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Synthesis and Reactivity in Inorganic, Metal-Organic, and Nano-Metal Chemistry (2015) 45, 323–326

Copyright © Taylor & Francis Group, LLC


ISSN: 1553-3174 print / 1553-3182 online
DOI: 10.1080/15533174.2013.831901

Transmission Electron Microscopy as Best Technique


for Characterization in Nanotechnology
MOHSEN ASADI ASADABAD and MOHAMMAD JAFARI ESKANDARI
Materials Research School, Nuclear Science and Technology Research Institute, Isfahan, I. R. Iran

Received 29 June 2013; accepted 27 July 2013

The authors summarize the applications of transmission electron microscopy in the field of nanotechnology. Transmission electron
microscopy (TEM) has represented as a very powerful instrument for studying and researching about the structure of nanomaterials
in the material science world. The quantitative measures of particle size, grain size, size distribution, size homogeneity, lattice type,
morphological information, crystallographic details, chemical composition of phases distribution, and parameters can obtain by
transmission electron micrographs. So, TEM is the best technique for characterization of the nanomaterials such as nanoparticles
and nanocomposites. Moreover, this study shows that electron diffraction pattern via the TEM is a perfect procedure for
determining the structure of materials, including perfect crystals, defect structure, and phases. The study tries to show ability of
TEM for characterization of nanomaterials.
Keywords: TEM, nanoparticles, characterization, electron diffraction, phases

Introduction 100 kV and a digital camera are used. We discuss the basic
principle and applications of the TEM in the field of nano-
Nanotechnology is considered to be the main technology for technology research. Therefore, samples of materials such as
all types of materials in the current century. For studying of nanoparticles, nanotubes, bulk metallic, grapheme, grapheme
materials in nanometer scale, investigation of nanostructures oxide, and polymer nanocomposites are investigated and dis-
is needed to discover the properties of nanostructured materi- cussed. In addition, electron diffraction pattern of several
als. However, there are many challenges in the research and materials are expounded and structure of materials are pre-
development of nanotechnology based products. The precise dicted with electron diffraction pattern results interpretation.
control of nanoparticles size, grain size, size distribution and
homogeneity, lattice type, crystal structure, dispersion, and
chemical and physical property of phases such as number,
morphology, and structure of the phases at nanolevel Transmission Electron Microscopy
needs sophisticated characterization techniques.[1,2] There-
fore, transmission electron microscopy (TEM) as best tech- TEM is a microscopy technique whereby a beam of electrons
nique for characterization in nanotechnology. The TEM has is transmitted through an ultra-thin specimen and interacts as
evolved over many years into a highly sophisticated instru- passes through the sample. The electron beam is focused on
ment that has found widespread application across the scien- strong magnetic fields and electrons are found a spiral trajec-
tific disciplines. Because the TEM has an unparalleled ability tory. An image is formed from the electrons transmitted
to provide structural and chemical information over a range through the specimen, magnified and focused on an objective
of length scales down to the level of atomic dimensions, it has lens, and appears on an imaging screen.
developed into an indispensable tool for understanding the
properties of nanostructured materials and in manipulating
their behavior.[3] Nanoparticles
In this research, an EM208S (Philips) transmission elec-
tron microscopy operating at an accelerating voltage of The size and size distribution of the nanoparticles is an
important and primary subject for its applications in different
fields. To determine the size of the nanoparticles and size
Address correspondence to Mohsen Asadi Asadabad, Materials homogeneity of particles, the images TEM can be the best
Research School, Nuclear Science and Technology Research way for understanding these subjects. Figure 1 shows the
Institute, Isfahan, I. R. Iran. E-mail: asadimohsen@gmail.com TEM image of oxide nanoparticles. This figure indicates high
Color versions of one or more of the figures in this article can be quality of synthesis method for production same nanopar-
found online at www.tandfonline.com/lsrt. ticles. TEM image also confirms the formation of
324 Asadabad and Eskandari

Nanotubes

To determine properties of the nanotubes such as diameter,


size, and their distribution, TEM analysis micrographs are
done. Also to distinguish single wall from multiwall nano-
tubes and peruse the structure of them, reaction between the
nanotubes and other element, for example, elements within
nanotube or attached to nanotube, TEM is the best way.
Figure 3a shows a carbon nanotube with different diameters.
As can be seen in Figure 3b, the diameter of the nanotube is
81.3 nm and one of the multiwall diameters is 2.18 nm.
Figure 3b pertains to a metal oxide nanotube.

Polymeric Nanocomposites

One of the most important methods to study and investigate


the nanostructure of nanocomposites and clay d-spacing is to
Fig. 1. TEM image, high homogeneity of CuO nanoparticles in the utilization of TEM method. The use of the TEM
size.

nanoparticle. Figure 1 shows a 56000£ magnification of the


CuO nanoparticles synthesis.
For particles that are size and shape polydisperse, a size
distribution can be obtained by measuring each particle
diameter with eye and hand method. The ImageTool soft-
ware is used for obtaining of size distribution. The size distri-
bution of the nanoparticles is a main parameter in synthesis.
By image analysis of TEM micrographs can predict the histo-
gram of size distribution. Figure 2 is the histogram of the
CuO nanoparticles synthesis.
This histogram for 50 of CuO nanoparticles is plotted. The
mean size distribution of the nanoparticles is almost
22.58 nm and most of the nanoparticles are in 22–24 ranges
in this histogram.

Fig. 2. The size distribution of CuO nanoparticles synthesized by Fig. 3. TEM micrographs: (a) carbon nanotubes; (b) wall of a
chemical method. metal oxide nanotube.
Transmission Electron Microscopy as Best Technique for Characterization in Nanotechnology 325

et al. as early as the 1940s.[1] Electron diffraction patterns


(DPs) are usually with TEM and are used to obtain quantita-
tive information such as the identity of phases and determine
of orientation relationships between two crystals, lattice
parameter information, exact crystallographic description of
crystals, and the structure of materials, including perfect crys-
tals, defect structure, and phases. Electron diffraction pattern
can be performed at a micro- and nanometer scale, for the
reason, this method is the best technique compared with the
other technique.

Selected Area Electron Diffraction

Electron diffraction pattern gives crystallographic informa-


tion about a material and determine different types of
materials that can be amorphous, crystalline, and polycrys-
talline. Polycrystalline materials have ring patterns that
Fig. 4. TEM image of a polymer nanocomposite. these patterns mostly used to identify of phases. Also, very
fine grains in nanoscale have ring patterns. This method
for determining nanoparticles is used. The ring patterns
create when the nanoparticle is formed. The radius of each
micrographs, structure and distribution of clay in polymer ring represents distance between the planes and set of
are studied. As can be seen in Figure 4, the clay layers in planes. Also, XRD analysis to determine the coefficients
the way of darker lines are seemed. So, exfoliation and miller for set of planes. So, XRD analyses confirm results
d-spacing of clay layers can be measured qualitatively. On of diffraction pattern in TEM. A ring diffraction pattern
the other hand, XRD data confirm as the result of TEM from a polycrystalline gold specimen is given in Figure 5.
for obtaining d-spacing of clay. As a result, this method is The interplanar spacing and lattice parameter can be calcu-
introduced as one of the important ways to getting quanti- lated with measurement the radius of each diffraction ring.
tative and qualitative values of the clay d-spacing in poly- Also, the indexing ring pattern can be performed by XRD
mer and to study of them. analysis.
In Figure 6, diffraction pattern intensity profile of gold
specimen is investigated by Diffraction-Ring-Profiler software.
Crystalline materials have a spot pattern that using this
Electron Diffraction
pattern the precipitates, twins, orientation relationship
between phases, perfect crystal, defect structure, and phases
The use of electron diffraction to solve crystallographic prob-
can be identified. Two diffraction patterns from two different
lems was pioneered in the Soviet Union by B. K. Vainshtein
points of gFe material are taken (Figure 7). Analyses of DPs
are performed by ImageTool software. With calculating the
interplanar spacing, angles, and their structures are known

Fig. 5. A ring diffraction pattern from a polycrystalline gold


specimen. Fig. 6. Diffraction pattern intensity profile of gold specimen.
326 Asadabad and Eskandari

that these patterns are related to the f.c.c structure. Also in


Figure 7b, the twin is observed.

Conclusion

TEM has represented as a very powerful instrument for


studying and researching about the structure of nano-
materials. In this article we tried to show ability of TEM
for characterization of nanomaterial. For this purpose,
several micrographs of nanomaterials were investigated
quantitatively and qualitatively. Also, examples of DPs of
different materials with various structures have been
studied.

Funding

The authors would like to thank the TEM laboratory in


Advanced Materials Group of Materials Research School
(NSTRI) for its financial supports.

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