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Lecture 14
Pavel Zinin
HIGP, University of Hawaii, Honolulu, USA
www.soest.hawaii.edu\~zinin
Resolution of SEM
Transmission electron microscopy (TEM) is a
microscopy technique whereby a beam of
electrons is transmitted through an ultra thin
specimen, interacting with the specimen as it
passes through. An image is formed from the
interaction of the electrons transmitted through
the specimen; the image is magnified and
focused onto an imaging device, such as a
fluorescent screen, on a layer of photographic
film, or to be detected by a sensor such as a CCD
camera.
The first TEM was built by Max Kroll and
Ernst Ruska in 1931, with this group
developing the first TEM with resolution power
greater than that of light in 1933 and the first
commercial TEM in 1939.
Positioning of signal
detectors in electron
microscope column.
magnification: X 50 to X 1,000,000
1.4 ngstom resolution (LaB6 source)
backscattered and secondary electron detectors
Gatan Digi-PEELS Electron Energy Loss Spectrometer, software and off axis
imaging camera
Kevex Quantum 10 mm2 X-ray detector (detects elements down to boron),
with spatial resolution to as little as 20 nanometers (on thin sections)
IXRF X-ray analyzer with digital imaging capability, X-ray mapping, feature
analysis and quantitative software.
Gatan Be double-tilt analytical holder for quantitative X-ray work
Gatan cryo-TEM specimen holder (to -150C)
$700,000 as currently configured at current prices
Bright Field
TEM: Imaging
Image contrast is obtained by
interaction of the electron beam
with the sample. Several contrast
effects play a role. In the resulting
TEM image denser areas and areas
containing heavier elements appear
darker due to scattering of the
electrons in the sample. In
addition, scattering from crystal
planes
introduces
diffraction
contrast. This contrast depends on
the orientation of a crystalline area
in the sample with respect to the
electron beam. Because of the high
resolution of the TEM, atomic
arrangements
in
crystalline
structures can be imaged in large
detail
http://www.phys.rug.nl/mk/research/98/hrtem_localprobe.html
Electron Diffraction
Simplified ray diagram (Abbe diagram) that shows simultaneous formation of the
diffraction pattern and the corresponding real space image in a transmission
electron microscope (TEM) (From Weirich Electron Crystallography, 235257.).
Simplified ray diagram (Abbe diagram) that shows simultaneous formation of the
diffraction pattern and the corresponding real space image in a transmission
electron microscope (TEM) (From Weirich Electron Crystallography, 235257.).
Thin Lenses;
Ray
Tracing
Refraction
1 1 1
d o di f
A Ao exp[i (ko r t )]
C
A Ao exp(iko j ) exp[i (ki ri t )]
rj
where
C
A Ao
exp i (kR) exp[i (ko k ) j ] exp(it )]
R
C
A Ao
exp[i (ko k ) j ] exp[i (k R t )]
R
r Rj
| r || R |
C
A Ao
exp[i (ko k ) j ] exp[i (k R t )]
R
k k ko
A exp[ik j ]
direct lattice
j ua vb wc
R
B
iG
A( R )
exp[ik (ua vb wc )] max
e
1
R u ,v , w
c k 2l
ak 2h
b k 2k
k (ua vb wc ) 2N
bc
ca
ab
If G is reciprocal vector a*
;b*
;c*
: G ha * kb * lc *
V
V
V
k 2G
bc sin
ac sin
ab sin
a*
; b*
; c*
2
2
a
a
a2
It is possible to show that
1
Ghkl
d hkl
The reciprocal lattice is constructed as follows:
Choose a point to be the origin in the crystal
lattice.
Let the vector normal to a set of lattice planes in
the real lattice radiate from that origin point
such that the distance of the vector is the
reciprocal of the d spacing for each family of
planes. i.e. the vector for the plane (hkl) has a
distance of 1/d(hkl) (or, more generally K/d(hkl)).
Repeat for all real lattice planes.
k 2G
Consider a set of planes determined by Miller
indices hkl, then
1
Ghkl
d hkl
2
k
2 sin hkl
2 sin hkl
1
d hkl
y
ky
Real space:
x,y,z
Reciprocal space:
kx, ky, kz
10 nm
10 nm
TEM used to determine if the graphene-based sheets were present as exfoliated sheets or
multi-layered platelets
Electron diffraction patterns and d spacings as well as high resolution TEM suggest that
platelets are individual graphene sheets randomly dispersed in the polymer matrix
High resolution TEM shows regions where fringes are observed and regions where they are
not indicating significant local curvature in the graphene sheets
S. Stankovich et al., Graphene-Based Composite Materials, Nature 442 (2006) (2006).
SEM image of the small wedge of the cBC3 phase removed by focused ion beam
(FIB) instrument.
(111)
(220)
(311)
Diffraction
pattern.
Internal
calibration provided by FIBdeposited Pt layer.
eels.kuicr.kyoto-u.ac.jp/eels.en.html
(b)
360
320
Intensity
280
240
200
160
120
280
285
290
295
300
305
310
(c)
Intensity
140
*
120
100
390
395
400
405
410
415
420
425
430
10-3 m
Head of a pin
1-2 mm
200 m
Fly ash
~ 10-20 m
Microworl
d
10-4 m
10-5 m
MicroElectroMechanical
(MEMS) devices
10 -100 m wide
0.1 mm
100 m
P
O
0.01 mm
10 m
1,000 nanometers =
1 micrometer (m)
Pollen grain
Red blood cells
O
O
Visible
10-6 m
The Challenge
1,000,000 nanometers =
1 millimeter (mm)
Infrared
Dust mite
Human hair
~ 60-120 m wide
Things Manmade
1 cm
10 mm
Microwave
Ant
~ 5 mm
10-2 m
10-8 m
~10 nm diameter
ATP synthase
0.1 m
100 nm
Ultraviolet
Nanoworl
d
10-7 m
0.01 m
10 nm
Self-assembled,
Nature-inspired structure
Many 10s of nm
Nanotube electrode
10-9 m
Soft x-ray
1 nanometer (nm)
DNA
~2-1/2 nm diameter
Atoms of
silicon
spacing 0.078
nm
10-10 m
0.1 nm
Carbon nanotube
~1.3 nm diameter
Carbon
buckyball
~1 nm
diameter
General References
Scanning Electron Microscopy and X-Ray Microanalysis, Third Edition by J. Goldstein, D.E.
Newbury, D.C. Joy, C. E. Lyman, P. Echlin, E. Lifshin, L. C. Sawyer, and J.R. Michael. Plenum
Press. 2003.
Scanning Electron Microscopy and X-Ray Microanalysis, Second Edition by Goldstein, Newbury,
Echlin, Joy, Fiori and Lifshin. Plenum Press. 1992.
Scanning Electron Microscopy and X-Ray Microanalysis, First Edition, by Goldstein, Newbury,
Echlin, Joy, Fiori and Lifshin. Plenum Press. 1981.
Electron Microprobe Analysis by S. J. B. Reed. Cambridge Univ. Press. Second edition, 1993.
Electron Microprobe Analysis and Scanning Electron Microscopy in Geology by S. J. B. Reed.
Cambridge Univ. Press. 1996.
Center for Advanced Materials Characterization in Oregon (Facilities):
http://epmalab.uoregon.edu/lecture.htm