticles demonstrate excellent electrocatalytic performance for the hydrogen evolution reaction and hydrogen peroxide electrooxidation. This work provides a general strategy for a facile and rapid synthesis of bimetallic nanoparticles directly from their salts for a range of emerging applications.

Composite materials with ordered microstructures often lead to enhanced functionalities that a single material can hardly achieve. Many biomaterials with unusual microstructures can be found in nature; among them, many possess anisotropic and even directional physical and chemical properties. With inspiration from nature, artificial composite materials can be rationally designed to achieve this anisotropic behavior with desired properties. Here, a metallic wood with metal continuously filling the wood vessels is developed, which demonstrates excellent anisotropic electrical, thermal, and mechanical properties. The well‐aligned metal rods are confined and separated by the wood vessels, which deliver directional electron transport parallel to the alignment direction. Thus, the novel metallic wood composite boasts an extraordinary anisotropic electrical conductivity (σ_||/σ_⊥) in the order of 10¹¹, and anisotropic thermal conductivity (κ_||/κ_⊥) of 18. These values exceed the highest reported values in existing anisotropic composite materials. The anisotropic functionality of the metallic wood enables it to be used for thermal management applications, such as thermal insulation and thermal dissipation. The highly anisotropic metallic wood serves as an example for further anisotropic materials design; other composite materials with different biotemplates/hosts and fillers can achieve even higher anisotropic ratios, allowing them to be implemented in a variety of applications.