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This is intended as an assistance for any
microscopist interested in doing ECCI. Despite the apparent difficulty
involved in early ECCI work [1], for a properly equipped microscope, ECCI
is remarkably easy to do. Note the important phrase, 'properly equipped';
this (I suspect) is the major reason ECCI is not as common an experimental
method as Z-contrast in the SEM. The essentials for ECCI include:
- A high brightness electron gun. (Some type of field
emitter is recommended, although for lower resolution work a LaB6
gun is sufficient.[2])
- A small beam convergence angle. I have typically used
a probe convergence angle of very approximately 6 mrad (2a).
The contrast doesn't drop off sharply for larger a,
but channeling contrast does get worse for higher a.
Joy [3] recommends a<10 mrad from a simplified
theoretical treatment, which seems a decent approximation.
- A backscattered electron detector with a large solid
angle of collection. Much of my work so far has used a polepiece mounted
Si diode detector with ~0.6p steradians.
- A clean, smooth sample surface free of preparation
artifacts. This means minimal layers of surface contamination, and no
alteration of the near-surface crystallinity through polishing, etc.
An surface that is (optically) mirror-smooth will not work if there
are sub-surface dislocations that have been introduced by polishing.
[4] (At least if you are interested in the base material instead of
the polishing artifacts.)
- Some way of collecting channeling patterns to align
your sample to the channeling contrast conditions. If your sample is
a large single crystal, than the regular scanning action of the electron
beam at low magnification will be enough to yield channeling patterns,
however most polycrystals will require selected area channeling capability
to collect selected area channeling patterns (SACPs).
- A sufficiently high probe current to resolve the channeling
contrast above the detector noise. (A rule of thumb I use is at least
1.5 nA.)
Some things which are also useful are:
- A sample stage that is eucentric for at least one tilt
axis. (This allows you to tilt to the channeling contrast conditions
without chasing the area of interest all over the sample, which gets
old fast.)
- Fine control over the stage tilt angle.
Also, I recommend:
- Avoid carbon tape, samples mounted in Bakelite/epoxy,
and other sources of hydrocarbon contamination around the sample. The
contamination that builds up on the sample surface reduces the coherency
of the beam and obscures the channeling contrast. The scan square build-up
due to the high probe currents is often considerable. I recommend mechanically
mounting the sample in some sort of vice fixture.
[5] This has the added advantage of being easily reusable.
Although historically people have used a high sample tilt
angle for ECCI, this involves some problems including foreshortening of
the image, greater constraints on sample size and maneuverability, and
some sort of custom BSE detector. The constraints come from operating
near the end of the tilt range available in most microscopes, and the
custom BSE detector because of the need to get high collection efficiencies
at high sample tilts. Typically, this involves some sort of retractable
detector that is snuggled in close to the sample surface, which in turn
restricts sample motion even further.
In contrast, I would recommend the low tilt configuration
[6], which places the sample approximately normal to the beam axis (allowing
sample sizes limited more by the chamber and stage size) and uses commercially
available polepiece mounted BSE detectors.
For whatever sample geometry chosen, the procedure is
as follows:
- Prepare your sample in such a way that there is minimal
disruption of the near-surface crystallinity. This usually
means electropolishing or chemical attack.
A further caveat is that topography must be suppressed
so as not to overwhelm the comparatively weak channeling contrast with
topographic contrast.
- Mount your sample in the microscope so as to maximize
your BSE detector collection efficiency, minimize your beam convergence
angle, and still allow room to move your sample + stage without destroying
anything.
- After aligning the microscope and adjusting your sample
to the eucentric height, choose a grain or area of interest. Collect
the channeling pattern/SACP from this region. Assuming your sample 1)
isn't heavily deformed, 2) isn't dirty, and 3) isn't overwhelmed by
topographic or Z contrast, then you will get something like figure 1.
- Tilt your crystal so that the microscope beam axis
(the center of the channeling pattern) is on the edge of the band for
your desired channeling contrast condition, as is marked by the cross
in fig. 1.
- Return to image mode (if using SACP), raise magnification,
and focus. If there are channeling contrast features to be seen under
these channeling conditions (and your contrast is sufficient), you will
have an ECC image, as exemplified in figure 2. (Note: often you will
need to use a very long frame time, or recursive filtering to bring
the image out of the noise. A very high BSE gain is essential!)
Figure 1 shows a SACP from polycrystalline g-TiAl,
covering roughly 15o of tilt; the central 10o or
so is from a single grain, while the remainder is from the surrounding
sample.
Because of the way the SACP is captured, the microscope
beam axis can be thought of as the orientation described by the center
of the SACP (indicated by the cross in the figure), so a BSE image of
this crystal formed by a beam parallel to the microscope axis would be
expected to have a greyscale intensity equivalent to the point appearing
at the center of the SACP. This is seen in the channeling contrast image
(which is simply the BSE image) taken under the channeling conditions
of figure 1.
 |
 |
| Figure 1: SACP from polycrystalline g-TiAl.
The cross indicates the approximate microscope axis. |
Figure 2: ECC images of a deformed grain of g-TiAl
taken under the contrast conditions in fig. 1. Note the dislocations
appearing as bright and dark specks in b. |
The grey level of the background in the image corresponds
to the grey level along the beam direction in the SACP. Note that for
the low magnification image (fig. 2a), the beam rock due to the scanning
action is sufficient to move the beam position far enough off the microscope
axis to change the background grey level. At low enough magnification
this is seen as a small portion of the channeling pattern. (In fig. 2a
the channeling pattern fragment is inverted and rotated relative to the
SACP. This is due to the difference in electron optics used between the
two modes.)
Copyright 2001 Benjamin Andrew Simkin
REFERENCES
| 1. |
Electron-channelling imaging in scanning electron
microscopy
P.Morin, M.Pitaval,D.Besnard,G.Fontaine, Philosophical Magazine
A, 40, 4, pp. 511-524 (1979) |
| 2. |
Electron channelling contrast imaging of interfacial
defects in strained silicon-germanium layers on silicon
A.J. Wilkinson, G.R. Anstis, J.T. Czernuszka, N.J. Long, P.B. Hirsch,
Philosophical Magazine A, 68, 1, pp. 59-80 (1993) |
| 3. |
Direct Defect Imaging in the High Resolution
SEM
D.C. Joy Mat. Res. Soc. Symp. Proc., 183, p. 199 (1990) |
| 4. |
Use of electron channelling contrast imaging
to assess near-surface mechanical damage
B.A. Simkin, M.A. Crimp, Philosophical Magazine Letters,
80, 6, pp. 395-400 (2000) |
| 5. |
Re-Usable Vice-Style SEM
Sample Holder for Pin-Mount Stages
B.A. Simkin Microscopy Today, 01-4, p. 3 (2001) |
| 6. |
An experimentally convenient configuration for
electron channelling contrast imaging
B.A. Simkin, M.A. Crimp, Ultramicroscopy, 77, pp.
65-75 (1999) |
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