Microwave-Assisted Synthesis of Core–Shell Structured Pd@PdPtCuFe Recessed Truncated Octahedral Nanocrystals for Multifunctional Electrocatalysis

Authors

• Dezhong Hu, New Energy Research Institute, School of Environment and Energy, South China University of Technology, 382 East Waihuan Road, 510006, China.
• Wendan Jiang, New Energy Research Institute, School of Environment and Energy, South China University of Technology, 382 East Waihuan Road, 510006, China.
• Wei Keat Ng, New Energy Research Institute, School of Environment and Energy, South China University of Technology, 382 East Waihuan Road, 510006, China.
• Jun Yang, School of Chemical Engineering, Guangdong University of Petrochemical Technology, 139 Guandu Er Road, 525000, China.Follow
• Xiongwu Kang, New Energy Research Institute, School of Environment and Energy, South China University of Technology, 382 East Waihuan Road, 510006, China.Follow

Document Type

Article

Corresponding Author(s)

Jun Yang(yangjun@gdupt.edu.cn);
Xiongwu Kang(esxkang@scut.edu.cn)

Abstract

Developing cost-efficient and durable multifunctional electrocatalysts of hydrogen evolution reaction (HER), oxygen reduction reaction (ORR) and oxygen evolution reaction (OER) is crucial for improving energy conversion efficiency in electrolytic water splitting electrolyzer and advancing rechargeable zinc–air batteries (ZABs). Polyhedral shaped nanocrystals with well-defined crystal facets represent a type of model catalysts that enables the exploration of structure-activity. However, it is still very challenging to prepare alloy nanocrystals with multiple metal components due to their complicated redox potentials and mixing enthalpy. Herein, we report a rapid microwave-assisted polyol reduction method for synthesis of core–shell Pd@PdPtCu, Pd@PdPtCuNi, Pd@PdPtCuCo and Pd@PdPtCuZn octahedra nanocrystals and recessed truncated-octahedra Pd@PdPtCuFe nanocrystals. Ascribing to the fast reduction and nucleation rate of Pd precursors, Pd core was first formed. Further concurrent reduction and efficient diffusion of the rest metal precursors result in the PdPtCu or PdPtCuM (M = Ni, Co, Fe and Zn) alloy shell. It is observed that Fe plays a decisive role in driving the morphological evolution from octahedral to recessed truncated-octahedra nanocrystals. The Fe³⁺–Br⁻ coordination modulates crystal growth kinetics by altering surface adsorption dynamics, resulting in a mixed exposure of {111} and {100} facets rich in edge and vertex sites. Structural analyses confirm a well-defined Pd core and homogeneous PdPtCuFe alloy shell with a face-centered-cubic phase. Owing to the synergistic electronic coupling between Fe and noble-metal components and the strain-regulated surface configuration, Pd@PdPtCuFe/C exhibits superior multifunctional activity with a HER overpotential of 18 mV at 10 mA⋅cm^-2 and Tafel slope of 27 mV⋅dec^-1, the most active HER catalysts among the five prepared core@shell catalysts and superior to that of commercial Pt/C. In addition, it delivers an OER overpotential of 360 mV at 10 mA⋅cm^-2 and a Tafel slope of 75.9 mV⋅dec^-1, comparable to that of the benchmark IrO₂ catalysts. All the prepared catalysts exhibit certain ORR activity, together with an ORR half-wave potential of 0.792 V in alkaline electrolyte. When applied as a cathode catalyst in ZABs, Pd@PdPtCuFe/C delivers a peak power density of 81.2 mW⋅cm^-2 and maintains stable cycling for over 50 h. This work provides a generalizable route for ultrafast morphology-controlled synthesis of multimetallic nanocrystals, paving the way for the rational design of high-performance, low-PGM bifunctional catalysts for next-generation energy conversion and storage systems.

Graphical Abstract

Keywords

octahedra, recessed truncated-octahedra, microwave-assisted, core–shell, multifunctional electrocatalysis

DOI

10.61558/2993-074X.3617

Online Date

6-10-2026

Recommended Citation

Dezhong Hu, Wendan Jiang, Wei Keat Ng, Jun Yang, Xiongwu Kang. Microwave-Assisted Synthesis of Core–Shell Structured Pd@PdPtCuFe Recessed Truncated Octahedral Nanocrystals for Multifunctional Electrocatalysis[J]. Journal of Electrochemistry, doi: 10.61558/2993-074X.3617.