Correlation study of graphitic shell encapsulated nickel: A multi-spectroscopic approach
Graphite-encapsulated metal nanoparticles hold great potential across various applications due to their unique combination of metal and graphitic properties. While Raman spectroscopy is widely used to assess the graphitic shells, metrics derived from prominent Raman bands often prove unreliable when...
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| Published in: | Carbon (New York) Vol. 232; p. 119704 |
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| Main Authors: | , , , , , , , |
| Format: | Journal Article |
| Language: | English |
| Published: |
Elsevier Ltd
15-01-2025
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| Subjects: | |
| Online Access: | Get full text |
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| Summary: | Graphite-encapsulated metal nanoparticles hold great potential across various applications due to their unique combination of metal and graphitic properties. While Raman spectroscopy is widely used to assess the graphitic shells, metrics derived from prominent Raman bands often prove unreliable when analyzing such structures with a large number of heterogeneous flakes and are mostly applicable to few-layer graphene. However, researchers continue to face challenges in identifying reliable metrics that accurately reflect two key properties of graphitic shells: thickness and degree of graphitization. In this study, graphitic shells were synthesized via plasma-enhanced chemical vapor deposition (PECVD) at low temperatures (500 °C), seeded by nickel nano-islands. A full-factorial experiment was designed to explore a diverse sample space by varying two key input factors: the initial thickness of the nickel seeding film and the duration of carbon deposition. Using resource-intensive surface characterization techniques (SEM, EDS, XPS, and AFM), we verified encapsulation efficiency and morphology, identifying strong correlations between the input factors and properties of the shells. To gain insights into structural characteristics, we employed conventional spectroscopy techniques (Raman, UV–Vis-nIR transmission, and Transient Absorption Spectroscopy), introducing 107 metrics derived from spectral data. Principal Component Analysis (PCA) aligned the input factors, and their corresponding shell properties, with the first two principal components. Accordingly, we identified the most relevant metrics including new candidates derived from less prominent Raman bands. Additionally, inter-metric correlations enable interchangeable use of spectroscopy techniques. This study marks the first multi-spectroscopic correlation analysis of graphitic shells and provides a novel framework for evaluating their properties.
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•A multi-spectroscopic correlation method has been introduced for studying carbon shelled structures.•Significant correlations identified between spectroscopy metrics and two input factors.•Uncovered inter-metric correlations enable interchangeable spectroscopy use for shell encapsulation studies.•Principal component analysis aligned input factors with the first two principal components.•Spectroscopic metrics relates PC1 to graphitic shell thickness and PC2 to shell graphitization. |
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| ISSN: | 0008-6223 |
| DOI: | 10.1016/j.carbon.2024.119704 |