HRTEM

High-resolution transmission electron microscopy (HRTEM) is an imaging mode of

the transmission electron microscope (TEM) that allows for direct imaging of the atomic
structure of the sample. HRTEM is a powerful tool to study properties of materials on the
atomic scale, such as semiconductors, metals, nanoparticles and sp2-bonded carbon (e.g.
graphene, C nanotubes). While HRTEM is often also used to refer to high resolution
scanning TEM (STEM, mostly in high angle annular dark field mode), this article
describes mainly the imaging of an object by recording the 2D spatial wave amplitude
distribution in the image plane, in analogy to a "classic" light microscope. For
disambiguation, the technique is also often referred to as phase contrast TEM. At present,
the highest point resolution realised in phase contrast TEM is around 0.5 ngstrms
(0.050 nm). At these small scales, individual atoms of a crystal and its defects can be
resolved. For 3-dimensional crystals, it may be necessary to combine several views, taken
from different angles, into a 3D map. This technique is called electron crystallography.
One of the difficulties with HRTEM is that image formation relies on phase contrast. In
phase-contrast imaging, contrast is not necessarily intuitively interpretable, as the image
is influenced by aberrations of the imaging lenses in the microscope. The largest
contributions for uncorrected instruments typically come from defocus and astigmatism.
The latter can be estimated from the so-called Thon ring pattern appearing in the Fourier
transform modulus of an image of a thin amorphous film.
What is HRTEM
HRTEM is an instrument for high-magnification studies of nanomaterials. High
resolution makes it perfect for imaging materials on the atomic scale. A main advantage
of a TEM over other microscopes is that it can simultaneously give information in real
space (in the imaging mode) and reciprocal space (in the diffraction mode). The
instrument has a single tilt stage and maximum Tilt Angle of -10 to +10o in Goinometer
and the instrument can operate in Bright-Field, Dark-Field, High resolution, SAED and
CBED modes. It has a standard probe and a variable temperature probe (100 to 500 K).
TEM is coupled with a Gatan digital camera for digital image processing. The instrument
can go upto a maximum magnification of 1.5 million. It has an ACD (anti contamination
device) working with the aid of liquid nitrogen, which helps the filament from
contamination caused by volatile sample. Depending upon the sample compatibility, it
can work at three different accelerating voltages i.e., 300, 200 and 100 kV. This has a
filament made up of LaB6. The instrument works under a vacuum in the range 10-5 to
10-6 Pa. This gives a lattice resolution of 0.14 nm and a point to point resolution of 0.12
nm.
Theory of operation
Basic principle of TEM is quite similar to their optical counterparts, the optical
microscope. The major difference is that in TEM, a focused beam of electrons instead of
light is used to "image" and achieve information about the structure and composition of

the specimen. An electron source usually named as the Gun produces a stream of
electrons which is accelerated towards the specimen using a positive electrical potential.
This stream is then focused using metal apertures and magnetic lenses called condenser
lenses into a thin, focused, monochromatic beam. Beam strikes the specimen and a part
of it gets transmitted through it. This portion of the beam is again focused using a set of
lenses called objective lenses into an image. This image is then fed down the column
through the intermediate and projector lenses, which enlarges the image, depending
upon the set magnification. A phosphor image screen is used to produce the image. The
image strikes screen and light is engendered, which enables the user to see the image. The
darker areas of the image represent the thicker or denser region of the sample (fewer
electrons were transmitted) and the lighter areas of the image represent those areas which
are thinner or less dense (more electrons were transmitted)
Image contrast and interpretation
The contrast of a HRTEM image arises from the interference in the image plane of the
electron wave with itself. Due to our inability to record the phase of an electron wave,
only the amplitude in the image plane is recorded. However, a large part of the structure
information of the sample is contained in the phase of the electron wave. In order to
detect it, the aberrations of the microscope (like defocus) have to be tuned in a way that
converts the phase of the wave at the specimen exit plane into amplitues in the image
plane.
The interaction of the electron wave with the crystallographic structure of the sample is
complex, but a qualitative idea of the interaction can readily be obtained. Each imaging
electron interacts independently with the sample. Above the sample, the wave of an
electron can be approximated as a plane wave incident on the sample surface. As it
penetrates the sample, it is attracted by the positive atomic potentials of the atom cores,
and channels along the atom columns of the crystallographic lattice (s-state model). At
the same time, the interaction between the electron wave in different atom columns leads
to Bragg diffraction. The exact description of dynamical scattering of electrons in a
sample not satisfying the WPOA (almost all real samples) still remains the holy grail of
electron microscopy. However, the physics of electron scattering and electron microscope
image formation are sufficiently well known to allow accurate simulation of electron
microscope images.

Simulated HREM images for GaN[0001]

As a result of the interaction with a crystalline sample, the electron exit wave right
below the sample e(x,u) as a function of the spatial coordinate x is a superposition of a
plane wave and a multitude of diffracted beams with different in plane spatial frequencies
u (spatial frequencies correspond to scattering angles, or distances of rays from the
optical axis in a diffraction plane). The phase change e(x,u) relative to the incident wave
peaks at the location of the atom columns. The exit wave now passes through the imaging
system of the microscope where it undergoes further phase change and interferes as the
image wave in the imaging plane (mostly a digital pixel detector like a CCD camera). It
is important to realize, that the recorded image is NOT a direct representation of the
samples crystallographic structure. For instance, high intensity might or might not
indicate the presence of an atom column in that precise location (see simulation). The
relationship between the exit wave and the image wave is a highly nonlinear one and is a
function of the aberrations of the microscope. It is described by the contrast transfer
function.

HRTEM can provide structural information at better than 0.2 nm spatial resolution. In
most crystalline inorganic materials, including ceramics, semiconductors, and metals, the
positions of individual atomic columns can be resolved, at least in low-index zones.
When recorded under optimum conditions, electron micrographs can be directly
interpreted in terms of the projected crystal potential. In other cases, image simulations
are necessary to match proposed structures to image features. Digital image recording
and quantification of diffraction pattern intensities is possible with the extreme linearity
and high DQE of a CCD camera. Dynamic events induced by the electron beam or
indirectly with a heating holder can be followed by video-tape recording from a TV-rate
image pick-up system. At lower resolution, amplitude contrast images can be used to
observe material features in the 1m-0.5nm range.
Possible Applications

distribution and structure of defects, interfaces and grain boundaries

nano-crystalline features in amorphous films
small particle analysis in heterogeneous catalysts
sub-micron morphological and device features
thermodynamic decomposition, diffusion, and phase transformations

Specimen Requirements
For highest resolution, specimens must be <10nm thick. In general, specimens prepared
by chemical thinning, crushing, or ion beam milling will contain suitable regions.
Limitations
High magnification imaging requires a high electron dose, so specimens need to be
relatively beam insensitive. The technique, by itself, provides very limited chemical
information. Heating experiments must be designed to minimize contamination of the
microscope.
Suitable Microscopes
This technique is available on the following instruments:

FEI Tecnai F20

JEOL JEM 2000FX
JEOL JEM 2010F
JEOL JEM 4000EX
Philips CM200-FEG

Topcon 002B

References
1.
2.

3.
4.
5.
6.

D.J. Smith, Reports Prog. Phys. (1997) p. 1513-1580.

P.R. Buseck, J.M. Cowley, and L. Eyring, Eds., High-Resolution Transmission
Electron Microscopy and Associated Techniques (Oxford University Press, New
York, 1988)
J.C.H. Spence, in: Experimental High Resolution Electron Microscopy (Oxford
University Press, 1988, 2nd ed.).
W.J. de Ruijter and J.K. Weiss, Ultramicroscopy 50, (1993) p. 269.
R. Sinclair, et al, Acta Crystallographica A44, 965 (1988).
P. Hirsch, et al, in: Electron Microscopy of Thin Crystals (Krieger, Malabar FLA,
1977).