Simulation of electron-matter interaction during wet-STEM electron tomography

Rahmat Firman Septiyanto, Karine Masenelli-Varlot, and Ferry Iskandar

Citation: AIP Conference Proceedings 1586, 82 (2014); doi: 10.1063/1.4866735
View online: http://dx.doi.org/10.1063/1.4866735
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Simulation of Electron-matter Interaction during wet-STEM

Electron Tomography
Rahmat Firman Septiyanto1,2*, Karine Masenelli-Varlot1, and Ferry Iskandar2
1
MATEIS, INSA-Lyon, CNRS UMR5510, F-69621, FRANCE
Physics of Electronic Material, Departement of Physics, Faculty of Mathematic and Natural Sciences, ITB Jalan
Ganesha No. 10, Bandung, Indonesia 40132
Email: karine.masenelli-varlot@insa-lyon.fr

Abstract. Tomography is an efficient tool to probe the 3 dimensional (3D) structure of materials. In the laboratory, a device
has been developed to perform electron tomography in an environmental scanning electron microscopy (ESEM). The
configuration of Scanning Transmission Electron Microscopy (STEM) in Environmental Scanning Electron Microscopy
(ESEM) provides a novel approach for the characterization of the 3D structure of materials and optimizes a compromise
between the resolution level of a few nm and the large tomogram due to the high thickness of transparency. Moreover, STEM
allows the observation in 2D of wet samples in an ESEM by finely controlling the sample temperature and the water pressure
of the sample environment. It has been recently demonstrated that it was possible to acquire image series of hydrated objects
and thus to attain 3D characterization of wet samples. In order to get reliable and quantitative data, the present study deals with
the simulation of electron-matter interactions. From such simulation on the MCM-41 material, we determine the minimum
quantity of water layer which can be detected on wet materials.
Keywords: STEM, ESEM, water layer, electrons.
PACS: 68.08.De

INTRODUCTION
Tomography is an efficient tool to probe the threedimensional structure of materials and thus better
understand the relationships between the materials
structure and their macroscopic properties. One of the
most famous applications of tomography is the material
scanner. The concept of tomography is presented for
several techniques, which are complementary. One can
cite for example X-ray tomography [1], electron
tomography in Transmission Electron Microscopy [2],
Focused Ion Beam Microscopy [3] or Atom Probe
Tomography [4]. A device to perform electron
tomography is an environmental scanning electron
microscopy (ESEM) has been developed in the
laboratory [5]. The principle of electron tomography is
based on the STEM (Scanning Transmission Electron
Microscopy) configuration and presents a new
approach for the characterization of the 3D structure of
materials. Indeed, it gives an interesting compromise
between the resolution-generally of a few tens of nm but
which can be down-and the large tomogram size due to
the large thickness of transparency.

The present study deals with a new generation of

tomographic device, which includes a Peltier stage for
the control of the sample temperature. The control of
the water environment pressure then allows the
observation of objects in suspension in liquid water [6,
7].With such device, it is now possible to acquire image
series of hydrated objects (wet-STEM tomography) [8].
When primary electrons bombard a solid sample,
they enter into the microstructure and can interact with
the positive atomic nucleus or with the electrons of the
atomic shell sample. Since the colliding particles are
charged, the interaction is governed by electro-static
Coulomb forces. Elastic scattering occurs when a
primary electron collides an atomic nucleus. This
induces a large scattering angle and a negligible loss of
energy... This phenomenon leads to the generation of
backscattered electrons. The secondary processes
coming from the energy transfer of the primary
electrons are the emission of secondary electrons, the
excitation of electron plasma in the solid, the emission
of x-rays, Auger electrons and the generation of
electron-hole pairs. They occur side by side and
simultaneously. As a result, an electron probe,
originally sharply focused in vacuum, spreads over a

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greater volume. The material and the incidence angles

of the probe electrons influence the shape and size of
this scattering volume as well as on the energy of the
primary electrons [9]. Monte Carlo simulations
determine the most accurate theoretical values for
extension and shape of scattering volume.
There are three main parts of electron tomography
technique tomo-STEM (see Fig. 1): (a) a tilting system,
(b) a system to keep the area of interest in the field of
view and (c) system of detection [5]. Although not used
during this work, we can explain them one by one: (a)
the tilting system: The large microscope chamber
allows the introduction of piezoelectric systems for
rotation over 360 around the horizontal axis; the
rotation is performed with high accuracy (typically
about 1 m). (b) The system to keep the area of interest
in the field of view: translation piezoelectric systems
are used to place the area of interest at the eucentric
position before the acquisition of the image series.
Then, the usual microscope stage movements ensure the
fine positioning of the area of interest during the
acquisition. (c) The system of detection: As for the
conditions of wet-STEM imaging [6, 8], the annular
detector for backscattered electrons collection is
removed from its position and placed below the thin
sample, for the collection of electrons scattered
(indirectly transmitted) through the sample. The Lab
View software interface allows the control of the whole
device.

Motors

METHOD
The first step is to define the chemical components
in the sample; these components can be either pure or
compound. In our work, we use either MCM-41
(chemical formula equal to silica material but different
density) covered by a water layer, or asingle material of
MCM-41 (without water layer) in the simulation.
On wet MCM-41, two components are located in the
sample, MCM-41 and liquid water. The sample
structure is used with the computation box: x = 5000
nm, y = 5000 nm, and a thickness ranging from 200 nm
to 4000 nm. The x and y dimensions of the computation
box have been chosen to avoid electrons escaping from
the x and y sides of the rectangles, by carrying out
Monte Carlo simulations on bulk materials (see figure
2 for the trajectory of Monte Carlo simulation) . For
liquid water, a precipitate is defined with a spherical
shape of radius 1000 nm and thickness equal to 10 nm,
20 nm, 30 nm, 50 nm, or 100 nm.
The paths of 100.000 electrons have been
determined and the number of electrons escaping with
angles ranging between 14 and 40 (experimental
collection angles) has been measured.

Incident e-beam
Sample

Tilting
motor

Annular
STEM
detector

FIGURE 1. STEM stage for the new electron tomography

technique combining STEM and ESEM [5, 8]

As MCM-41 had been characterized before in the

dry and wet states [8], MCM-41 has been also used for
simulations in this work.
The purpose of this work is to simulate the contrast
observed in wet-STEM tomography and to determine
the minimum quantity of water which can be detected.
Monte-Carlo simulations will be performed using a
commercial software (Hurricane software from SAMx).

FIGURE 2. Monte Carlo electron-trajectory simulation at

MCM-41 as a function of the incident beam energy 30 keV.

When the water partial pressure is experimentally

increased, then water condenses on MCM-41 sample,
which results in a contrast variation compared to what
is observed on the dry MCM-41 sample. For the
determination of the minimum thickness of water, we
have arbitrarily set that the contrast variation has to be
larger than 5%.

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RESULTS AND DISCUSSION

Minimum detectable water layer thickness on
MCM-41
Calculations of the number of electrons, collected
for different thicknesses of MCM-41, are shown in
function of the water layer thickness (see Fig. 3). For a
given water thickness, the number of collected electrons
first increases when increasing the sample thickness
since more and more electrons are scattered. Then, a
maximum is reached and when the MCM-41 sample is
thicker than 2 microns (2000 nm). The scattered angles
become larger than 40, which induces a decrease of the
number
of
collected
electrons.

FIGURE 3. Average numbers of electrons collected between

14 and 40 after having passed through a MCM-41 sample
of different thicknesses (in microns) and eventually a layer of
liquid water.

The total number of electrons coming out of sample

is slightly affected by the water layer. Therefore, it is
possible to calculate the variations of a contrast in the
images. The contrast used in the following will be
defined as the variations in the grey level from the dry
(no water layer) to the wet state (presence of a water
layer).

FIGURE 4. Expected contrast variation from the dry to the

wet state, in function of the MCM-41 matrix thickness.

The contrast variation between the dry and wet

states is shown in Figure 4. This gives information
regarding the possibility of detecting a water layer on
MCM-41.
When considering that a water layer can be detected
when the contrast variation is at least equal to 5%
(arbitrary value), a minimum water layer thickness can
be determined from Figure 4 for each MCM-41
thickness. The results are shown Figure 5. The
minimum water layer thickness which can be detected
is equal to 10 nm, 20 nm, 30 nm, and 50 nm on MCM41 thicknesses of 200 nm, 300 nm, 400 nm, and 500 nm,
respectively. Interestingly, the relation between the
minimum water thickness and the MCM-41 sample
thickness is linear (see figure 5).

FIGURE 5 Contrast Variation of MCM-41 in which is

collected electrons on the minimum water layers

CONCLUSIONS
Monte Carlo calculations have been performed to
simulate the contrast obtained during wet-STEM
experiments. The sample was composed of a MCM-41
layer of variable thickness covered by a layer of liquid
water, also of variable thickness.
The variations of the contrast between the dry and
wet states give pieces of information regarding the
possibility of detecting a water layer on MCM-A
minimum water layer which can be detected has been
determined by taking the values of thicknesses of
MCM-41 with the contrast variation had to be larger
than 5% (arbitrary value). The relation between the
minimum water thickness and the corresponding
MCM-41 sample thickness has been found to be linear.
In further works, the simulation results on MCM-41
have to be compared with the experimental tomograms
which have been acquired previously. This could help
quantifying the local water content in the sample.

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ACKNOWLEDGMENTS
We acknowledge the Institut Universitaire de
France and DIKTI for financial support.

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