R. A. VARIN e t al.

: Transniission Electron Microscopy Contrast 711

phys. stat. sol. (a) 34,711 (1976)

Subject classification: 1.4 and 10.1; 21.1.1

Institute of Materials Sciences ( a ) and

Institute of Mechunical Constructions ( b ) , Warsaui Technical University l )

Analysis of Transmission Electron Microscopy Contrast

at Extrinsic Grain Boundary Dislocations
BY
R. A. VARIN (a), J. A. KOZUBOWSRI
(a), M. W. GRABSRI(a), and
R. BUCZKOWSKI
(b)

Transmission electron microscopy contrast effects from extrinsic grain boundary dis-
locations (EGBDs) are investigated by computations of intensity profiles. The contrast
changes dependent on diffraction conditions and on the geometry of the EGBD line are
differentiated. On this basis the rules for the interpretation of the experimental cases are
given.
Die von fremden I(0rngrenzenversetzungen (HGV) herruhrenden, im Durchstrahlungs-
elektronenmikroskop entstehenden Kontrasteffekte werden mit Hilfe von Computer-
berechnungen der theoretischen Beugungsbilderprofile untersucht. Es werden einerseits
die von Beugungsbedingungen und andererseits die van der Geometrie der KGV-Linien
abhangigen Kontrastveranderungen unterschieden. Auf dieser Grundlage werden Richt-
linien fur die Deutung der experimentell erhaltenen Bilder der KGV gegeben.

1. Introduction
Extrinsic grain boundary dislocations (EGBD’s), i.e. dislocations produced
by the reaction of lattice dislocations with the grain boundary plane, or by other
external influences, observed with the transmission electron microscope (TEM),
generally appear as black, white or black-white lines irregularly distributed
along the boundary plane [l t o 121. Changes of diffraction conditions lead to
characteristic changes of the contrast of the lines, which are different froin
those expected from lattice didocations [ 1 , 3 , 4 , 7 , 1 0 , 1 3 ] . General rules governing
the changes of contrast from EGBD’s have been experimentallv determined by
McDonald and Ardell [9] with the method of inverting the thin foil in the
electron microscope. More recently similar results were obtained b y Varin et al.
[ 14, 151 on the basis of a syst>ematicanalysis of image contrast changes in dark
and bright field obtained from the upper and lower grains.
However, only limited studies have been made on the theoretical analysis of
the contrast expected for different diffraction conditions from EGBD with
different orientation (i.e. edge, screw, mixed) and geometry (inclination of the
dislocation line with respect. to the foil surface, orientation of the Burgers
vector with respect t o the boundary plane). The contrast profiles were calculated
by Balluffi et al. [ l G ] and Marcinkowski e t al. [ 171 for the simple case of a GBD
line parallel to the foil surface and perpendicular t o the electron beam. Tunstall
[ 181 has used computer simulated images to investigate the changes of contrast
from inclined GBD.
I ) Narbntta 85, 02-524 Warsaw, Poland.
712 R.A. VARIN,J. A. KOZUBOWSKI,
M. W. GRABSKI, and R. BIJCZKOWSKI

The main aim of this work is a theoretical analysis of changes in the EGBD
contrast for a variety of diffraction conditions and of various types of EGBD’s
with the purpose of obtaining information which can be helpful for the inter-
pretation of experimental results.

2. Experimental Procedure
The contrast profiles were computed for the cases which are most commonly
found in thin foils prepared from bulk material, i.e. EGBD inclined to the foil
surfaces. The calculations were carried out for certain r‘model’’ boundaries
(assumed axis-angle pair, orientation of the boundary plane, direction of the
EGBD line). The directions of EGBD lines and directions of their Burgers
vectors were indexed with respect t o the upper or lower grains according to the
analysed situation. The intensities of the transmitted and diffracted beams
were calculated by numerical integration of the Howie-Whelan equations
for the two-beam dynamical diffraction theory, given in a suitable form in [ 191.
A matrix approach to the description of the displacement vector R for a n
inclined dislocation in electron beam coordinates was used [ZO, 211 which is
outlined in the Appendix.2) The isotropic linear elastic approximation was
used because the symmetry of the diffraction contrast image is shown to be
invariant with respect to the degree of elastic anisotropy [22].
The foil thickness was assumed to be equal t = 8 t e and the absorption
parameters tg/& = 0.1 and 5; = 6; were taken. Computations were carried
out for three intersections of EGBD lines: one in the middle of the foil, i.e.
4tg, and the others in positions ltgand 7Ep.
It was assumed that the Burgers vectors of EGBD’s are of 4 2 (110) type,
and the crystallography and the material constants of copper were used.
For simplicity it was also assumed that the electron beam is perpendicular
to the foil surface.
The profiles computed on the computer ODRA 1204 are presented on Fig. 1
to 4. The geometrical data for the boundaries are given in captions. Full curves
refer t o the int,ensity of the transmitted beam (bright field), broken curves
refer to the intensity of the diffracted beam (dark field). The reflecting grain
is hatched.
3. Results
The results of cumputations can be divided into two groups. The first one
describes general rules governing the changes of contrast from EGBD’s independ-
ent of the orientation of dislocation, the second shows the dependence of contrast
on the orientation of EGBD.
3.1 General rules governing the contrast changes
a) The intensity profiles preserve the shape along the EGBD line (Fig. l a to
d). It should be noted that this rule is valid only when the parameter w describ-
ing the deviation from the exact Bragg condition is equal to zero for a given
vector g. For the special situation w + O , small oscillations of contrast can be
observed (see Fig. 2c for w = -2).
b) Towards the thin part of the wedge the contrast of EGBD diminishes
(Fig. l a to d , Fig. 2a to c).
z , It should be noted t h a t a similar method for the determination of the displacement
vector of an inclined dislocation has been recently used by Montheillet e t al. [23].
 Transmission Electron Microscopy Contrast a t Grain Boundary Dislocations 713

7 + + 4 L . - *
1 /- -
jd 1
I

a b c d
uu-u
-7 0 +I - I 0 +I -1 0 +I -1 a +I
XI$ -
Fig. 1. The effect of reversal of b- and g-vectors on contrast profiles of edge EGBD with
Burgers vector perpendicular to the boundary plane. Grain boundary misorientation is 39"
[Oil], boundary plane (IIO), direction of EGBD line [IIZ]. electron beam direction [OIl]
(in indices of the upper grain). a ) b, = 4 2 [IlO], gu = 111, cp = 270"; b) b, = a/2[1IO],
yu -- 111, p = 270" or b, = u p [ilo], g, = i i i , p = 90"; c ) bl = lii a/2 [ilo], gl = 111,
,.
~1 =231"; d) b , = ~ u / 2 [ l I O ] , g l = 1 1 1 , p = 2 3 1 " o r b , = ~ a a / 2 [ I 1 0 ] , g l = ~ ~ 1 , p =
= 51". M denotes the misorientation matrix, II the upper grain, 1 the lower grain

*+++I
I
\ /

p-& 1
I
- ',p ----!
I--- A --TJ

I
r+

a b C

u-u
a
0
-7 +I -1 0 +I -1 +I
"Kg -
Fig. 2. The effect, of deviation from the Bragg condition on contrast profiles of edge EGBD.
Grain boundary misorientation 45" [loo], boundary plane ( O l l ) , direction of EGBD line
[OII], electron beam directlion [OOl], Burgers vector b = a13 [ O l l ] , g = 200. a) w = 0;
b) w = +2; C) w = -2
714 R.A. VARIN,J. A. HOZUBOWSKI,
M. W. GRABSKI,and R. BUCZKOWSRI

I I I

I Y

u-
a
-7 +I -7
4%
0
- +I

Fig. 3. Contrast profiles for screw EGBD. Grain boundary misorientation 37" [OOl], bound-
ary plane (Oil), direction of EGBD line [ O l l ] , electron beam direction [OOl], Burgers vector
b = 4 2 [ O l l ] , g = 020, p = 0, w = 0 (in indices of the upper grain); in the lower grain
g = 020, p = 370, w = 0

dislacafian line

Fig. 4. Dependence of contrast profiles on the operating g-vector, w = 0 (change of p)

for edge EGBD with Burgers vector perpendicular t o the boundary plane. a, e , g ) The upper
grain diffracting; b, c, d, f ) the lower grain diffracting. Parameters used are given in
Table 1
 Transmission Electron Microscopy Contrast a t Grain Boundary Dislocations 715

n
3
0
s
0
r-
M

0.
47 physica (a) 34/2
716 R. A. VARIN,J. A. KOZUBOWSKI,
M. W. GRABSKI,and R. BUCZKOWSEI

c) If the upper grain is diffracting, the contrast in the bright-field and in

+
the dark-field images for the same diffracting vector g (BF g , D F +
g or
B F -g, D P -g) is always opposite, but if the lower grain is in diffracting
conditions, the contrast is the same (Fig. l a to d).
d ) As expected, the reversal of the direction of the Burgers vector b (for the
same g-vector) reverses the contrast without changing the profile shape. The
reversal of the direction of the g-vector gives the same results. This rule is
valid for the upper and lower grains, however, in case of the lower grain the
changes can a little increase the contrast (Fig. I d ) .
e) As expected the fulfilment of g b = 0, 9 . ( b x u) = 1 or g b = 1, -
g ( b x u)= 0 conditions for a dislocation (other than pure screw) inclined
to the electron beam does not result in any considerable weakening of contrast
(see Fig. l a , b and Fig. 2a).
f ) For positive values of the parameter w (w >
0) the contrast in both grains
is considerably weakened for both B F and DF images (Fig. 2 b for w = +2),
and a t w = + 5 the contrast disappears completely. For negative values of the
parameter w (w < 0) the contrast of the B F image is slightly weakened but in
dark field it can still be strong (see Fig. 2c for w = -2).
g) The computed intensity profiles for the situation when one grain is in
diffracting conditions (w = 0) are not affected significantly by taking into
account the weak diffraction (w= 5) in the second grain.

3.2 Effect of orientation and geometry of EGBD’s on contrast changes

a ) For pure screw EGBD the black-white contrast is observed independent
of the operating g-vector, with the exception of the case g b = 0 where the
contrast disappears (the contrast profiles for screw EGBD are shown on Fig. 3).
b) The EGBD’s with pure edge orientations and 6-vectors perpendicular or
nearly perpendicular to the boundary plane are giving black-white contrast
if the g-vector is parallel t o the projection of the EGBD line on the T E M
image (pl = 0 ) s ) . If pl increases, the contrast changes to asymmetrical black
(or white). With increasing pl the asymmetry gradually diminishes and finally
for 9 = 90” (g perpendicular t o the projection of the EGBD line on the TEM
image) the contrast is symmetrical black (or white). The sequence of these
changes is shown on Fig. 4. The changes are the same for the upper and lower
grains in diffraction conditions.
c) For EGBD’s with pure edge orientation and b-vector lying in the boundary
plane, the sequence of contrast changes with the change of q~ is similar to that
in the previous case, however contrast profiles are much more diffuse.
d ) For EGBD’s with mixed orientation the sequence of contrast changes
with pl was difficult to systematize.

4. Discussion
General rules governing the dependence of contrast on diffraction conditions
(Section 3.la to e) obtained from these calculations are in agreement with
experimental observations [ l to 121 and with theoretical computations [14 to
181. The preservation of the intensity profile shape along the EGBD line
(Section 3.la) shows the absence of “zip-zag” or “dotted” contrast effects on
EGBD’s [ l to 12, 241 which are typical for lattice dislocations.
s, The definition of the angle p is given in Fig. 7.
 Transmission Electron Microscopy Contrast at Grain Boundary Dislocations 717

The basic method of determination of lattice dislocations Burgers vectors is

-
based on the disappearance of contrast a t y b = 0. This is valid only for
screw dislocations; in case of edge dislocations additionally the g ( b x u) = 0
criterion has to be fulfilled [25]. Generally, similar conditions apply for the case
of a n EGBD perpendicular to the electron beam. However, for an edge EGBD
line inclined to the electron beam, the contrast will not disappear completely
-
even in case when both conditions, g b = 0 and g . ( b x u) = 0, are fulfilled.
It is easy to show that then the phase angle a (see Appendix) for the edge
EGBD with the Burgers vector perpendicular to the bonndary plane is

and for the edge EGBD with the Burgers vector in the boundary plane is

whereC is given by (A 13) (see Appendix) and the angle is shown on Fig. 5
and 6 (Appendix). As the phase angle a does not equal zero, the contrast
cannot vanish completely. This can explain the difficulty quoted by many
authors [l, 9, 26,271 to obtain the disappearance of EGBD contrast for the
determination of the Burgers vector with the conventional method. However,
if complete disappearance is obtained, the dislocation observed is either of
pure screw orientation or of edge orientation with the line perpendicular to the
electron beam.
On the basis of the rule given in Section 3.1 d) i t is clear that if two parallel
dislocations on the boundary plane have opposite contrast, then most probably
they also have opposite Burgers vectors. The rule in Section 3.lg) shows the
validity of the assumption that if only one grain is strongly diffracting (w = 0)
and the other one is weakly diffracting, then the second grain can be regarded in
the computations as a vacuum layer.
It should be noted, that calculations based on the assumption that both
grains are strongly diffracting (w = 0 for both grains) show important changes
of contrast as compared with the situation for two-beam conditions. The
method of the Burgers vector determination of EGBD based on the comparison
of computer simulated images with the experimental ones taken for two grains
in strong diffraction was proposed recently by Porwood and Humble [28, 291.
I n all cases in this work the directions of EGBD lines were assumed t o be
perpendicular to the direction of the intersection of the boundary plane with
the foil surface. When the EGRD line is inclined to that direction, the numerical
integration of the Howie-Whelan equations is more complicated (see Appendix),
however the resultant profile has the same shape as in the former case, only its
width is different. Because the profile width changes are produced not only by
the change of dislocation orientation but also by the changes of its geometry
estimates of the Burgers vector magnitude on the basis of image width measure-
ments only [13] are impossible.
Taking into account the complicated contrast changes of EGBD’s resulting
from changes of its geometry, and the dependence on the orientation of the dis-
location, i t is clear that the interpretation of experimental images of inclined
EGBD’s on the basis of calculations of contrast profiles for dislocations parallel
to the foil surfaces as did Marcinkowski et al. [17] is misleading.
On the basis of the rules given in Section 3.2 i t is possible t o determine the
orientation of EGBD’s in an experimental situation by appropriate choice of
47*
718 R.A. VARIN,J. A. KOZUBOWSKI,
M. W. GRABSKI, and R. B n c z ~ o w s ~ r

diffraction conditions. The method of computations given in this work has been
used for the identification of the Burgers vectors of EGBD's in Cu [ 161.

Acknowledgement
The authors would like t o express their thanks to Dr. P. H. Pumphrey for
many helpful discussions.
Appendix
A m a t r i x approach to the description of the displacement field of the extrinsic
grain boundary dislocation i n electron b e a m coordinates, and computer procedure
used i n the calculations
For the computations of contrast profiles or simulated TEM images of EGBD
the description of the displacement vector R of EGBD should be expressed in
the coordinate system connected with the electron beam.
We consider the case of a dislocation lying in the grain boundary inclined to
the foil surfaces, the foil being inclined to the electron beam. This dislocation
has the mixed orientation and the coordinate system (x"', y"', z"'), the unit
vector u of the dislocation line is parallel to the y"'-axis. Accordingly the displace-
ment vector in (x"', y"', d " ) coordinates is denoted by R"'.
By rotation of the coordinate system (XI", y"', 2"') around the y'"-axis by
a n angle x such that x"' becomes simultaneously perpendicular to electron
beam and dislocation line, we obtain a new coordinate system (x", y", 2").
The coordinate system (x', y', 2') is produced by subsequent rotation of (x", y",
z") around the x"-axis by the angle /3 to obtain the y"-axis perpendicular t o the
electron beam direction. Finally, we denote by (x, y, z ) the coordinate system
of the electron beam, the z-axis being parallel to the beam direction. The

Fig. 5 Fig. 6
Fig. 5. EGBD line lying on the grain boundary plane inclined to the foil surface, electron
beam along the z-axis
Fig. 6. Cross-sectionalong the plane given by dislocation line and electron beam (cf. Fig. 5).
n normal to the foil surface, y angle between n and electron beam, [x angle between disloca-
tion line ZL and n, a distance between dislocation line and grain boundary plane (in com-
putations a = 0 was assumed), p real distance between dislocation line and foil surface
measured along n , c effective distance between dislocation line and foil surface measured
along the electron beam
 Transmission Electron Microscopy Contrast a t Grain Boundary Dislocations 719

coordinate systems used are scheniatically shown on Fig. 5 and 6, where the
vector n1is the normal to the plane given by the dislocation line and the Burgers
vector (slip plane). For the calculation of the phase angle a we should first find
the displacement vector R of the dislocation in the coordinate system (x,y, z )
which is related to the electron beam. The displacement vector in the "new"
coordinate system is given by the transformation
A

R, = TR, , (All
where R , denotes the displacement vector in "new" coordinates, R, that in
A

"old" coordinates, and T is the transformation matrix.

We can now use ( A l ) for the situation in Fig. 5 and 6, and then we have

R" = TIR"' , (A21

A A A

R' = T,R" = T,T,R"' , (A3)

where R" is the displacement vector of the dislocation in (x",y", z") coordinates,
R' that in (x',y', 2') coordinates, F1denotes the matrix of the transformation
from (x"', y'", 3"') to ( x " , y", 2") coordinates and F2
denotes the matrix of the
transformation froin (x", y", z") to (x', y': z " ) coordinates. Knowing that the
coordinate system (x',y', z ' ) can be transformed to the beam coordinates
(x,y, z) solely by a parallel shift of the magnitude c, we can finally obtain that
the displac,ement vector R in beam coordinates is given by
A A

R = T,TIR"' . (A4)
Because in the expression given above the vector R is still expressed in terms of
(x"',y"', z " ' ) coordinates, the reverse transformation should be applied to
express (x"', y"', 2"') in terms of (x,y, z)

and
x'=x,
Y'=Y,

The transformation matrices are given by

2' = z -c. I
cosx 0 sinx

I n components of R"' the expression (A4) can be written as

720 R. A. VARIN,J. A. KOZUBOWSKI, M. W. GRABSRT,and R. BUCZIZOWSKT

Inserting the appropriate values for Ri*, R;, and R',"for the case of a mixed
dislocation [30, 311, we obtain the expression for the phase angle in its final
form
a = g . be, (A sin q cos 15 - C sin 7 sin x ) +
+ g . b e , ( - Asinqsinxsinfl+ Bcosqcosfl-
- C sin q sin fl cos x ) , (*W
where A , B , C are given [32] by the following equations:

A = tg-l X"'
-
z'"
+ 2(1 Z"'X"'
- Y ) (p2
+ xrrr2) 3

1 - 2v x'''2 - z"'2
C=
4(1 - Y )
+
In ( x " ' ~ ~"'2) + 4(1
~

- +
Y) ( z " ' ~ ~"'2) '
(A13)

e,, e , are unit vectors of the coordinate system (x, y, z ) of the electron beam.
We should note that for computations the coordinates (x"', y"', 2"') in ( A l l )
to (A13) have t o be transformed with the use of (A5)and (AG) into (z,y, z).
Because the y-vector is always in the (xy) plane, and the projection of the
EGBD line is always parallel to the y-axis (Fig. 5 and 6) we can write, in con-
sistence with Fig. 7
g . be, = ( g [b s i n v = n l , (A14a)
9 .be, = 191 b cos pl =n2. (A14b)
The angle q~ can be easily found for each experimental case.
I n case when the direction of the EGBD line is not perpendicular to the line
of intersection of the boundary plane with the foil surface, the integration limits
for x = const (i.e. for each integrated column) are changing according to the
expression
z=c+ (tgu-tg6)x, (A151
(-) integration in the upper grain, (+) integration in the lower grain, where c
i s the effective distanceof the dislocation segment from the foil surface, u denotes
the angle between the x-axis and the projection of the x-axis on the foil plane,
and 6 the angle between the x-axis and the projection of the x-axis on the
grain boundary plane. It should be pointed out that the determination of
angles x , fl, and q has to be made in a self-consistent manner.

I0 /defed

.t

Fig. 7. Definition of the angle q Fig. 8. Variation of step size of integration in

the plane crossing the dislocation line
gration procedure used was the Runge-
Kutta fourth-order process. The inte-
gration steps were chosen to be about
ategrutian
o f Howie-Whelm equations
Icompututian I,, 1,)
- procedure for
Runge-Kufta
method

1
-
1/40 t over most of the length of the
-I
column (in the foil t = 86,) but it be- infegrulion procedure for
came smaller in the vicinity of the o f Hawie-Whelm equations calculuhn
dislocation line to account for changes for bockgroundinfensi~ o f derivahver

of the displacement function j3’. Three

regions of integration along the column
J[UPh
u f mlensdy profile I

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(Received Februwy 3, 1976)