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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Main Authors: Jan Reimers, Martin Mikulics, Marta Lipinska-Chwalek, Berit Zeller-Plumhoff, Lidia Kibkalo, Maximilian Kruth, Regine Willumeit-Römer, Joachim Mayer, Hilde Helen Hardtdegen
Format: Article
Language:English
Published: MDPI AG 2025-03-01
Series:Nanomaterials
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Online Access:https://www.mdpi.com/2079-4991/15/6/430
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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
collection DOAJ
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.
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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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