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Krutaya Shtuka
Krutaya Shtuka
Krutaya Shtuka
FINAL ANALYSIS
Fig. 1. Principle of SE
Primary beam signal detection
Filter grid
In-lens detector
(Annular SE detector)
Magnetic lens
Final pole piece
Scan coil Electrostic lens
SE
det
ect
or
Backscattered Secondary electrons
electrons SE2 (1–50 nm)
(~300 nm) SE1
(a) (b)
2 μm 2 μm
Fig. 2. Palladium on carbon catalyst: (a) SE image taken at 20 kV using ET detector; (b) in-lens image taken
at 1.6 kV
is that the sample is made up of low atomic number BSEs which originate directly from the beam spot centre
atoms which cause larger interaction volumes for SE2, (3). The EsB image would avoid the contrast which
which in turn causes blurring. is contributed by those BSEs originating in ranges
relatively far away from the beam spot centre.
Energy Selective Backscattered Detection In order to clearly understand the meaning of the
The in-lens backscattered detector (also known as LL-BSE detection, it is necessary to explain a little bit
an energy selective backscattered (EsB) detector) is about the energy distribution of all possible electron
placed on the top of the in-lens SE detector (2) (as scattering processes. Figure 4 shows the whole energy
shown in Figure 3). When compared with a normal spectrum of the secondary and BSEs (conventionally
BSE detector, the EsB detector collects the low loss (LL)- energies >50 eV) plotted with increasing energy (4).
EsB detector
Filter grid
In-lens detector
Magnetic lens
Specimen
Figure 4 also shows a number of defined features loss events which are shown by the sharp low loss
in the spectrum such as Auger electrons, multiple peak at the right side of the spectrum. Under the low
inelastic scattered electrons, plasmon losses and low voltage primary beam energy conditions as shown
SE BSE
Low loss
Number of electrons
Discrimination
area set by EsB
detector
Plasmon
Auger losses
electrons
50 eV Electron energy, eV
Fig. 4. Spectrum of scattered electron energies from the SE process to the LL-BSE (based on low voltage
primary beam landing energies, where SE and BSE become relatively high compared to the broad saddle of
multiple inelastically scattered electrons between them)
200 nm
(b)
200 nm
in Figure 4, the SE and LL-BSE intensities become possible to distinguish the contrast difference between
relatively high when compared with the broad saddle Pt and C due to their large atomic number difference
of multiple inelastic scattered electrons in between. (Pt=78, C=6) in both images. But the main difference is
The regions in the low loss peak coloured blue, green the level of detail and the difference in the number of
and yellow represent the discrimination areas set by particles that can be observed between the two images.
the filter grid voltage of the EsB detector shown in In Figure 5(b), it is clear that the EsB image
Figure 3. In practice, it is possible just to cut off the SEs better shows the placement and morphology of Pt
and the whole blue spectrum area when the filter grid particles on carbon. By using lower energy electrons
is set to an optimum threshold. It would then result it is possible to reduce the interaction volume and
in a LL-BSE image with a good signal to noise ratio therefore the contrast from the surface layer is exposed
and good contrast. These fine contrast differences in this image. This is the reason that we only see the
are obtained from electrons with very little energy particles near the surface whereas in the BSE image in
loss generated in a very shallow region beneath the Figure 5(a), the carbon is blurred and we can see
surface away from the area where multiple inelastic all the particles as the signal comes from deeper
scattered electrons are produced. parts of the sample. The natural deduction would be
Figure 5 shows the images which were collected that it should be possible to change the voltage and
from platinum particles on a carbon support. It is observe particles at various depths (5). The clarity is
also associated with the filtering of the LL-BSE which The Authors
seems to make the biggest difference in the way the Winson Kuo obtained his PhD from the
Metallurgy and Materials Department
carbon is imaged as distinct particles rather than a
at the University of Birmingham,
blurred background. UK, in 2010. He has more than ten
years’ research experience in both
academic and industrial use of SEM,
Conclusions scanning transmission electron
The in-lens imaging technique using both SE and microscopy (STEM) and electron
probe microanalysis (energy dispersive
BSEs gives a distinct advantage to catalyst imaging. microanalysis (EDX), wavelength-
The two examples demonstrate that the SEs provide dispersive X-ray spectroscopy (WDX)
a more detailed and surface sensitive topography and electron backscatter diffraction
(EBSD)). Since 2012, he has been
and the BSEs provide a more depth sensitive responsible for developing electron
characterisation of the metal nanoparticles as well microscopy techniques customised for
Johnson Matthey materials, as well as
as helping to visualise these on individual units of developing and managing research
support material. projects with other partners from
industry and academia.
WINSON C. H. KUO*, MARTHA BRICENO and Martha Briceno received her doctoral
DOGAN OZKAYA degree in Materials Science from the
University of Oxford, UK, and she
Johnson Matthey Technology Centre, carried out postdoctoral studies in
Blount’s Court, Sonning Common, Reading RG4 9NH, UK the University of Illinois at Urbana-
Champaign, USA, and the University of
*Email: winson.kuo@matthey.com Oxford until she joined the Analytical
Department at Johnson Matthey
Technology Centre, Sonning Common,
UK. Her main scientific interest is
Acknowledgement to develop new methods to help
catalyst researchers obtain the best
The authors would like to thank both Henry Cai, microstructural characterisation from
Application Manager ASIA/PACIFIC, Zeiss NTS, their experiments. She is also expert
on cryo-electron microscopy (TEM and
Singapore, and Johnson Chen, Country Manager, Zeiss SEM) and in-situ TEM experiments
NTS, Taiwan, for sharing this EM information. Special (in-situ heating experiments, in-situ
straining and in-situ irradiation).
thanks to Johnson Matthey Electron Microscopy team
for support and discussion on this topic. Dogan Ozkaya works as a Senior
Principal Scientist and is in charge
of the electron microscopy team in
the Analytical Department at the
References Johnson Matthey Technology Centre,
Sonning Common. He holds a PhD in
1 J. Ackermann, ‘Manual for the SUPRA (VP) and ULTRA Materials Science and Metallurgy from
Scanning Electron Microscopes’, 2005, Carl Zeiss SMT the University of Cambridge, UK. He
carried out postdoctoral research in
2 J. P. Vermeulen, Microsc. Today, 2005, 13, 8 electron microscopy of various materials
in several university departments,
3 H. Jaksch, M. Steigerwald, V. Drexel and H. Bihr, Microsc. including the Cavendish Laboratory,
Microanal., 2003, 9, (S03), 106 University of Cambridge, and the
4 H. Jaksch, Microsc. Microanal., 2008, 14, (S2), 1226 Materials Department, University of
Oxford, before joining Johnson Matthey
5 J. Liu, Mater. Charact., 2000, 44, (4–5), 353 in 2003.