Towards Correlative Raman Spectroscopy–STEM Investigations Performed on a Magnesium–Silver Alloy FIB Lamella
In this study, a lamella prepared using focused ion beam (FIB) milling from a magnesium–silver alloy wire was investigated. The wire, intended for biomedical applications, was initially degraded in simulated body fluid (SBF) under physiological conditions. Raman spectroscopy was performed across the...
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MDPI AG
2025-03-01
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| author | Jan Reimers Martin Mikulics Marta Lipinska-Chwalek Berit Zeller-Plumhoff Lidia Kibkalo Maximilian Kruth Regine Willumeit-Römer Joachim Mayer Hilde Helen Hardtdegen |
| author_facet | Jan Reimers Martin Mikulics Marta Lipinska-Chwalek Berit Zeller-Plumhoff Lidia Kibkalo Maximilian Kruth Regine Willumeit-Römer Joachim Mayer Hilde Helen Hardtdegen |
| author_sort | Jan Reimers |
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| description | In this study, a lamella prepared using focused ion beam (FIB) milling from a magnesium–silver alloy wire was investigated. The wire, intended for biomedical applications, was initially degraded in simulated body fluid (SBF) under physiological conditions. Raman spectroscopy was performed across the entire FIB specimen and the results were correlated with findings from scanning transmission electron microscopy (STEM). Our micro-Raman analysis identified chemical compounds at distinct regions within the specimen. Dominant Raman modes at ~1350 cm<sup>−1</sup> and ~1590 cm<sup>−1</sup>, likely derived from elemental carbon from the FIB protection layer, were observed. Additionally, modes indicative of the alloy’s interaction with SBF, attributable to the constituents of SBF, were detected. Notably, Raman modes at ~3650 cm<sup>−1</sup> corresponding to the OH stretching mode were identified in the targeted areas of the lamella, highlighting the chemical interaction between magnesium (Mg) and the SBF. The micro-Raman mapping images showed localized Mg(OH)<sub>2</sub> distributions, which correlated strongly with the STEM analyses. This study underscores the effectiveness of correlating Raman spectroscopy, revealing chemical changes and STEM, capturing the corresponding microstructural changes. The combined approach is crucial for a deeper understanding of material degradation and reactivity in biocompatible alloys under physiological conditions and advances the characterization of biocompatible materials in physiological environments. |
| format | Article |
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| institution | OA Journals |
| issn | 2079-4991 |
| language | English |
| publishDate | 2025-03-01 |
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| series | Nanomaterials |
| spelling | doaj-art-72db2cb8709742beaeaaddc6b0151b4e2025-08-20T01:48:57ZengMDPI AGNanomaterials2079-49912025-03-0115643010.3390/nano15060430Towards Correlative Raman Spectroscopy–STEM Investigations Performed on a Magnesium–Silver Alloy FIB LamellaJan Reimers0Martin Mikulics1Marta Lipinska-Chwalek2Berit Zeller-Plumhoff3Lidia Kibkalo4Maximilian Kruth5Regine Willumeit-Römer6Joachim Mayer7Hilde Helen Hardtdegen8Ernst Ruska-Centre, Forschungszentrum Jülich, 52425 Jülich, GermanyErnst Ruska-Centre, Forschungszentrum Jülich, 52425 Jülich, GermanyErnst Ruska-Centre, Forschungszentrum Jülich, 52425 Jülich, GermanyInstitut für Metallische Biomaterialien, Helmholtz-Zentrum Hereon GmbH, Max-Planck Str. 1, 21502 Geesthacht, GermanyErnst Ruska-Centre, Forschungszentrum Jülich, 52425 Jülich, GermanyErnst Ruska-Centre, Forschungszentrum Jülich, 52425 Jülich, GermanyInstitut für Metallische Biomaterialien, Helmholtz-Zentrum Hereon GmbH, Max-Planck Str. 1, 21502 Geesthacht, GermanyErnst Ruska-Centre, Forschungszentrum Jülich, 52425 Jülich, GermanyErnst Ruska-Centre, Forschungszentrum Jülich, 52425 Jülich, GermanyIn this study, a lamella prepared using focused ion beam (FIB) milling from a magnesium–silver alloy wire was investigated. The wire, intended for biomedical applications, was initially degraded in simulated body fluid (SBF) under physiological conditions. Raman spectroscopy was performed across the entire FIB specimen and the results were correlated with findings from scanning transmission electron microscopy (STEM). Our micro-Raman analysis identified chemical compounds at distinct regions within the specimen. Dominant Raman modes at ~1350 cm<sup>−1</sup> and ~1590 cm<sup>−1</sup>, likely derived from elemental carbon from the FIB protection layer, were observed. Additionally, modes indicative of the alloy’s interaction with SBF, attributable to the constituents of SBF, were detected. Notably, Raman modes at ~3650 cm<sup>−1</sup> corresponding to the OH stretching mode were identified in the targeted areas of the lamella, highlighting the chemical interaction between magnesium (Mg) and the SBF. The micro-Raman mapping images showed localized Mg(OH)<sub>2</sub> distributions, which correlated strongly with the STEM analyses. This study underscores the effectiveness of correlating Raman spectroscopy, revealing chemical changes and STEM, capturing the corresponding microstructural changes. The combined approach is crucial for a deeper understanding of material degradation and reactivity in biocompatible alloys under physiological conditions and advances the characterization of biocompatible materials in physiological environments.https://www.mdpi.com/2079-4991/15/6/430Mg-Ag alloyscarboncorrelative characterizationRaman spectroscopyscanning transmission electron microscopy |
| spellingShingle | Jan Reimers Martin Mikulics Marta Lipinska-Chwalek Berit Zeller-Plumhoff Lidia Kibkalo Maximilian Kruth Regine Willumeit-Römer Joachim Mayer Hilde Helen Hardtdegen Towards Correlative Raman Spectroscopy–STEM Investigations Performed on a Magnesium–Silver Alloy FIB Lamella Nanomaterials Mg-Ag alloys carbon correlative characterization Raman spectroscopy scanning transmission electron microscopy |
| title | Towards Correlative Raman Spectroscopy–STEM Investigations Performed on a Magnesium–Silver Alloy FIB Lamella |
| title_full | Towards Correlative Raman Spectroscopy–STEM Investigations Performed on a Magnesium–Silver Alloy FIB Lamella |
| title_fullStr | Towards Correlative Raman Spectroscopy–STEM Investigations Performed on a Magnesium–Silver Alloy FIB Lamella |
| title_full_unstemmed | Towards Correlative Raman Spectroscopy–STEM Investigations Performed on a Magnesium–Silver Alloy FIB Lamella |
| title_short | Towards Correlative Raman Spectroscopy–STEM Investigations Performed on a Magnesium–Silver Alloy FIB Lamella |
| title_sort | towards correlative raman spectroscopy stem investigations performed on a magnesium silver alloy fib lamella |
| topic | Mg-Ag alloys carbon correlative characterization Raman spectroscopy scanning transmission electron microscopy |
| url | https://www.mdpi.com/2079-4991/15/6/430 |
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