Acxc mrnll Vol. 33. No 7. pp. 1293-1305.1985 0001-616085 53.00+ 0.

00
Prmtcd I" Greal Br~tam All nghts reserved Copqrighl c 1985 Pergamon PressLtd

ELECTRON MICROSCOPY OF H.C.P. COBALT

AT VARIOUS TEMPERATURES
C. HITZENBERGER, H. P. KARNTHALER and A. KORNER
lnstitut fiir Festkiirperphysik. UniversiM Wien. Strudlhofg. 4. A-1090 Wien. Austria

(Received 24 September 1984; in revised ,form 14 December 1984)

Ahtract-In undeformed h.c.p. Co a large density of grown-in dislocations and stacking faults is observed
at room temperature. They lie on basal planes and are formed during the phase transformation when
growing the single crystals. The density of I, faults is by about two orders of magnitude larger than the
density of E faults. In-situ experiments are used to determine the stacking fault energy 7 of I, faults as
a function of temperature. In bright field images the asymmetric splitting of glide dislocations is studied,
which lie inclined to the foil; from this splitting the value of ;’ is deduced. The experimental results show
that y decreases with increasing temperature yielding a value of ‘J = 3.0 + 1.5 mJ/m’ at 425’C. and that
an increasing number of dislocations, indicating ‘J 5 0, is observed in the temperature range 430-450X.
The transformation on heating of the bulk specimen occurs at 433 +- 5’C. The very low value of ;’ which
is found near the transformation temperature agrees very well with theory. This is contrary to previous
results where even at SOO’Cthe value of y did not drop below I5 mJ/m!.

R&urn&On observe g la temptrature ambiante, dans le Co h.c. non dCformC, une forte densit de
dislocations et de dCfauts d’empilement. 11ssont situ& dans les plans de base et se ferment pendant la
transformation de phases au tours de la croissance des monocristraux. La densit de dCfauts I, est plus
grande d’environ deux ordres de grandeur que la densitt de difauts E. Nous avons determine 21l’aide
d’exp&iences in situ I’Cnergie de difaut d’empilement ; des fautes 1: en fonction de la temp&ature. Nous
ttudions la dissociation dissymitrique des dislocations glissiles en champ clair; nous en dirduisons la valeur
de 7. Nos r&ultats exp&imentaux montrent que ;’ diminue lorsqu’on augmente la temp&ature, ce qui
conduit P une valeur 7 = 3,0 + I.5 mJ/m’ P 425’C. et que I’on observe un nombre croissant de dislocations
entre 430 et 450-C. ce qui montre que ; 5 0. La transformation au tours du chauffage d’un khantillon
massif se produit d 433 + 5’C. La tris faible valeur de ;’ que I’on trouve au voisinage de la temptrature
de transformation. est en trCs bon accord avec la theorie. Ceci est contraire P des r&hats anttrieurs dans
lesquels meme i 5OO’C la valeur de y ne tombait pas au-dessous de 15 mJ/m’.

Zusammenfassung-In unverfonntem h.d.p. Co wird bei Raumtemperatur eine hohe Dichte ein-
gewachsener Versetzungen und Stapelfehler beobachtet. Sie liegen in Basisebenen und entstehen w&hrend
der Phasenumwandlung bei der Einkristallherstellung. Die Dichte der I,-Fehler ist urn ungefiihr zwei
Griilknordnungen hBher als die Dichte der E-Fehler. Durch in-siru-Experimente wird die Sta-
pelfehierenergie ;’ der I,-Fehler als Funktion der Temperatur bestimmt. In Hellfeldbildern wird die
asymmetrische Aufspaltung von Gleitversetzungen, die geneigt in der Folie liegen, untersucht und aus
dieser Aufspaltung der Wert von ;I bestimmt. Die experimentellen Ergebnisse zeigen, daD ; mit steigender
Temperatur abnimmt und bei 425’C den Wert 7 = 3.0 & 1.5 mJ,‘m? erreicht. Eine zunehmende Zahl von
Versetzungen, die 7 5 0 ergeben, wird im Temperaturbereich 430 bis 45O’C beobachtet. Beim Aufbeizen
der massiven Probe findet die Umwandlung bei 433 + 5’C statt. Der sehr niedrige Wert von ;’ nahe der
Umwandlungstemperatur stimmt sehr gut mit der Theorie tiberein. Dies steht im Gegensatz zu friiheren
Ergebnissen, in denen 7 sogar bei SOO’Cnicht unter lSmJ/m? absank.

1. INTRODUCTION value of the stacking fault energy ;’ play a main role

Pure Co has a martensitic phase transformation
(f.c.c.Mh.c.p.), and since the transformation tem-
perature T, = 420°C (mean value of heating and
cooling experiments for the bulk material) is quite
below the melting point (1495°C) it is difficult to grow
single crystals [I]. The density of the grown-in stack-
ing faults and dislocations is rather high [2,3]. The
characteristic structure of the grown-in dislocations is
caused by the phase transformation and is studied by
transmission electron microscopy (TEM) methods in
the first part of this paper.
As the phase transformation takes place between
the two close packed lattices, stacking faults and the
I293
in all the models describing this simplest case of a
martensitic transformation (for a review see [4]). To
a first approximation y should be proportional to the
difference in free energy between the two phases.
Therefore when the temperature approaches the
phase boundary, y should decrease and be zero at T,.
Contrary to this, previous TEM results report that 7
does not go below 18 mJim? at the transition point
[5]. As it is difficult to understand this disagreement,
it is also the purpose of this paper to investigate
carefully the change of y as a function of temperature.
To achieve this the non-parallel dissociation of dis-
locations inclined to the foil is studied in single
cr> stalline specimens.
1294 HITZENBERGER el al.: ELECTRON
Table I. Burgers vectors of perfecf and oartial dislocations
Perfect dislocations Pamal dislocations
a= I3~1lzo) p= l3(IToo)
c= (0001) c2=12(0001>
e+a= 13(lf23) P 2 + p = i ,6<2?03>
2. THEORETICAL ASPECTS
2.1. Low-energ), type stacking faults in the h.c.p.
lattice
In the h.c.p. lattice three kinds of low-energy type
stacking faults (i.e. they do not disturb nearest-
neighbour packing) can occur in the stacking se-
quence of the basal planes: two intrinsic faults (I, and
Ir) and one extrinsic fault (E) [6]. The faults I,, I2 and
E are bounded by partial dislocations with Burgers
vectors p + c/2. p and cj2, respectively (see Table 1).
Only I? faults but not I, and E faults can be formed
by shear since the latter have a Burgers vector with
a component lying outside the plane of the fault, In
pure Co the ratio of the lattice parameters
c/a = 1.623 (at room temperature) is very close to the
ideal value of 1.633.
2.2. Elastic constants of h.c.p. Co
The value of 7 can be determined from the dis-
sociation of the partials when the elastic constants of
Co are known. Contrary to other common metals the
elastic constants of Co are not well documented in the
literature, especially for temperatures near the phase
transformation. Fisher and Dever [7] used ultrasonic
wave velocity measurements to obtain the elastic
constants of Co in the temperature range -269’ to
+ 25O’C. At higher temperatures excessive acoustic
attenuation makes it impossible to obtain values of
the constants with the exception of c3s which was
measured up to F, and decreases about linearly.
fn the case of c,r, c,r and cu we extrapolate linearly
the values given by Fisher and Dever (cf. Table 6 and
Fig. 6 of [7]). in the case of c,,, which is proportional
to the shear modulus G measurements made by
neutron scattering are available [8]. These c’&values
are shown together with the c& values (stemming
from ultrasonic measurements [7]) in Fig. 1. The c&
0 100 200 300 400
Tf'Cl
Fig. 1. The elastic constant c,, is shown as a function of
temperature; c& and c& are taken from [8] and [7], re-
spectively. c; is extrapolated as described in the text.
MICROSCOPY OF H.C.P. COBALT
Table 2 The Isotropic elastic constants
C and 1 for the basal plane at \anous
temperatures
T( C) G(GPa) 1
IS0 69 1 0.421
300 65.4 0 430
350 63.4 0.435
423 48.7 0 465
values are higher than the cf$ ones but the difference
decreases with increasing temperature. We assume
that at lower temperatures the absolute values of c!&
are correct; for the extrapolation to higher tem-
peratures (dashed line in Fig. 1) we take into account:
(i) the sharp decrease of the CL values and (ii) the
decrease of the difference between c; and c;.
As the basal plane of h.c.p. crystals is isotropic [9]
it is convenient to use isotropic elasticity theory for
the calculation of the equilibrium separation L of
partial dislocations which lie in the basal plane. In
this plane the isotropic elastic constants G and Y
(Poisson’s ratio) were determined using the formula
161.
Gp’ (2 - r)
;‘L =-
*n -(l-F)
assuming two different values for 6 (character of the
total dislocation measured from screw to edge) since
yt can also be determined within the framework of
the anisotropic elasticity theory [IO, 1I] using the
above mentioned constants. In Table 2 the values of
G and 1’are given for different temperatures.
2.3. The ecaluation of y from the shape of inclined
dislocations showing non -parallel dissociation
From the splitting width of the Shockley partials
the value of 7 can be determined rather directly. To
resolve the parallel partials in Co at room tem-
perature it is necessary to apply the weak-beam
method of TEM, and exposure times of about 30s.
have to be used; from the splitting width of the
partials 7 = 27 k 4 ml/m’ is deduced [12]. The rather
low stability of the heating holder, the single tilt and
the magnetic properties of Co made it necessary to
use a different method to evaluate y from the in situ
heating experiments. Glide dislocations which are
inclined to the foil have a characteristic non-parallel
dissociation of their partials [13]. In this case the
partials can be resolved even by bright field images,
since their splitting at the surface can be several times
larger than the splitting width of dislocations which
lie parallel to the foil. Therefore it is possible to
evaluate 7 by comparing the observed non-parallel
configurations with calculated ones. To find the
equilibrium configuration the energy minimum of the
whole configuration (partials and stacking fault) is
determined [ 131. Several assumptions which facilitate
the calculation are made: (i) the partials are assumed
to be straight, (ii) interaction image forces are
neglected, (iii) the glide plane is assumed to be
 HITZENBERGER et al.: ELECTRON
---ST-- --d- -“-A-- b0ttomsecond step the crystal is passed over the phase
30 66 191
150 300 425 TPC]
13 8 3 7 [mJ/m*] either parallel to the basal plane or 30” inclined to it.
Fig. 2. Examples of calculated equilibrium configurations of
dissociated dislocations which lie on a glide plane perpendic- (33% H2S04 and 67% H,O at room temperature), and
ular to the foil. In this case the shortest line of the
dislocation is equal to the foil thickness and is taken 250 nm. 99% CH,OH was used at -70°C. Discs which have
Dislocations tiih different initial 6, (0, 30, 60 and 90”) are
considered. Three cases of different values of Y (13, 8 and
3 mJ/m’) are shown using the appropriate elasiic‘constants
(corresponding to 150, 300 and 425°C respectively). The
hatched regions mark the I2 faults. The splitting widths at
both surfaces of the foil and the inclination of the partials
are indicated.
perpendicular to the foil and (iv) surface relaxations
bending the TEM foil are ignored.
Figure 2 shows some examples of calculated equi-
librium configurations of dissociated dislocations
which lie on a glide plane perpendicular to the foil.
Dislocations with different initial character 6, = 0,30,
60 and 90” are considered (6, is the angle between the
Burgers vector of the total dislocation and the short-
est line in the glide plane). The elastic constants given
in Table 2 are used for the temperatures 150, 300 and
425°C; the value of y is assumed to be 13, 8 and
3mJ/m*, respectively. The shortest line of the dis-
location is taken 250 nm. The splitting widths at the
top and bottom surface of the foil are indicated (e.g.
L, = 22 and L2 = 0.25 nm, respectively). The inclina-
tion between the partials and the shortest line is also
shown (e.g. -2.5 and -2.5”, respectively). For the
calculation the lattice parameter a = 0.25071 nm [7]
and the outer cut-off radius R = 1 pm are used and
it is assumed that the minimum separation of the
partials is identical with the lattice parameter a.
MICROSCOPY OF H.C.P. COBALT 1295
3. EXPERIMENTAL PROCEDURE
The single crystals were grown from polycrystalline
rods (70 mm long, 5 mm dia; purity 5 N) supplied by
Johnson, Mathey Ltd. The phase transformation
makes it difficult to grow single crystals, which are
more than 20mm long. To achieve this a modified
Bridgman technique was applied [l]. A “soft” mould
of A&O, is used, and in a first step a f.c.c. single
crystal is grown under vacuum ( < 10m3Pa) at a speed
of 60 mm/h and afterwards cyclically annealed for
about 50 h to reduce the dislocation density. In a
transfo~ation from about 1400°C to room tem-
perature at a speed of 30mm/h. This takes into
account that the chances to get a h.c.p. crystal are
better when the temperature gradient is large during
the phase transformation [ 141. In our case the proba-
bility to get a single crystal of more than 50mm
length was about 10%. Additionally to these crystals
one crystal which was made by the Czochralski
method and supplied by Metals Research Ltd
(Cambridge, England) was used in this study.
It should be pointed out that only one crystal was
deformed in tension (see Section 4.2.2.), all others
were investigated in the as-grown state.
Using a spark cutter the crystals were sectioned
TEM foils were prepared by standard jet technique
for the final polishing a solution of 1% HClO,, and
a diameter of only 1 mm were made to reduce the
astigmatism. The foils were examined at 100 kV in a
Philips EM 300; a double tilt holder was used at room
temperature and a single tilt heating holder for the
annealing experiments. In this case the temperature
was measured using a thermocouple supplied with the
holder and calibrated by Philips. It is difficult to judge
the temperature of the specimen since it might be
lower (about 3-5°C) than the one of the thermo-
couple; but it is safe to assume that the relative
temperatures are correct.
4. EXPERIMENTAL RESULTS
The grown-in dislocation structure of undeformed
crystals is studied at room temperature. Figure 3
shows a foil parallel to the basal plane. The density
of the grown-in dislocations is rather high:
2 t_ 1.5 +lO”/m*, and has a large range of scatter; Fig.
3 shows an area with a relatively high density (about
3.4. 10L3/m2). The grown-in dislocations lie in the
basal plane and are arranged in bundles and net-
works. The networks contain several straight dis-
locations, which lie along (1120) and are sessile
partial dislocations (p f e/2). Some glide dislocations
(marked with G) are observed in the neighbourhood
of the networks. It should be mentioned that in foils
1296 HITZENBERGER FI a/.: ELECTRON MICROSCOPY OF H.C.P. COBALT

Fig. 3. Grown-in dislocation structure of undeformed h.c.p. Co at room temperature. The foil plane is
parallel to the basal plane.

oriented parallel to prism planes only very few, short
dislocations not lying in the basal plane (with Burgers
vector c) have been encountered [3].
Figure 4 shows a foil which is inclined at 30” to the
basal plane. The stacking faults are in contrast; they
are of type I, and bounded by partial dislocs
which he often along (1120) (cf. at A). A few glide
dislocations G are also observed.
Figure 5 shows an area which contains I, a.nd E
faults. In Fig. 5(a) (g = [Oil 11) two E fault s are
 HITZENBERGER et ul.: ELECTROT MICROSCOPY OF H.C.P. COBALT

(b)

Fig. 4. Undeformed Co at room temperature; foil plane

inclined at 30 to basal plane. Several I, faults are imaged;
they are frequently bounded by straight partials parallel lo
(I 120) cf. at A.

Cc)
Fig. 5. Undeformed Co: foil plane inclined at 30. to basal
plane. (a) I, faults and two E faults are imaged (g = [OTI I]:
RT). (b) The E faults are out of contrast (g = [oTII]; RT).
(c) When the temperature is increased one of the E faults
transforms into an I, fault (g = [OTIS]; T = 314 C).

imaged. In Fig. 5(b) (g = [OT12]) they are out of

contrast since their shear vector R = c/2. The faint
fringes which are difficult to avoid in this reflection
can arise from the excitation of nonsystematic
reflections. It car. be excluded that the faint contrast
of the narrow fringes is caused by an additional
distortion of the fault as described by Brooks et al.
[15] since in this case the width of the fringes should
be the same as the one of the other faults. Figure S(c)
(g = [0112], T = 314’C) illustrates the transformation
of an E fault into an I, fault (although this micro-
graph is taken from an annealing experiment it is
(a) included here). One of the E faults [cf. Fig. 5(b)] has
1298 HITZENBERGER e! al.: ELECTRON MICROSCOPY OF H.C.P. COBALT

reacted with a p partial and transformed into an I,

fault.
The density of I, faults is in the range 1 to 4.106/m;
whereas the density of E faults is by about two orders
of magnitude lower.

4.2. Annealing experiments

4.2.1. Basal plane inclined at 30 to the foil plane
4.2.1. I. Dislocations with initial character 0, = 30”.
Figure 6 (a, b and c) show the same area in an in situ

Fig. 6. Undeformed Co; foil plane inclined at 30 to basal

plane; heating series. I, faults and glide dislocations (initial
character B02 30 ) are imaged. With increasing temperature
their dissociation width increases. (a) 150 C; the 1: faults
bounded by the partials of the glide dislocations are clearly
visible in (b) (3Oo’C) and (c) (425-C).

annealing experiment. The I, faults remain un-

changed whereas the dissociation of the glide
dislocations (I, faults) increases with increasing
temperature. The value of y can be determined by a
comparison with the calculated shapes (cf. Fig. 2). In
Fig. 6(a) (15O’C) the increased dissociation (at one
surface) is just visible: L, = 20 k 5 nm which leads to
y = 13.3 f 1.8mJ/m’. In Fig. 6(b) (300 C) the
I2 faults are clearly visible, the partials bounding
them are rather straight: L, = 56 + 14 nm yields
y = 7.0 k I .2 mJ/m*. The dislocation marked with X
behaves differently. It seems to be hindered by some
obstacle, therefore it was not taken into account. In
Fig. 6(c) the temperature (425°C) is close to the
transformation temperature on heating (Trh); L, =
94 + 24 nm is observed leading to 7 = 3.1 + 0.7 mJ/
m2. The dislocation X shows a normal behaviour
indicating that the obstacle was overcome.
At r,,, = 433 + 5°C the phase transformation takes
place in the thick (bulk) regions of the specimen (it
might correspond to the bulk material since the outer
rim of the specimen is about 0.2-0.3 mm thick). This
transformation is always connected with vigorous
vibrations of the TEM image and a large deflection
of the zero order beam, which is caused by the change
of the magnetic properties.
Figure 7 shows an area close to the one of Fig. 6;
the micrograph was taken at a temperature of 43O’C,
(b) which is about 2’ above Tth of the bulk specimen in
 HITZENBERGER PI al.: ELECTRON
Fig. 7. Undeformed Co; foil plane inclined at 30’ to basal
plane; T = 430 C (2. above the bulk transition temperature
of this specimen). The dislocations (A and B) bounding Iz
faults show a different behaviour. A is undissociated at one
foil surface while B is split at both surfaces (the latter
indicates ;’ I 0). The splitting width increased during the
exposure time.
this case. The dislocations bounding the I2 faults
show a different behaviour. At A the partials are still
closed at one surface; from the dissociation at
the other surface L, = 140 +_ 1Onm the value
7 = 0.2 f 0.2 mJ/ m* can be deduced. Whereas at B
the partials are widely separated and the dissociation
width doubled during the exposure time; this leads to
y I 0 mJ/m*. The different behaviour at A and B
could be caused by the contamination (oxide) layer
which forms during the annealing (cf. the light spots).
It could also account for the discontinuous expansion
of the I1 fault at B. The dissociation of the partials
of the dipole D which lies near screw orientation is
very small even when y * 0, which is in agreement
with theory [16].
4.2.1.2. Dislocations with initial character 0, = 60”.
Figure 8 shows an annealing series. As the reflection
g = k [IO'fI] is used the glide dislocations
(b = + 1/3[1210]) show a residual contrast, which is
relatively strong. In Fig. 8(a) (room temperature) the
glide dislocations deviate by an angle of about
22 f 6 ’ from the shortest line in the slip plane (which
is perpendicular to the fringes of the fault). The
MICROSCOPY OF H.C.P. COBALT 1299
Table 3. Values of 7 at diRerent temperatures
T( C) 7&J/m’) ___. ;&J:m2)
~__.___
310 6.1 i 2.2 (L2 below resolution)
425 2.9 + I .l 2.3 i 2.1
430 0.2 0.2
455 0.1 * 0.1 0.1 f 0.1
y is deduced from the dissociation of dislocations with 0, = 60 (cf.
Fig. 8) at both foil surfaces (L, and L,. respectively)
Table 4. Values of 7 at 425-C deduced from
dislocations with different 0,
0” y,,(mJ/m’) y,+J/m2)
0 2.7 * 1.7 (No dissociation)
30. 3.1 20.7 (No dissociation)
60 2.9 k 1.7 2.3 ?r 2.7
90 1.9* 1.1 5.1 f 1.2
experimental result is in good agreement with the
calculated equilibrium position where this angle is
22”. In Fig. 8(b) (215°C) the dissociation of the
partials is just visible at the surface and it increases
when the temperature is increased [cf. Fig. 8(c)
(307°C) and Fig. 8(d) (426”(Z)]. Figure 8(a)-(d) and
(f) show the same area (cf. the mark A) whereas in
Fig. 8(e) the area is slightly moved out of place. In
Fig. 8(e) (430°C) the temperature is just below T,h
(434°C) of the bulk specimen in this case. In Fig. 8(f)
(455°C) the value of y in the h.c.p. structure should
be below zero and the I2 faults should therefore
expand through the whole crystal. This is not the case
in Fig. 8(f), the reason might be that in the thin foil
the movement of the partials can be hindered by
surface contamination.
The results of Fig. 8 are summarized in Table 3.
From the observed values L, and L2 the values yL,
and yL2are deduced, respectively.
4.2.1.3. Dislocations with initial character 0, = 0
and 90”. At 425°C (just below Tth) micrographs were
taken of dislocations with B,,= 0 and 90”, re-
spectively. When screw dislocations (0, = 0’) lie along
the shortest line in the glide plane, they dissociate at
one surface only (cf. Fig. 2). In the case of edge
dislocations the partials dissociate at both surfaces
and are frequently bent.
The values of y which were deduced for 425°C are
given in Table 4. The agreement of the y values
corresponding to the different values of 0, is quite
good. When 0, = 90” the values of yr, and yL2 are
different; the reason might be that the partials are not
straight as assumed in the calculation.
4.2.2. Basal plane parallel to the foil plane
Figure 9 shows an annealing experiment of a
crystal which had been deformed in tension (90%
resolved shear strain). In Fig. 9(a) the area is imaged
at room temperature whereas in Fig. 9(b) the tem-
perature (42 1“C) is close to T, and the dissociation of
the glide dislocations is clearly visible. They are
frequently constricted (e.g. jogged); some of the
constrictions are marked with arrows. From the
observed dissociation width and taking into account
1300 HITZENBERGER Ed al.: ELECTRON MICROSCOPY OF H.C.P. COBALT

(b)
Fig. 8(a)-(b)
HITZENBERGER et al.: ELECTRON MICROSCOPY OF H.C.P. COBALT

Fig. 8(c)-(d)
1302 HITZENBERGER et al.: ELECTRON MICROSCOPY OF H.C.P. COBALT

Fig. 8. Undeformed Co; foil plane inclined at 30’ to basal plane; heating series. Some glide dislocations
with &,h 60’ are imaged. With increasing temperature the splitting width increases. The point marked
A is the same in {a)-(d) and (f). The area of(e) has moved slightly out of place. The bulk transition took
place between (e) and (f). (a) RT, (b) 215’C. (c) 307-C. (d) 426 C. (e) 430 C, (f) 455 C.

(b)
Fig. 9. Co, deformed 90% in tension; foil plane parallel to basal plane. Several glide dislocations are
imaged. (a) RT, (b) 421 ‘C, the dissociation of the dislocations can be seen. They are frequently jogged.
some of the jogs are indicated with arrows.
 HITZENBERGER er al.: ELECTRON
the character of the dislocations (using this and other
areas) the value of ; was determined leading to
7 = 3.0 + I .5 mJ ‘m’.
5. DBCL’SSION
5.1. Srructure qf he grown-in dislocations and
stacking fuui!s
The dislocation density of undeformed Co crystals
is rather high (cf. section 4. I) and corresponds to the
one of f.c.c. crystals deformed into stage II of the
work-hardening curve. The structure of the grown-in
dislocations and stacking faults is the same in both
Czochralski and Bridgman grown crystals and agrees
with the one observed by Thieringer [Z]; except the E
faults which were not analyzed by Thieringer. The
formation of the grown-in dislocation structure can
be explained in the following way (21: during the
phase transformation (f.c.c.+ h.c.p.) partial dis-
locations which lie in the plane of the transition move
through a network of dislocations iying on inclined
{I 113 planes. At the phase boundary mainIy two
reactions can occur:
p, + (c,‘2 -t pz) = (c:‘2- pJ (1)
p, + (c/2 - p,) = c:2
(2)
The h.c.p. notation is used and therefore the glide
dislocations in the f.c.c. lattice are of type D = (p?- p,)
(on the transition plane) and (c,‘2 + p) on the inclined
{111f planes.
The dislocations resulting from reactions (1) and
(2) lie along the trace of inclined (111) planes with the
transition (basal) plane. i.e. along (1120). The obser-
vations seem to confirm this since the partials bound-
ing I, faults are frequently along (1120) (cf. Fig. 3).
Reaction (I) leads to the formation of i, faults
whereas (2) leads to a fault with shear c/2. Thieringer
assumes that this fault has a stacking sequence of
ABAABA (i.e. a high energy fault) and reacts imme-
diately with a p dislocation. and an I, fault is formed.
However the formation of an E fault is equally
possible.
The different densities of I, and E faults (cf. section
4.1) can be explained in the following way. Firstly the
lower density of E faults corresponds. to their lower
formation probability. For a given p dislocation (e.g.
p,) there is only one (c/2 + p) dislocation [i.e.
(c/2 - p,)] which leads to reaction (2) forming a c/2
fault. On the other hand I, faults are formed by
reaction (1) in two cases [i.e. (c/2 + p.,) and (42 + pJ]
and preserved in three cases [i.e. (c/2 + p,), (c/2 - p2)
and (c/2 - p3)]. Therefore I, faults are formed in five
eases, whereas c/2 faults in one case only. If every
other r/t fault is a high energy fault which transforms
into ft by spontaneous nucleation and shear of a p
dislocation, the density of E faults should be an order
of magnitude lower than the one of I, faults. Second-
ly, as shown in Fig. 5(b), E faults can react with a p
dislocation and transform into I, thus reducing their
MlCROSCOPY OF H.C.P. COBALT 1303
Table 5. Final results of ; at
difkrcnr temperatures
WC) y(mJ ,m’)
150 13.3 * 1.8
300 7.3 5 2.5
425 3.0 * 1.5
430-450 50
The value of ;’ given for 1SO’C is a
lower boundary. The transition
temperature on heating of the
bulk specimen is 433 + YC.
In the temperature range
430-45O.C an mcrcasing num-
ber of dkxations shows y d 0
with increasing temperature.
energy. (This has been reported recently fl?]). We
assume that this process which is sometimes observed
on heating can happen quite frequently near the
phase boundary below the transformation tem-
perature where many mobile p partials should be
available for the reaction to take place. Therefore it
can be understood that the densities of 2, and E faults
differ by about two orders of magnitude.
5.2. The measurement ofthe stacking fault energy y us
a function of temperature
5.2. I. Room temperature to transition temperature.
The value of 7 was determined by comparing the
calculated asymmetric dislocation configurations
with the observed ones (e.g. Fig. 2 and Fig. 6,
~s~ctiveIy}. The parameters of the calculations were
varied on such a fine scale that any errors arising this
way are far below the experimental errors. The main
difficulty is caused by the assumption made in the
calculations that the partials are straight. Contrary to
this the observed partials are frequently bent, es-
pecially in the case of 8, = 60 and 90’ where the
partials have a character near edge orientation and
therefore a low line tension [6]. This might be the
main reason for the large scatter of the y values
shown in Table 3 (dislocations which are obviously
jogged were excluded from the consideration). In the
case of (3,= 0 and 30’ the observed partials are rather
straight since their line tension is high. They are split
at one surface only and thus the probability of being
hindered by some obstacles in achieving their equi-
librium configuration is less. Also the inftuence of any
uncertainties of the elastic constants (cf. section 2.2)
is smaller. Therefore the scatter of y shown in
Table 4 is less for 6, = 0 and 30’ than for $ = 60 and
90’. respectively.
The final result is shown in Table 5. The y values
are taken from dislocations with &, i= 0 and 30”.
Dislocations with 0,= 0’ were observed in rather
thick regions of the specimens only, where the in-
crease of the splitting width is small; therefore they
were mainly used at temperatures above 300°C. The
value given for 150°C is a lower boundary since the
observed dislocations are not straight. Above 400°C
the parallel dissociation of the partials in (0001) foils
was also analysed. The y values deduced from parallel
I304 HITZENBERGER cl al.: ELECTRON
and asymmetric dissociation agree very well and seem
to justify the simplified assumptions made in section
2.3. This is confirmed by recent calculations showing
that the inclination of the glide plane to the foil plane
is important below 10. only. where the interaction
image forces tend to reduce the splitting width [18].
In our case this angle is 30’ and therefore the effect
can be ignored.
5.2.2. Above the transition temperature. Around
and above the transition temperature on heating (T,,,)
of the bulk specimen (mean value at 2 433’C) the
following typical observations are made: An in-
creasing number of dislocations shows a very wide
dissociation in the temperature range 430-450°C
indicating y I 0 (cf. Fig. 7, dislocation B). Some
dislocations show even up to 5 45O’C the same finite
splitting width as below the transformation which
would correspond to 7 z 0.2-3.0 mJ/m’ [cf. Fig. 8(f),
dislocation B]. This observation is independent of 0,
and it is the same in (0001) foils. A possible expla-
nation for this different behaviour could be the
influence of obstacles (jogs) on the moving partials.
In the case of inclined dislocations a localized surface
contamination (e.g. oxidation, cf. Fig. 7) can hinder
the partials to reach the equilibrium configuration.
The effect will be more pronounced when y and
therefore the driving force is low. In the case of (0001)
foils the splitting width can be reduced by the inter-
action with other dislocations of the same sign (cf.
Fig. 9). It should be mentioned that when the tem-
perature is reduced similar effects are observed, i.e.
some dislocations recontract at temperatures below
400°C.
Above Tth the number of the stacking faults in-
creases rapidly, they mostly extend from the thicker
30.
25
r “:
5 20
b
IL : i
1!5-
ZI
0
lo-
5- + shape and do not lie on a specific glide plane. This
$ indicates that most of the dislocations observed in
O- 1 *
1 The glide of the p partials on every other basal plane
2bo 3ho b 4&o a dot
0 ’ lb0 *
Fig. 10.Stacking fault energy ;’as a function of temperature.
0 Results of this paper (the value at RT is from [IZ]).
q Results from [5]. The broken lines continuing the error
bars indicate that at ISO’C the value of 7 is a lower
boundary and that near the transition temperature the
results of individual dislocations deviate considerably from
the mean value.
MICROSCOPY OF H.C.P. COBALT
regions (bulk) of the specimen into the thin foil. If;
is negative the energy gain of the expanding II faults
is proportional to their area and therefore larger in
the thick regions than in the thin foil: the same is true
for their ability to overcome obstacles,
5.2.3. Comparison with previous results. Values of;
as a function of temperature are summarized in [l9)
for various metals and alloys; more recent in-
vestigations of Cu- and Ag-alloys are given in
[20,21]. For a comparison with the results presented
here only measurements of metals showing a phase
transition f.c.c.++h.c.p. are of interest. They were
carried out in the case of pure Co [5] and CoNi [5, 191
using the dislocation-node method. In both cases ;
does not extrapolate to zero at r, (7 2 l0mJ m’).
In Fig. 10 our results of 7 are compared with the
ones of Ericsson [5]. Although Ericsson finds a
decrease of y with increasing temperature, ;’ has a
value of ‘c 18 mJ/m’ at r, and even at 500 C it does
not drop below 15 mJ/m’. We tried to analyse the
micrographs published in [5] where one can find I:
faults showing the typical triangular shape indicating
0, z 30’ and yielding 7 2 5 mJ:m’ at 37O’C, which
agrees well with our results. Most of the dislocations
however seem to be heavily jogged which hinders
their dissociation and could account for the
high value of 7 given by Ericsson. Therefore the
value of d;,/dT (mean value in the temperature
range 20425C) is - 0.07 + 0.01 mJ ‘m’K and
-0.03 k 0.02 mJ/m’K deduced from this experiment
and the one by Ericsson. respectively. (They cannot
be compared with theory since no value of the
entropy of a stacking fault is given in the literature.
at least to our knowledge.)
5.3. The phase transition
Although no direct evidence of the mechanism of
the phase transition is observed some information
can be deduced from the experimental results.
The observed structure of the grown-in dis-
locations can be explained in principle (cf. section
5.1); yet the high density of the dislocations is not
immediately clear. It can be assumed that the density
of the grown-in dislocations in the f.c.c. Co crystals
is about the same as in Ni crystals, i.e. about 4.109:mZ
[22], since Ni has almost the same melting point and
the crystals were made in the same way. Also these
dislocations are heavily jogged, have an irregular
Fig. 3 are formed during the phase transformation.
leads to a deformation of the transformed region.
Therefore stresses are exerted on the untransformed
matrix and this can effect the activation of glide
dislocations in the f.c.c. lattice near the phase bound-
at-y. They will react with the p dislocations yielding
the observed sessile (c/2 + p) partials. Therefore the
grown-in dislocations can be explained by a partial
dislocation mechanism.
 HITZEKBERGER et Ql.: ELECTRON MICROSCOPY OF H.C.P. COBALT
The annealing experiments show the result that 7
is very low at T,. This agrees with the models of the
transfo~at~~~ which are based on the assumption
that ;’ corresponds to the energy difference of the two
structures {e.g. the pole dislocation mechanism pro-
posed by Seeger [23] or the modeIs assumiu~ the
nucleation of partials at a boundary [24,25]). From
the present experiments it cannot be concluded which
model is correct. The transformation of the thin foil
is not comptete which agrees with the pole dislocation
model since the probability to find a pofe dislocation
in a thin foil is extremety low; on the other hand the
result agrees afso with a boundary model if one
assumes that the tra~sfo~in~ partials are not rtucte-
ated at a stress-free surface. On the whole we are
slightly in favour of a model where the boundary is
under stress since in this case the grown-in dis-
locations would be part of the mechanism and not
just obstacles for the moving partiafs. The im-
portance of stresses for a martensitic phase trans-
formation has recently been observed by Riihle and
Kriven [26] using TEXS methods.
FinaJJy it should be mentioned that the experi-
ments show 7 IT 0 at T,,,, whereas from the theory one
would expect 7 2 0 at r, (where Tth > T,, caused by
the hysteresis). The reason for the positive value of y
which is deduced at 425’C (about T,) could be that
the partiafs do not reach the e4u~Ji~~~~rnposition (cf.
section S.2.2.).
Ackno,r~ledgemanrs-The authors would like to thank Pro-
fessor Dr F. Stangler for the provision of laboratory
facilities. Financial assistance from the Austrian “Fends zur
Fiirderung der ~j$~n~haftJich~ For~b~u8 in &err&%”
is acknowledged.
Note added in proof-A detailed anaiysis of the contrast of
intrinsic and extrinsit stacking faults in h.c.p. Co will be
given in PhJ,sicu SIUIUSsolidi (a). Vol. 89 (1985).
1305
REFERENCES
H. M. Thieringer, Z. ~~f~~~~.59, 400 (1968).
: W. M. Thieringer, Z. ~erff~~~.59, 476 (1968).
3:C. Hitzenberger* Ph.D. thesis, University of Vienna
(1982).
4. J. Singh and S. Rangaoathan. ~~~si~u S~QIEG
solidi (a)
73, 243 (1981).
5. T. Ericsson, Acln metali. 14, 853 (1966).
6. J. P. Hirth and I. Lothe, ?%eog of Dislocufions, 2nd
edn. Wiley. New York (1982).
7. E, S. Fisher and D. Ilever, Trans. Am. Inst. Min. Enps
X39,48 (196-O.
8. F. Frey, W. PrandI, J. Schneider. C. &yen and K.
Ziebeck, .& Phys. f. ?* 603 (1979).
9. A. Seeger and G. Scftoeck, &‘Fff ~~fu~~. f, 519 (1953).
10. A. N. Stroh, Phil. ,Wag.3, 625 (1958).
Il. A. K. Head, P. Humble, L. M, C~a~~brou8h, A. J.
Morton and C. T. Forwood. Computer Electran Micro-
graphs and Dejecr Identification. North-Holland, Am-
sterdam (1973).
12, A. Korner and H. P. Kamtbaler. Phil. Mug. A 48,459
(1983).
13. P. M. Hazzledine, H. P. Ka~tha~~ and E. Wintrier,
Phil. Mffg. 32, 81 (1975).
14. K. J. Bachmann and T. Wakiyama, J. Opt. Grow& 3i?,
327 (1975).
J. W. Brooks, H. M. Loretto and R. E, Smallman, Acta
metali. 27, 1839 (1979).
E. Wintner and H. P. Kamthaler, Phi/. Mug. 36, 1317
(1977).
C. Hitzenbcrger and H, P. Kamthaler, &xx. Tewh Inr.
Coffp. on Electron N&r., ~ambur8* Vol. 2,535 (1932).
P. M. Hazztcdine and S. J, Shaibani, Srrengrh 01
Metals and Allqrs (K&WA 6). Pram. Sixth Inr. Corz+K~
Melbourne, Australia, Vol. f, p. 45 11982).
19. L. Remy, A, Pineau and 8. Thomas, Murer. Sri. Eegng
36,47 (1978).
20. H. Saks, Y. Sueki and 7. imura. Phi!. Msg. A 3’7, 273
(1978).
21, H. Saks, T. Kondo and T. Imura. Phil. Maa. A 47,8J9
v
(1983).
22. t. Fixher. Ph.D. thesis. U~jv~~ity of Vienna (1975).
23. A. Seeaer. 2. MetaRk. 47. 553 (19561.
24. H. Bib&. F. SebiIfeaauand C. B&k&, f. Insr. Me&s
87, 71 (1958).
25. E. de Lamotte and C. Altstetter, Tracts Am. fnsr. M&z
Engrs 245, 651 (1969).
26. M. Riihle and W. M. K&en, Ber. ~~nsenges. P&s.
Chem. 87, 222 (1983).