金属及其化合物作为能源催化领域的核心材料，其性能受限于传统少组元体系活性位点单一、电子结构调变能力不足，难以实现复杂反应路径和产物选择性的精准调控。高熵化策略虽为突破材料性能提供了全新途径，但其多组元的引入也带来了严重的相分离倾向，使得单相、均匀高熵材料的可控制备成为制约其应用研究的核心瓶颈。本文总结了针对高熵合金、高熵陶瓷及二维高熵磷硫化物等体系，发展的一系列可控制备技术：熔体抽丝法制备高熵合金纤维；无压烧结工艺实现致密高熵金属碳化物的合成；固相合成辅以超声剥离技术获得二维高熵磷硫化物；金属有机框架(MOF)前驱体衍生策略合成高熵金属氧化物。这些方法实现了高熵材料合成在成分均质化、结构致密化、材料维度控制以及前驱体设计等方面的突破。在此基础上，进一步阐述了高熵化在催化性能调控中的作用机制，揭示了多组元协同效应在激活惰性基面、优化金属—O键的共价性、增强结构稳定性等方面的关键作用。本文旨在通过制备方法的创新和机理的解析，为高性能高熵材料的发展提供切实可行的技术路径和理论依据。

Metals and their compounds are core materials in energy catalysis; however, their performance is often constrained by conventional few-component systems, which typically feature single active sites and limited electronic-structure tunability. These limitations hinder precise regulation of complex reaction pathways and product selectivity. High-entropy strategies offer a promising route to overcome these challenges by enabling multi-element synergistic effects. Nevertheless, introducing multiple elements increases the tendency toward phase separation, making the controllable synthesis of single-phase, compositionally uniform high-entropy materials a key bottleneck for practical applications. To address this issue, this study develops a series of controllable synthesis strategies for high-entropy alloys, high-entropy ceramics, and two-dimensional (2D) high-entropy phosphorus trichalcogenides. Specifically, melt extraction is employed to fabricate high-entropy alloy fibers; pressureless sintering is used to synthesize dense high-entropy metal carbides; solid-state synthesis combined with ultrasonic exfoliation enables the production of 2D high-entropy phosphorus trichalcogenides; and a metal-organic framework-derived strategy is adopted to construct high-entropy metal oxides. These methods enable key advances in high-entropy material synthesis, particularly in compositional homogenization, structural densification, dimensional control, and precursor design. Moreover, the role of high-entropy engineering in regulating catalytic performance is systematically elucidated, highlighting the critical contributions of multicomponent synergy to basal-plane activation, optimization of metal—oxygen covalency, and enhancement of structural stability. Overall, this study aims to provide practical technical pathways and a theoretical framework for developing high-performance high-entropy materials through innovative synthesis strategies and in-depth mechanistic insights.