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Updated: Jun 2, 2026

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Effect of Microwave Synthesis Conditions on the Structure of Nickel Hydroxide Nanosheets
Published on: August 18, 2023
Structure and stability of nickel/nickel oxide core-shell nanoparticles
S D'Addato1, V Grillo, S Altieri
1CNR-Istituto Nanoscienze, Centro S3, Via G Campi 213/a, I-41125 Modena, Italy. sergio.daddato@unimore.it
Summary
This study reveals that nickel nanoparticles (Ni NPs) retain a metallic core even after oxidation, with an icosahedral structure. Nickel oxide forms as islands on the nanoparticle surface.
Area of Science:
- Materials Science
- Nanotechnology
- Surface Chemistry
Background:
- Nickel nanoparticles (Ni NPs) are crucial in catalysis and materials science.
- Understanding their oxidation behavior is key to controlling their properties.
- Previous studies have explored Ni NP oxidation, but detailed structural analysis post-oxidation remains important.
Purpose of the Study:
- To investigate the structural and chemical changes in Ni nanoparticles during oxidation.
- To characterize the core-shell structure of oxidized Ni NPs.
- To determine the specific crystalline structure of the Ni NP core and the NiO phase.
Main Methods:
- Combined in situ X-ray Photoelectron Spectroscopy (XPS) and High-Resolution Transmission Electron Microscopy (HR-TEM).
- Preparation of pre-formed Ni NP films (4-8 nm diameter) within a controlled experimental setup.
- Controlled oxidation using O(2) gas and atmospheric exposure, with in situ XPS analysis.
Main Results:
- XPS revealed a composite Ni 2p spectrum indicating both metallic Ni core and NiO shell.
- The metallic Ni core signal persisted even after air exposure.
- HR-TEM and simulations confirmed a multitwinned icosahedral structure for the Ni NP core.
- Nickel oxide (NiO) was observed as distinct islands on the NP surface.
Conclusions:
- Nickel nanoparticles maintain a metallic core even after significant oxidation.
- The core exhibits a well-defined icosahedral structure.
- Oxidation results in the formation of NiO islands on the nanoparticle surface, suggesting a heterogeneous oxidation process.

