1928 |
Shoji Nishikawa and Seishi Kikuchi The Diffraction of Cathode Rays
by Calcite. Proc. Imperial Academy (of Japan) 4 (1928) 475-477 The
first EBSP was published by S. Nishikawa and S. Kikuchi in 1928.
They directed a beam of 50 keV electrons from a gas discharge on a cleavage face of calcite at a grazing incidence of 6°. Diffraction patterns were recorded on
photographic plates placed 6.4 cm behind the crystal, normal to
the primary beam. The patterns consisted of pairs of parallel black
and white lines, and in some cases contained diffraction spots in
addition. They were similar to those patterns obtained by S. Kikuchi
in a transmission experiment on mica foils (first published in the
same volume). When the photographic plates were placed in front
of the specimen (parallel with the primary beam, as nowadays in modern "EBSD" setups), the
same type of pattern was observed as well "which must have been produced by the
electrons deflected through an angle greater than 90° ". Since
transmission and backscatter patterns were quite similiar, they
have been likewise interpreted and indexed. The relative intensities of
high-order reflections were compared with those of X-ray diffraction.
Cleavage faces of mica, topaz, zincblende and a natural face of quartz were
also tried and it was found that they give similar backscatter patterns. |
The
authors called this new type of pattern "P-pattern" (=
"black and white lines in pairs due to multiple scattering
and selective reflection") or "pattern of the fourth kind".
They have later been named "transmission
Kikuchi patterns" respectively "reflection Kikuchi patterns"
or "backscatter Kikuchi patterns". The low quality
of the first BKP may be caused by specimen contamination due to
the poor vacuum facilities at that time.
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Seishi Kikuchi and Shigeo
Nakagawa concentrated their studies on the deviation of the
lines from the exact Bragg position due to anomalous dispersion
of crossing lines and the effect of the refractive index of the
lattice on fast electrons. S.
Kikuchi and Sh. Nakagawa On the reflection of cathode rays
from single crystal surfaces. (paper in German) Sc. Pap. Inst.
Phys. Chem. Res. 21 (1933) 80-91 S. Kikuchi and Sh. Nakagawa The
anomalous reflection of fast electrons from single crystal surfaces.
(paper in German) Sc.
Pap. Inst. Phys. Chem. Res. 21 (1933)
256-265
Already
in 1928, Seishi Kikuchi grew fond of atomic physics. He published
an investigation on the mode of disintegration of Radium (J.J.Phys.
4(1928) 143.), met Werner von Heisenberg on his visit to Japan,
and joined for some time Heisenberg's team at the university of
Leipzig (Germany). Back in Japan, starting in 1934 he installed
a 600 kV Cockroft-Walton high-voltage generator, the most powerful
at that time, and a charged particle accelerator at the (now) Osaka
University Physical Science Department. Seishi Kikuchi is known as an outstanding Japanese
nuclear physicist.
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1932/33
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K. Shinohara:
Diffraction of cathode rays by single crystals. Part III. Sc.
Pap. Inst. Phys. Chem. Res. 20 (1932/33) 39-51 Kikuchi envelops are
reported in backscatter Kikuchi patterns from cleaved calcspar (calcite,
CaCO3)
at 44 keV.
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1933
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R. von Meibom and E. Rupp Wide-angle
electron diffraction. (paper in German) Z. Physik 82
(1933)
690-696 In
backscatter diffraction of fast electrons from rocksalt, sylvine,
fluorspar, diamond, calcspar and quartz crystals, dark bands (on
the photographic negative) have
been reported that are bordered on both sides by (Kikuchi)
lines. The bands were visible through acceptance angles up to 160°. The angle of beam incidence was varied between 3°
and 30°, the beam voltage from 10 kV to 40 kV. The band width
is proportional to l/d. Intensity profiles across two typical bands
are sketched. Experiment showed that the bands are formed by backscattered electrons of
virtually the same energy as the primary beam energy. The center lines
of the bands - now
called Kikuchi bands - have been indexed as zone circles sectioning
the cylindrical recording film.
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1937
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H. Boersch About bands
in electron diffraction. (paper in German) Physikalische
Zeitschrift 38 (1937) 1000-1004 Boersch studied thoroughly
- in addition to transmission - also backscatter Kikuchi patterns
(at 20 kV, about 5° of incidence and up to 162° of acceptance
angle) obtained from cleaved, polished respectively etched NaCl, KCl, PbS,
CaCO3,
CaF2,
quartz, mica, diamond, Cu and Fe surfaces.
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Backscatter Kikuchi patterns
obtained from iron (left) and fluorspar (fluorite) (right, recorded
on a cylindrical film) at 20 kV.
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He used flat photographic
plates as well as a cylindrical specimen chamber with a cylindrical
film to produce high-angle Kikuchi patterns. The angular range is
considerably larger than that obtained before in the TEM and in
present SEM appliances. The patterns are remarkably sharp and rich
in detail. The widths of the bands was found, in agreement with
Bragg's law, to be related to the energy of the incident beam and
the interplanar lattice spacings.
Boersch has discussed
the origin of Kikuchi lines, dark and bright bands and envelops
taking von Laue's dynamical theory of electron diffraction into consideration.
G.I. Finch and H. Wilman The
study of surface structures by electron diffraction. Ergebnisse
der exakten Naturwissenschaften 16 (1937) 353-436

In this
review a collection of excellent backscatter Kikuchi patterns
form a variety of single crystal cleavage faces have been presented.
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1947, 1948
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K. Artmann On the
theory of Kikuchi envelops. (paper in German) Zeitschrift
fuer Physik 124 (1947) 80-104, 154-174; 125 (1948)
27-58, 298-335 The formation of Kikuchi envelops is treated without
using the reciprocity law as well as in a rigorous wave-dynamical
treatment based on the reciprocity law, a one dimensional and a
three dimensional periodic crystal lattice. A good agreement of
both features, surface lattice envelops and crystal lattice envelops,
with experimental findings has been obtained.
(Remark: Kikuchi envelops
can have a ring shape or a parabolic appearance. Perhaps due to
the similarity with HOLZ rings of spots in transmission electron
diffraction on thin foils, the ring shaped envelops are sometimes
named "HOLZ lines" in recent publications even in
the case of BKD. One should, however, bear in mind that Kikuchi
envelops are definitively an effect of dynamical rather than
kinematical diffraction. The Ewald construction is a very useful
model for illustrating the formation of diffraction spots,
but it is not applicable for BKD. In particular, there is no
coherence between a primary beam and the diffracted beams.)
K. Artmann On the theory
of Kikuchi bands. (paper in German) Zeitschrift fuer Physik
125 (1948) 225-249 The formation of Kikuchi patterns is treated
by using the reciprocity law and solving the Schroedinger equation
for bound electrons in the three dimensional crystal potential.
This approach of dynamical theory of electron diffraction
leads to a good agreement of the intensity profile and
location of Kikuchi bands with experimental results.
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...... many publications have appeared
since then, for example:
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1954 |
M.N. Alam, M. Blackman
and D.W. Pashley High-angle Kikuchi patterns. Proceedings of the Royal
Society of London A 221 (1954) 224-242 A
cylindrical specimen chamber and camera have been used to study the high-angle
Kikuchi patterns obtained by reflexion of electrons, of energy 6 to 50 keV,
from the cleavage surfaces of crystals with the sodium chloride structure.
Angles of scattering ranging from 0 to 164° were covered. The relative
intensity of the pattern at different scattering angles was measured using a
photographic technique. The intensity distribution was found to become less
steep as the energy of the incident electrons decreased. In photographs taken
with a large value of the glancing angle of incidence, defect bands were found,
starting near the shadow edge of the pattern; these changed to excess bands at
higher angles of scattering. The most striking feature of the results is the
remarkable intensity and clarity at the highest scattering angles of the
pattern produced by crystals such as lead sulphide and potassium iodide, the
constituents of which have a relatively high elastic scattering cross-section.
In marked contrast, a relatively low intensity and low clarity was found at
these angles for lithium fluoride under the same experimental conditions. An
investigation of the width of Kikuchi bands, visible over the whole available
angular range, showed that the electrons forming these bands had the same
energy as that of the incident electrons within the experimental error of 10%.
A possible mechanism is discussed by means of which electrons can be diffused
through large angles with high efficiency, relative to small angles, and with
relatively little loss of energy. |
1973 |
J.A. Venables, C.J. Harland Video camera attached to the SEM.
They have coined the new term "EBSP" (= Electron BackScatter
Patterns) for backscatter Kikuchi patterns.. |
1987 |
D. Dingley & Link: 1st commercial system
for the SEM The
user had to identify and locate 3 zone axes on the screen, then
the program calculated the rotation matrix; feasible for cubic crystal
symmetry. |
1990 |
N.-H. Schmidt (Risų; HKL): commercial
system ("Channel") The
user had to mark interactively 3 or more bands.
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1992 |
N. Krieger Lassen, D. Juul Jensen, K. Conradsen
Automated indexing using
the Hough transform and a butterfly mask. |
1993 |
B.L. Adams, S.I. Wright "OIM":
mechanical stage scan; Burns algorithm, Hough transform. |
1994 |
Niels Krieger Lassen (PhD Thesis at Risų
and Univ. Lingby, Denmark) Thorough
investigation of the Hough transform for automated EBSD. |