Integration of a confocal Raman microscope in an electron microscope

Aksenov, Y.; Reinders, E. G. I.; Greve, Jan; Blitterswijk, Clemens A. van; Bruijn, Joost D. de; Otto, Cees

doi:10.1117/12.410628

Cited by 5 publications

(3 citation statements)

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“…An Oxford CT1500B cryo preparation and transfer system (Gatan) was modified for a custom installation on the EMRAM instrument, a combination a Philips XL‐30 ESEM (FEI Company) and a MCS‐1A micro Raman assembly, which was home built at the University of Twente (Aksenov et al 2000, 2002, 2003; Apeldoorn et al 2005). The MCS‐1A uses a micro‐lens (N.A.…”

Section: Methodsmentioning

confidence: 99%

“…The introduction of In‐SEM Raman under ambient temperature conditions showed that, despite the difference in resolution between an electron‐optical image and a light‐optical spectroscope, a good correlation was made between microstructure and composition (Aksenov et al ., 2000, 2002, 2003; Apeldoorn et al , 2005). A drawback of the method described was found in the preparation of dehydrated SEM specimen, which involves chemical fixations and dehydrations of the sample volume that may lead to aggregation, redistribution and extraction of components comparable to the metamorphosis grapes undergo while being dried into raisins (Fig.…”

Section: Introductionmentioning

confidence: 99%

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The feasibility of Cryo In-SEM Raman microspectroscopy

Hazekamp

Reed

Howard

et al. 2011

Journal of Microscopy

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Summary The combination of noninvasive compositional analysis by Raman microspectrometry with high‐resolution imaging in the scanning electron microscope greatly expands the analytical capabilities of the electron microscope. However, the chemical preparation of scanning electron microscope (SEM) specimens, although adequate for low‐resolution imaging of superficial detail, is not the true representation of the chemistry and composition of the sample, as extraction and aggregation artefacts as a result of dehydrating and cross‐linking agents are abundant. The original chemical composition and ultrastructure is only preserved using cryo preparation methods. Therefore, a complete cryo transfer flange was designed and built to add cryogenic control of specimens to the configuration of the EMRAM instrument, a combined Raman spectrometer and XL‐30 ESEM instrument. The Raman spectra of two model specimen, polystyrene beads and 2.3M sucrose were studied at ambient and cryogenic temperatures as well as during a heating ramp. Comparing the fingerprint regions of polystyrene and sucrose, both measured at ambient and at cryogenic conditions, only small spectral differences were observed for the main peaks of both molecules. A pronounced sharpening of the bands occurred in the 800–400 cm−1 region, a result of the reduction of intermolecular interactions. The enhanced visibility of the lower frequency modes may offer interesting potential for more detailed interpretation of Raman spectra.

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Section: Methodsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

The feasibility of Cryo In-SEM Raman microspectroscopy

Hazekamp

Reed

Howard

et al. 2011

Journal of Microscopy

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“…Integrated fluorescence and electron microscopy has been used for the correlative analysis of many biological samples; fluorescence microscopes for integration in SEM are commercially available . Integration of a Raman microscope (RM) with SEM has been developed . Furthermore, compact RMs for integration in scanning electron microscopes are commercially available.…”

Section: Introductionmentioning

confidence: 99%

Integration of correlative Raman microscopy in a dualbeam FIB SEM

Timmermans

Liszka

Lenferink

et al. 2016

J Raman Spectroscopy

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We present an integrated confocal Raman microscope in a focused ion beam scanning electron microscope (FIB SEM). The integrated system enables correlative Raman and electron microscopic analysis combined with focused ion beam sample modification on the same sample location. This provides new opportunities, for example the combination of nanometer resolution with Raman advances the analysis of sub-diffraction-sized particles. Further direct Raman analysis of FIB engineered samples enables in situ investigation of sample changes. The Raman microscope is an add-on module to the electron microscope. The optical objective is brought into the sample chamber, and the laser source, and spectrometer are placed in a module attached onto and outside the chamber. We demonstrate the integrated Raman FIB SEM function with several experiments. First, correlative Raman and electron microscopy is used for the investigation of (sub-)micrometer-sized crystals. Different crystals are identified with Raman, and in combination with SEM the spectral information is combined with structurally visible polymorphs and particle sizes. Analysis of sample changes made with the ion beam is performed on (1) structures milled in a silicon substrate and (2) after milling with the FIB on an organic polymer. Experiments demonstrate the new capabilities of an integrated correlative Raman-FIB-SEM. Copyright

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An overview of emerging hyphenated SEM-EDX and Raman spectroscopy systems: Applications in life, environmental and materials sciences

Cardell

Guerra-Tschuschke

2016

TrAC Trends in Analytical Chemistry

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Integration of a confocal Raman microscope in an electron microscope

Cited by 5 publications

References 0 publications

The feasibility of Cryo In-SEM Raman microspectroscopy

The feasibility of Cryo In-SEM Raman microspectroscopy

Integration of correlative Raman microscopy in a dualbeam FIB SEM

An overview of emerging hyphenated SEM-EDX and Raman spectroscopy systems: Applications in life, environmental and materials sciences

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