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Efficient Separation of Secondary and


Backscattered Electrons with a Single Detector

White Paper

Efficient Separation of Secondary and


Backscattered Electrons with a Single Detector
Author:

Dr. Heiko Stegmann, Dr. Katja Tsyrulin, Dr. Sabine Lenz


Carl Zeiss Microscopy GmbH
Date:

April 2013

High resolution structural and compositional analysis of nano-materials in the scanning electron microscope (SEM)
requires secondary electron (SE) and backscattered electron (BSE) imaging at low primary beam energies. So far,
these imaging modes could only be performed using dedicated, separate detection systems for SE and BSE.
The ZEISS InLensDuo detector provides separate SE and BSE detection in a single, easy to use detector system.

SE and BSE detection for nano-materials


characterization
Nano-materials and nano-composites play an ever-growing

number of the interaction volume. Thus, they provide infor-

technological and economic role. Research and develop-

mation about the distribution of different elements in the

ment, as well as manufacturing process and quality control

sample. Multiply-scattered BSE (BSE2) take off at a lower

of such materials require their structural and compositional

angle. They carry a mixture of compositional and crystalline

analysis with nanometer resolution.

information of the sample. They can be efficiently collected


at medium to primary beam energy using below-lens seg-

In an SEM, such analysis can be efficiently performed using

mented detectors to provide compositional, cystallographic

the information that is conveyed by the SE and BSE produced

and topographic information.

during the interaction of the primary electron beam with the


specimen. They can be further classified according to their

Nano-materials characterization in the SEM requires highest reso-

origin. Due to their characteristic energy and spatial distribu-

lution and strong material contrast. The resolution needed is

tions, these different electron types can be separated in the

only achievable with sufficiently small interaction volumes and,

SEM by suitable detection systems.

thus, at low energy of the primary beam. Efficient detection of


SE1 and low energy BSE1 is only possible with InLens detectors,

SE1 are emitted into a high angle from close proximity to

making them the preferred detector type for nano-materials

the incidence of the primary beam. Therefore, they carry

characterization. However, two separate, standalone detector

high-resolution information of the sample surface, and can

systems for SE and BSE will significantly increase purchase and

be detected with column-mounted (InLens) detectors.

maintenance cost of the tool.

SE2 are generated in a larger volume and emit into lower


angles. They provide lower-resolution, topographical information and are usually collected with a chamber mounted

Solution

Everhart-Thornley type detector, along with a small


fraction of BSE.

The ZEISS InLensDuo detector available for the


MERLIN Compact FE-SEMs is a column-mounted detector

BSE1 are singly scattered BSE mainly emitted into high

comprising a scintillator with optically coupled photo-

angles. Their yield is strongly related to the mean atomic

multiplier and a filtering grid that can be biased with a

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retarding potential adjustable from -1.5 kV to 0 kV. Due


to the electron-optical design of the ZEISS GEMINI electron
column with its integrated beam booster, SE and BSE are
following a reverse beam path into the column. The InLensDuo
detector is placed at the proper position in the beam path to
accept and directly detect both BSE above 500 eV and SE
(Figure 1).

Figure 1. Schematic cross-sectional drawing of the GEMINI lens with the


InLensDuo detector.

The InLensDuo detector possesses two operating modes:


When the filtering grid is switched on, electrons with an
energy lower than the grid voltage, i.e. all SE, will be rejected
and only BSE will reach the scintillator. The bias voltage
applied controls the energy range of the BSE detected.
With the grid switched off, all electrons are permitted to
reach the scintillator, effectively resulting in SE imaging
due to the relatively small contribution of BSE to the total
electron yield.
Switching detection modes is a matter of seconds, and as
the filtering grid potential does not interfere with the field at
the polepiece gap, beam position, focus and astigmatism are
not affected (Figure 2).
Figure 2. Switching between different imaging modes produces no change in
focus, astigmatism, or beam shift (refer to the reduced scan area in the image
center).

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Application example
In high temperature applications such as gas turbines, the

Figure 4 presents the InLensDuo SE and BSE modes at 1500 V

typically used nickel based superalloys are operated close to

acceleration voltage, with the filtering grid set to 1000 V.

their melting temperature. For higher temperature applica-

The BSE mode image clearly shows two different phase

tions, they have to be actively cooled or coated with thermal

morphologies, lamellar and globular. Such images can easily

barriers. Rhenium is a refractory element with a high melting

be segmented for calculation of the distributions of the

point that readily dissolves in cobalt. It considerably increases

different morphologies [2]. At higher magnification, the

the melting temperatures of cobalt based alloys beyond those

high resolution capability of imaging with the InLensDuo SE

of Ni-based superalloys. Therefore, Co-Re alloys are being

mode reveals nanometer scale porosity at the void walls

developed to replace conventional materials in high tempera-

(Figure 5, left), while the BSE mode image shows material

ture applications [1]. Tuning their mechanical properties and

contrast detail on the same length scale (Figure 5, right).

oxidation resistance requires characterization of microstructure and distribution of small amounts of other additives.
To demonstrate the suitability of the InLensDuo detector for
characterizing such a material, an aged Co-17Re-23Cr-25Ni
sample was prepared by electropolishing. This quaternary
alloy contains fine microstructural features such as Re rich
phase particles distributed in the Co phase, as well as voids.
The sample was examined in a MERLIN Compact VP FE-SEM.

Figure 4. Low magnification InLensDuo SE (left) and BSE (right) mode micrographs of Co-Re alloy sample acquired at 1500 V acceleration voltage.

Figure 3 (left) shows a BSE micrograph image of the sample


acquired at 7 kV acceleration voltage with a conventional
below-lens BSE detector. While the and phases and voids
can be easily distinguished in this image by the typical BSE
material contrast, smaller detail cannot be discerned due to
the large interaction volume at such high primary beam
energy. Energy dispersive X-ray analysis (EDS) confirms the

Figure 5. High magnification InLensDuo SE (left) and BSE (right) mode micrographs of Co-Re alloy sample acquired at 1500 V acceleration voltage.

distribution of Re versus Co (Figure 3, right).


At very low beam energies, the backscattering coefficients
no longer monotonically increase with increasing atomic
number [3]. This behavior can be exactly reproduced with
the InLensDuo detector on this specimen (Figure 6).

Figure 3. Left: Co-Re alloy sample imaged with a below-lens BSE detector at 7 kV
acceleration voltage. Right: Co and Re EDS map of the same sample region.

References:
[1] D. Mukherji et al., Int. J. Mat. Res. 102(9):1125-1132 (2011).
[2] D. Mukherji et al., Proc. 9th Liege Conference: Materials for Advanced Power Engineering, 633-642 (2010).
[3] L. Reimer, Scanning Electron Microscopy, Springer (1998).

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Figure 6. InLensDuo BSE mode micrographs of Co-Re alloy sample surface imaged at 1500 (left), 850 (middle) and 400 V (right) acceleration voltage

At 1500 V, the Re rich phase appears bright and the Co rich

While the two signals cannot be recorded simultaneously as

phase dark, which is consistent with the magnitude of the

with a more complex solution that uses two separate InLens

electron backscatter coefficients at that beam energy.

detectors, the InLensDuo detector offers full BSE and SE

At 850 V, the backscatter coefficients are nearly identical

capability for the growing nano-materials community at a

and the contrast between the phases is strongly reduced.

competitive price.

However, inside the phase particles now subregions


become visible, indicating different compositions in these
regions. At 400 V, the backscattering coefficient and, thus,

Configuration and compatibility

the contrasts in the BSE mode image are reversed.


The ZEISS InLensDuo detector is available for the following
products: MERLIN Compact, MERLIN VP Compact. It replaces
Conclusion

the standard InLens SE detector.

In the above application example, we have shown that the


ZEISS InLensDuo detector is capable of efficiently charac-

Acknowledgements

terizing microstructure and phase distribution of a nanocomposite material by separately providing high resolution

The authors would like to thank Prof. Dr. J. Rsler

SE information and BSE compositional contrast. Taking

and Dr. D. Mukherji (Institute for Materials Science,

advantage of the backscatter yield variation at different

TU Braunschweig) for providing samples and for scientific

beam energies, the materials contrast can be precisely tuned

advice.

to collect even more compositional information.

Carl Zeiss Microscopy GmbH


07745 Jena, Germany
Materials
microscopy@zeiss.com
www.zeiss.com/microscopy
EN_42_011_036 | CZ 04-2013 | Design, scope of delivery and technical progress subject to change without notice. | Carl Zeiss Microscopy GmbH

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