SIM0216
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ELECTRON MICROSCOPY<br />
Fig. 3: (A) SEM image of multiple graphene flakes,<br />
noticeable by the darker color for multilayers. (B)<br />
Raman spectrum measured on the position indicated<br />
in A, of a representative location on the<br />
graphene flake, the D, G, and 2D bands are indicated.<br />
(C, D, E) integrated Raman intensity of the D,<br />
G, and 2D graphene bands.<br />
Chemical Specificity<br />
with Electron Microscopy<br />
Integrated Raman and electron microscopy<br />
enables the correlative analysis of<br />
samples with both chemical specific Raman-<br />
and nanometer resolution electron<br />
microscopy. Applications demonstrating<br />
correlative chemical specificity and high<br />
resolution are performed on multiple<br />
samples. First a sample containing multiple<br />
different crystals is analyzed, showing<br />
spectral Raman analysis correlated<br />
to particle morphologies observed with<br />
SEM. Second a sample of graphene flakes,<br />
fabricated through chemical deposition,<br />
is investigated for potential contaminations<br />
and spectral intensity analysis of<br />
the D, G, and 2D Raman bands. Correlative<br />
chemical and high resolution microscopic<br />
analysis is demonstrated in figure<br />
2, where crystal sub-micron morphological<br />
and chemical specific analysis is demonstrated.<br />
The samples contain many different<br />
structures two calcium carbonate<br />
polymorphisms, calcite and vaterite and<br />
calcium sulfate crystals, further the photosynthetic<br />
bacteria M. aeruginosa is analyzed.<br />
Figure 2A, and B shows the correlative<br />
SEM and Raman cluster image<br />
from the observed region of interest. Specific<br />
structures in the analyzed region<br />
are indicated in 2C, and the corresponding<br />
spectra are presented in figure 2D, E,<br />
and F. Calcium sulfate crystals are identified<br />
by their 1006 cm -1 Raman band, and<br />
a needle like shape is observed in the SEM<br />
analysis, the polymorphisms calcite and<br />
Fig. 4: (A) SEM image of FIB patterned silicon. (B) 1 st order silicon Raman band analysis. (C, D, E) Intensity,<br />
spectral width, and peak position of the 1 st order silicon band over the FIB patterned region. (F) Raman<br />
band of amorphous silicon, indicated on the 450 cm -1 region. (G) Intensity map of amorphous silicon [3].<br />
vaterite are identified by the Raman band<br />
positions at 1086 cm -1 and 1088 cm -1<br />
respectively.<br />
Correlative Raman Electron<br />
Microscopy of Graphene<br />
Correlative Raman micro-spectroscopy<br />
with electron microscopy is performed on<br />
a sample containing graphene flakes (fig.<br />
3). The sample is fabricated with a chemical<br />
vapor deposition method on a nickel<br />
substrate. The process fabricates singleand<br />
multi-layer graphene, with multi-layers<br />
visible as darker areas in SEM analysis.<br />
The graphene structure quality on<br />
nickel is investigated with Raman microspectroscopy.<br />
The known Raman bands<br />
for graphene the 2D, G and D bands are<br />
visible in the spectra. The graphene D<br />
band is often an indication of disorder in<br />
the graphene structure. Performing a Raman<br />
microscopic image reveals an overall<br />
high quality sample, low D-band intensity,<br />
specific the locations with high<br />
D-band intensity can potentially be further<br />
investigated at higher resolution using<br />
correlative electron microscopy. Further<br />
the Raman intensity maps of the<br />
G- and 2D- band are provided in figure 3D<br />
and E, showing increased Raman activity<br />
for multi-layer graphene on nickel. The<br />
use of Raman spectroscopy for detection<br />
of single or multiple layers of graphene<br />
and analysis of the thickness uniformity<br />
More information:<br />
http://bit.ly/IM-Raman<br />
More information on Focused Ion<br />
Beam: http://bit.ly/IM-FIB<br />
[1]<br />
All references:<br />
http://bit.ly/IM-Timmermans<br />
36 • G.I.T. Imaging & Microscopy 2/2016