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A study of defect sub-structures in

the FeCr sigma phase by means of
transmission electron microscopy
a a
M. J. Marcinkowski & D. S. Miller
a
Edgar C. Bain Laboratory for Fundamental Research ,
United States Steel Corporation, Research Center ,
Monroeville, Pennsylvania
Published online: 20 Aug 2006.

To cite this article: M. J. Marcinkowski & D. S. Miller (1962) A study of defect sub-structures
in the FeCr sigma phase by means of transmission electron microscopy, Philosophical
Magazine, 7:78, 1025-1059, DOI: 10.1080/14786436208212898

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 [ 1025 ]

A Study of Defect Sub-structures in the Fe-Cr Sigma Phase

by Means of Transmission Electron Microscopy
By M. J. MARCINKOWSKI and D. S. MILLER
Edgar C. Bain Laboratory for Fundamental Research, United States
Steel Corporation, Research Center, Monroeville, Pennsylvania
[Received November 30, 19611
ABSTRACT
A. number of defect sub-structures have been observed directly by means of
traiismission electron microscopy in thin foils of the Fe-Cr u phase prepared
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frorn the bulk material. These defects for the most part consist of faults
lyiiig on (100) and (010) planes and which have been identified as sequence
faulks. Certain modifications of this basic configuration however do exist and
have been considered in detail.
No glissile dislocations have ever been observed, although sessile Frank
partial dislocations which act as termini for sequence faults have been seen.
This behaviour has been tentatively associated with the difficulty that
Kronberg's zonal dislocations may encounter in moving through the ordered
Fe- Cr u phase structure.
All of the sub-structures observed in the u phase are postulated to arise
during the course of its transformation from the ferrite phase.

1. INTROD~JCTION
EXCEPT for the presence of a y loop, iron-chromium alloys form a complete
series of ferritic b.c.c. solid solutions with one another from about 8 1 5 ' ~
up to the melting point. In the region of equiatomic composition on the
other hand, and in a temperature interval of 815-6OO0c, the ferrite is
unstable and transforms to a hard and brittle intermetallic compound
known as the u phase, which possesses a complex crystal structure that
can be readily retained a t room temperature upon cooling. Bain (1923)
was the first to observe the formation of this compound which was
subsequently investigated in greater detail by Bain and Griffiths (1927).
Because of the difficulty in obtaining u phase single crystals of sufficient
size, it was not until relatively recently that Bergman and Shoemaker
( 1 954) were able to identify the structure as tetragonal, belonging to the
space group D4,14- p4,/mnm, and containing 30 atoms per unit cell. The
unit cell is shown in fig. 1 and will be discussed in detail in a later section.
Accoiding to Duwez (1955), twenty-three binary u phases had been
established up to that time, all of which are characterized by the important
feature that they contain only transition elements. A greater under-
standing of these intermetallic compounds is therefore desirable from a
theoretical point of view. Tucker and Senio (1953) have shown that
@-uraniumalso possesses a crystal structure which is essentially the same
as that possessed by the u phase alloys. Furthermore, unlike the very
brittle (r phases, Holden (1952) found that single crystals of p-uranium
P.M. 3u
 1026 M. J. Marcinkowski and D. S. Miller on

were ductile, with slip occurring on the (110) planes and the (001)
directions. Based on these observations in p-uranium, Kronberg (1959)
proposed a model for slip by highly complex zonal dislocations. I n
addition, Frank and Kasper (1959) have discussed the possibility of
sequence faults existing in the cr phase structure.
The purpose of the present investigation has been to observe the cr phase
directly using transmission electron microscopy techniques in order to
elucidate some of the features mentioned above. Specifically it was
thought desirable to look for evidence of both zonal dislocations as well
as sequence faults in a u phase alloy. Furthermore, we have confined our
effort to the classic Fe-Cr u phase, since it represents an alloy with which
most previous work has been done. I n addition, u phase formation in
austenitic stainless steels leads t o severe einbrittlement of these alloys, aiid
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thus from a technological point of view, it is important to gain some further

insight into its nature.

5 2. GENERALIZED TREATMENT OF SEQUENCE FAULTS IN THE Pe-Cr

u PHASE STRUCTURE
For convenience, and also since previous investigations have clearly
established the structure of the Fe-Cr u phase, the discussion in this
section will apply primarily t o this alloy. Howevev, the general con-
clusions reached are expected to hold for all CT phase alloys.

Fig. 1

.-
0 - ATOMS WHICH LIE

0-
I,

II
II

II
II

41
AT Z.0
11

11
z I f 1/2 co

Z = f \/4Co
Unit cell of the u phase projected on the (001)plane.

The arrangement of atoms within the unit cell of the Fe-Cr cr phase
is shown in fig. 1 as constructed from the data of Bergman and Shoemaker
(1854). For convenience, table 1has been included to show the particulars
 Downloaded by [University of Montana] at 11:42 09 April 2015

Table 1. Configuration of atoms in the imit cell of the Fe-Cr (T phase

Position Coordination Values of

of atom number Occupancy Coordinates coordinates
for Pe-Cr 0
12 Fe
15 Cr

14 Mixed

1% Fe

14 Mixed 1
-
xp0;11 z"-4
Defect Sub-structwes in the Fe-Cr Sigma Phase
1027
 1028 M. J. Marcinkowski and D. S. Miller on
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L p L * L ( d L * L p L
t t

(b)
(a) KagomB-tiling net derived from Z = & frcg layer o f unit cell shown in fig. 1.
Heavy lines represent division o f net into right-handed hexagon strips;
( 6 ) kagom6-tiling net derived from Z = O layer of unit cell shown in fig. 1.
Heavy lines represent division of net into left-handed hexagon strips.
 Defect Sub-structures in the Fe-Cr Sigma Phase 1029

associated with the atoms in fig. 1. The position of the atoms shown in
this table are labelled in accordance with the notation of the International
Tables for X-ray Crystallography (1952). Furthermore, the work of
Bergman and Shoemaker (1954) suggests a partial ordering of the iron and
chromium atoms as shown in the fifth column of table 1. A detailed review
of this aspect of the problem has been given by Kasper (1855) in which a
general (scheme of ordering is suggested in many of the various u phase
alloys.
Perhaps the simplest way to regard the structure in fig. 1 is in terms of
its layers parallel to the (001) plane. The atom sites in the Z = & $c, layer
can be joined by lines so as to produce the net shown in fig. 2 ( n ) . This
specific configuration of triangle pairs and hexagons has been termed
*kagom&tilingby Frank and Kasper (1959). The dotted square in the
upper left-hand corner of this figure corresponds to the outline of the unit
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cell shown in fig. 1. Both hexagons and triangles comprising the net in
fig. 2 ( a ) are not exactly regular, but have been distorted slightly. This
arises fi,onz the fact that the net of fig. 2 ( a ) constructed from regular
triangles and hexagons gives rise to unit cell edges a, outlining a rhombus
that must be sheared by 4% to make it square as shown in fig. 1. From the
viewpoint of the present investigation, however, this particular feature
is not important. A t positions where Z = 0 in fig. 1, the atom sites can be
linked up to form another sheet of kagomd-tiling. According to Frank
and Kasper (1959), the layers of kagomd-tiling can be dissected into
vertical strips, shown by the heavy lines of fig. 2 ( a )and ( b ) . Furthermore,
in accordance with their notation, the strips in fig. 2 ( a ) will be termed
right-handed hexagon strips and those in fig. 2 ( b ) will be denoted as
left-handed hexagon strips. The Z = 0 layer can be easily derived from
the Z = k +c, layer and vice versa by displacing one corner of the dotted
unit cell of fig. 2 ( a ) by one-half the diagonal distance of the unit cell;
i.e. +ao [110], and then rotating it by 90. Midway between these layers
at Z = ic,, atoms occupy positions which are located very nearly at the
projected centre of the hexagons, and are shown by the black dots in
fig. 2 (crl and ( b ) which we shall also refer to as centres.
In accord with the notation of Frank and Kasper (1959), the vertical
right-handed hexagon strips in fig. 2 ( a ) will be labelled R, while the
x-ertical left-handed hexagon strips in fig. 2(6) will be labelled L. The
vertical rows of triangle pairs will be designated by p. When the nets of
fig. 2 ( a ) and ( b ) are superimposed, the arrangement shown in fig. 3 is
obtained. This figure is identical to fig. 1, but presents a somewhat clearer
insight into the detailed relationship between the atoms in the various
layers. Another feature that is obvious from figs. 2 and 3 is that the
relationship between two contiguous Ls is plus while that between two
contiguous Rs is minus, where + means a positive y-displacement,
between adjacent strips, and - a negative displacement. If, on the other
hand, p is placed between either of these pairs, the sign is reversed. It
follows then that p must never lie above p. These conditions must be
 L p L . L p L - L p L
- + - f -
R . R p R . R p R - R
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L p L * L p- L ' t P- L
- t t
R ' R p R ' R p R ' R
Arrangement of atoms in unfaulted u phase structure formed by superposition
of the two kagomb-tiling nets shown in fig. 2 ( a ) and (b). Plane of
projection is (001).
Close examination of fig. 2 ( a )and ( b )shows that certain types of mistakes
in the sequence of vertical strips are possible without changing either the
number or distance between nearest-neighbour atoms. These faults are
therefore expected to be of very low energy, and thus to possibly occur
rather frequently in the u phase alloys. Frank and Kasper (1959) were the
first to suggest this type of fault which they termed a sequence fault. It
will be the purpose of the sections that follow to extend their analysis,
as well as to develop these sequence faults in terms of displacement
vectors. This can be seen most easily by referring to fig. Z(a). The
row of hexagons R' can be removed, and the right-hand side of the net
 Defect Sub-structures i n the Fe-Cr Sigma Phase 1031

can be displaced by the vector fR,. The notation of Read (1953)has been
used to tiesignate the fault vector, i.e. f, while the subscript R indicates
that the fault vector is associated with the Z = & icOlayer, i.e. the layer
corresponding to the right-handed hexagonal strips. The letter 0 in
fig. 2 ( a ) designates the origin cjf the displacement, while the tip of the
arrow donotes the terminal point of the displacement. It is apparent
that such a displacement results in a perfect matching of vertical strips
across the (100) plane. Furthermore, no wrong nearest-neighbour atoms
occur across this boundary. There is a total of three basic faults of this
type that can be produced on the (100) plane. These are shown in fig. 2 (a)
and are denoted by the subscripts 1, 2 and 3 after the letter R.
It is apparent that before the fR,- fault can be made, both p and R
strips must first be removed, whereas for the fR,- fault, only the p strip
need be removed. The superscript minus designates that the displacements
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of the right-hand portion of the crystal are made in a generally negative

direction so as to close up the gap that is created by the removal of a vertical
strip or strips. A superscript plus on the other hand indicates that the
same displacements can be made in a reverse or + direction ; however,
an extm row or rows must now be inserted in the resulting gap. The
same reasoning used above can be used for the Z = 0 layer of kagomd-tiling
shown i n fig. 2 ( b ) , where the fault vectors are described by subscripts L
t o denote that the vertical strips comprising this net are left-handed.
When considering the sequence fault of the three-dimensional crystal
as a whole, one would generally anticipate that the displacement vectors
in each Z layer should be the same as the net fault vector of the crystal.
This however is not so in the (T phase structure. Specifically, no two
displacement vectors in the R and L layers are identical, either with respect
to direction or magnitude. The closest that one can come to matching
them is to use vectors on R and L layers that have the same numerical
subscript and same sign. As an example, the magnitudes of fR,- and
fL,- can be readily found to be (a0/15)[720]and (a0/15)[%0]respectively.
This amounts to a vector difference of (ao/15)[i00] across successive
R-L planes. Figure 4 shows the arrangement of atoms resulting from the
superposition of a 2 = _+ $co and a Z = 0 layer containing faults of the type
fR,- and fL,-, respectively. The fault created across the (100) plane is
shown by the dotted line, both sides of which, with respect to this line,
have been joined together by rigid displacements parallel to the (001)
plane. An estimate of the degree of shear strain between successive R
and L layers can be obtained by observing the relative displacement
between hexagonal centres in fig. 4. The centres shown as small dots
a
correspond to Z = - layers, while those shown by small dots surrounded
by heavy circles correspond t o 2 = + t layers. The relative displacement
ZAfl-= (ao/30)[T00]gives rise to a shear strain of about 7% in the (001)
plane and in the negative x direction.
When the subscripts R and L are dropped from the f vector, it is to be
understood that we are referring to the crystal fault vector. Definitions
 1032 M. J. Marcinkowski and D. S. Miller on
of fl- and Af1- are shown on fig. 5 ( b ) and explained below. A highly
schematic model of the manner in which a fl- fault is formed is shown in
fig. 5 (a)and (6). For simplicity, the atom centres are indicated by vertica.1
lines. After the L, p and R rows are removed, such as shown in fig. 5 ( a ) ,
a rigid displacement of the right-hand portion of the crystal must nest
be made to the left. However, such a rigid displacement cannot be made
which at the same time preserves continuity of material across the fault,
unless we extend the L layer along the x direction by 2Af1 and contract
the R layer along the same direction by 2Afl as shown in fig. 5 ( 6 ) . This

Fig. 4
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fl- type sequence fault (shown dotted) lying in the (100) plane o f the (7 phe.e
structure. Plane of projection is (001).

adjustment will of course be made only in the vicinity of the fault. The
net fault vector for the entire crystal across the (100) plane, which will
henceforth be termed the crystal fault vector, is now given by
fl-= (a0/30)[i5,4,0]. I n other words, the entire right side of the crystal
is displaced by this amount with respect to the left-hand portion of the
crystal across the fault plane. A comparison of the faulted structure of
 Defect Sub-structures in the Fe-Cr Xigma Phase 1033

fig. 4 with that of the unfaulted one in fig. 3 shows clearly that there is
very little distortion in the former. One therefore anticipates that faults
of the type fi- will be of very low energy.
All of the basic faults, both + and - that can occur on the (100) planes
of the Fe-Cr cr phase structure are shown in table 2 . The symbolic descrip-
tion is shown in the third column where the vertical lines have been added
to mark out the sequence of symbols associated with the unit cells. It is
immediately evident that the relationship between the various symbols
obey the rules stated earlier in this section. It can also be seen from the
third column of table 2 that the sequence faults always fall between like
signs.
Fig. 5
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323s- -R
L LAYER
LAYER
(a)

M
G;= 2 [Ti201
I

IH
-AT -Af I

((I) Highly schematic illustration of the manner in which a fl- type fault is
formed. Above figure illustrates situation immediately after L', p' and
R' rows are removed. Ckystal viewed along Y axis; ( 6 ) above shows
how material in vicinity of potential fault of fig. 5 ( a ) must be mutually
ccinstrained so that continuity of material can be preserved across the
fault. Eault is produced simply by displacing material to the right of
gap by f1-=(a0/30)[T5, 4, 01.

Thus far we have considered only the three basic sequence faults, i.e.
faults uhich cannot be formed by any combination of the other two.
However, reference to table 2 shows that one might possibly combine
 Downloaded by [University of Montana] at 11:42 09 April 2015

Table 2. Basic sequence faults lying on the (100) plane in the Fe-Cr 0 Phase

Layer
Operation needed to forin fault Symbolic description of faulted structurc Crystal fault vector
Vector
_-__ _____--_-
Perfect crystal

f -=%[820] Remove L and p strips

L1 15

fRF = [720] Remove R strip

15

Add L and p strips to left of L strip
15
a0
fR1+ = - [720] Add R strip to left of R strip
15

Remove L strip

U
fRz- 15 [820] Remove p and R strips

afl
fL: = T;s [720] Add L strip to left of L strip

Add p and R strips t o left of p strip

f -= a0 [ 1401 Add p strip to left of L strip

L3 15
a
f - =0
[Tiio] Remove p strip
R3 15
a
fL3+= L[T40] Remove R strip L 1 I, . 1, . L . I, p L
15

Add p strip to right of R strip R * RpRp R p R R

fR3+= 15 [1401 -1 + ; + +
- - -
 Defect Sub-structures in the Fe--Cr Sigma Phnse 1035

several like faults. For example, Nf,- faults might be combined to give
a total fault vector of N(u0/30)[ E , 4 , O ] leading to the following sequence :

L p L . L . ... L . L . L p L
- + + N ( +) + -
R * R p R p ... R Y R p R . R
A new structure is thus generated in the vicinity of the fault. Depending
on either the particular number and combination of f vectors used, an
infinite number of structures can be generated in the neighbourhood of the
fault, a6 Frank and Kasper (1959) have shown. On the other hand, it was
shown earlier that each basic sequence fault has associated with it a shear
strain. Combinations of fault vectors of the same sign increase this strain
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consideiably. As an example, a fault of 2f1- would give rise to a shear

strain of about 14% or double that for a single basic fl- fault. It is
concluded therefrom that multiple sequence faults would in general be
unstable in the Fe-Cr (T phase. On the other hand, table 2 shows that
certain combinations of faults could combine and annihilate one another.
This would be the case for the pairs fl---fl+, f2--f2+ and f,--f,+.
For a complete description of the sequence fault, the plane on
which it lies should be indicated after the fault as follows, fl(loo)-.
Table 2 lists only the three basic faults which lie on (100) planes.
Three similar faults can also lie on (010) planes. They are readily
found to be fl(olo)= k (a0/30)[4, 15, 01, fi(olo)= k ( a 0 / 3 0 ) [ 415,
, 01 and
f3(010)= -t ( a 0 / 3 0 ) [ 8
0,, 01, where the k notation indicates that the fault
can be either + or -, respectively. The following sections will be
concerned primarily with the experimental verification of the hypotheses
discussed above.
3 3. EXPERIMEXTAL
PROCEDURE
The iron-chromium alloy used in this investigation contained 47.8 at. yo
(46wt. "6) chromium and was obtained from the same ingot as that used
by Fisher et al. (1953) in their study of the 4 7 5 " embrittlement
~ problem.
SectionP were cut from the ingot and then hot rolled a t 1 1 5 0 " into
~ narrow
strips. These strips were in turn recrystallized for I hour at 1 1 5 0 " ~and
then air cooled to room temperature. One group of specimens was heated
to 8 2 8 " ~
and
~ slowly cooled to 5 0 0 " ~
at a rate of %74"c/hrin order t o trans-
form the ferrite, which is stable above about 815"c, into the u phase.
Because of the well-known sluggishness of this transformation, only a
fraction of the ferrite transformed to (T. From the work of Cook and
Jones (1 943) and Duwez and Martens (1957), however, it is known that
prior plastic deformation of the ferrite greatly accelerates the transforma-
tion. For this reason two additional groups of specimens were cold rolled
20% and 70%, and were in turn annealed a t 7 2 5 " for ~ 9 hours and 1 hour,
respectively, with an additional 1 hour anneal being given to some of the
7 0 7 , spucimens. According to Duwez and Martens (1957), this procedure
resulted in the transformation of about half the ac phase into the u phase.
 1036 M. J. Marcinkowski and D. S. Miller o n
The specimen thickness during the final a+u transformation was 0.004in.,
and is expected to show behaviour characteristic of the bulk specimens.
All annealing treatments were carried out in sealed and evacuated quartz
capsules. I n many cases the encapsulated specimens fragmented into
numerous small pieces, presumably due to the volume changes accompany-
ing the transformation, coupled with the extreme brittleness of the u
phase. Nevertheless, pieces suitable for polishing could usually be obtained.
These specimens were in turn electrochemically thinned to thicknesses
suitable for transmission electron microscopy using the method described
by Fisher and Szirmae (1969). The electrolyte employed was the
chrome-acetic acid solution developed by Morris ( 1949), while the polishing
conditions used were essentially those found suitable for the Cu,Au alloy
investigated by Fisher and Marcinkowski (1961). All of the transmission
electron microscopy and electron diffract'ion observations were made with
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a Siemens Elmiskop I operating a t 100 kv. I n order to ensure that no

diffracted rays contributed to the bright field image, a 2 0 p objective
aperture was used throughout the entire investigation.

5 4. RESULTS SXL) DISCUSSIOX

4.1. Direct Observation of Sequence Faults in the Fe-Cr (5 Phase

Figure 6 shows a transmission electron micrograph of the faulted u phase
structure which was developed from the ferrite by slow cooling as described
in the previous section. Nearly all of the faults, which are characterized
by a number of fringes parallel to their length, lie on (010) planes, while
a few lie on (100) planes. These latter faults appear as very narrow lines
since they lie essentially perpendicular to the plane of the foil. From
energy considerations alone, it is expected that the faults in fig. 6
associated with the (010) planes should be of the type fi(olo) and fi(olo).
A further interesting aspect of this figure concerns the fault configuration
immediately to the right of A. This is believed to represent the coalescence
of two faults either of the same type but opposite sign, i.e. fl+ and f,- or
of the same sign but opposite type, i.e. fl- and f2-. Either one of these
combinations would eliminate the fault. However, a very faint contrast t o
the right of A in fig. 6 remains, indicating that the faults have not been
entirely eliminated by coalescence.
Some areas such as those to the right of B in fig. 6 show enhanced contrast
along a portion of the fault. This behaviour is due to what appears to be
very closely spaced, if not in fact entirely combined, faults of the same type
and sign. These features will be discussed in the following section dealing
with contrast effects associated with these sequence faults.
Since the u phase structure is tetragonal, care should be taken so as not
to use indices of direction and the Miller indices associated with the nornial
to a crystal plane interchangeably, as can be done in the case of cubic
crystals. On the other hand, for tetragonal crystals, these indices can be
used interchangeably for all planes which lie in the [ O O l ] zone since this
axis possesses four-fold symmetry.
 Defect Sub -structures in the Fe-Cr Sigma Phase 1037

A much simpler orientation of the CT phase is shown in fig. 7 ( a )where the

[ O O l ] axis is essentially perpendicular to the plane of the foil. The very
narrow 1-inesrepresent sequence faults which lie on (100) planes and are
therefore also essentially perpendicular to the plane of the foil. They are
thought to be of the type fi(loo~or fi(loo). These narrow faults are not

Fig. 6
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Sequence faults in the Fe-Cr CJ phase, formed by cooling from 828"c t o 500"c at
a rate of 2*74"c/hr. Direction normal t o foil is [ O i l ] .

continuous across the entire area of the micrograph, but are repeatedly
interrupted by oblique segments of fault which link up the narrow faults
that lie on different but parallel (100) planes. As deduced from their
varying width, these short segments of fault do not appear to lie on any
given crystallographic plane, but rather on a variable non-crystallographic
 1038 M. J. Marcinkowski and D. 8. Miller on
surface. Furthermore, since these short broad non-crystallographic
segments of the fault are continuous with the narrow long crystallographic
portions, it is presumed that they have the same fault vector as the latter.
This is also borne out by the similar contrast exhibited by these various
areas along the fault. However, it was shown earlier that the (100) plane
was expected to be a much more favourable plane for the fault to O C C U ~ J T
than any other, because of the smaller distortion associated with the atoms
across it. It is suggested that the faults lying on non-crystallographic
surfaces do not represent the lowest energy configuration, but are formed
in some nianner as a result of the (T to 01 transformation as will be discussed
in a later section. Another important feature of inany of the non-
crystallographic portions of the fault is that they are stepped, such as
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Fig. 7
 Dpject Sub -structures in the Fe-Cr Sigma Phase 1039

Fig. 7 (continued)
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(b)
(a) Sequence faults in the Fe-Cr CT phase formed as described in fig. 6. Direction
normal to foil is [OOl]; ( b ) selected area diffraction pattern of area
shown in fig. 7 (a).

can be men just above A in fig. 7 (a). I n some cases only one side of the fault
is stepped such as that immediately to the left of B in this same figure.
The detailed manner in which these steps are thought to develop is
shown diagrammatically in fig, 8 ( a )through ( c ) , The light lines represent
the idealized rectangular foil, while the heavy ones designate the fault. The
pair of dotted lines which run roughly parallel to the direction of the fault
represent the fringes arising from diffraction contrast. They correspond
to fixed distances within the crystal, i.e. one-half the extinction distance,
when the foil is oriented a t the exact Bragg angle for reflection.
 1040 M. J. Marcinkowski and D. S. Miller on
Figure 8 ( a )shows a sequence fault in which only the portions AB and
CD, which are displaced from one another on parallel planes, lie on low
energy (100) planes. These portions in turn are joined by the segment
of fault B-C which in general lies on a high energy non-crystallographic
surface. The area, and thus the energy of this high energy portion of the
Fig. 8
D

(a)
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(u)Portion of sequence fault BC lying on high energy plane in thin foil of the
Fe-Cr u phase; ( b ) energy of fault BC is reduced by nucleation of steps
in upper portion of foil which lie on (100) planes; (c) completion of step
formation which was initiated as shown in previous figure.
fault, can be reduced if a series of steps were t o form in the following
manner. The nucleation of the steps on the upper surface of the foil as
shown in fig. 8 ( 6 ) corresponds to the fault immediately to the left of B in
 Defect Sub -structures in the Pe-Cr Sigma Phase 1041

fig. 7 (a). The completion of the stepped fault is shown in fig. 8 (c) and
corresponds to that portion of the fault immediately above A in fig. 7 (a).
Note that the angle 3, that the high energy portion of the fault makes with
the foil surface shown in fig. 8 (c) varies considerably in many cases. This
can be seen by the varying width along the [ O l O ] direction of the stepped
faulted Hegment immediately to the right of C in fig. 7 (a).

Fig. 9
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Closed f.iiultsurface in the Fe-Cr u phase. u phase formed from 70% cold-rolled
ferrite byLannealing for 2 hours at 725"~.

The selected area diffraction pattern of the area shown in fig. 7 ( a )is
given int fig. 7 (b). As a result of the relatively large unit cell size of this
structure, i.e. a, = 8.800 H and co = 4.544 A, together with its low symmetry,
the number of reflections in fig. 7 ( b ) is quite large. Furthermore, the
P.M.
3x
 1042 M. J. Marcinkowski and L). S. Miller on
spacing between adjacent reciprocal lattice planes is sufficiently small
so that a considerable number of reflections corresponding to these planes
also contribute to the pattern of fig. 7 (6). This in turn makes the detailed
analyses of the patterns corresponding to the various orientations relatively
difficult. I n addition, dark field analysis is also made quite difficult
because of both these factors.
Fig. 10
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Polygonized sub-grains of ferrite formed concomitantly with the u phase in 70%

cold-worked ferrite which had been annealed for 1 hour at 725C.

Another interesting micrograph of the faulted structure in the 46%

Cr-Fe u phase which was developed by annealing a 70% cold-rolled ferrite
~ shown in fig. 9. The geometry of the fault
specimen for 2 hours at 7 2 5 " is
is believed to arise from the coalescence of a portion of fault loop possessing
 Defect Sub-structures in the Fe-Cr Xigma Phase 1043

a displacement vector f, over the length A-B. The fault vector of the
segment A-B is then 2f. I n other words, the material within the loop is
displaced with respect to the matrix by f, and is quite reminiscent of the
antiphaso domains in the Fe,Al-B, superlattice observed by Marcinkowski
and Brown (1962). Figure 9 is thought to represent a possible process for
fault elimination whereby the loop continually shrinks until it finally
disappears, leaving behind a sessile dislocation at the end of the fault
A-B at 1:. Notice again that steps have formed on the fault loop in order
to reduco its energy.
During the transformation from the 01 to the c phase in specimens that
were previously deformed plastically, it was found that two processes
were occurring simultaneously. The first was the transformation of the
cold-workedferrite to u,while the second process involved the recrystalliza-
tion of tthe cold-worked ferrite into large strain-free grains. It was also
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found however that numerous regions within the ferrite were incompletely
recrystallized, giving rise to typical sub-structures as shown in fig. 10.
These regions are clearly seen to be comprised entirely of polygonized
sub -grains about 4000rf in diameter which are separated from one another
by grids consisting of dislocation networks of varying complexity.
Somewhat similar type sub-grains were observed by Nenno et al. (1960)
after annealing a heavily cold-worked 55wt.(?)yo (3-Fe alloy at 720"c
for 24 hours. Similar networks have also been observed in cold-worked
3$ wt. %, Si-Fe prior to recrystallization by Hu (1962) using transmission
electron microscopy techniques. He has in turn considered the mechanisms
involved in detail in connection with the recrystallization processes
occurring in this alloy.

4.2. Contrast Effects Associated with Faults in the Cr-Fe u Phase

A comprehensive review of the contrast effects produced by dislocations
and stacking faults has been given by Whelan (1958-59). Marcinkowski
(1962), on the other hand, has recently given a review of these contrast
effects as applied to sub-structures in superlattices. For these reasons
therefore, only those features of diffraction contrast which apply to this
investigation will be considered in any detail in the present paper.
Whelan and Hirsch (1957) have shown theoretically that fault contrast
can be observed using transmission electron microscopy when the foil is
critically oriented for Bragg reflection from some plane hkl. The reason
for this is that the diffracted waves undergo a change in phase angle 01
in the faulted region given by
O1=2rrg.f, .... .. . (1)
where g is the reciprocal lattice vector corresponding to the reflection hkl
and f is the fault vector. Consequently, the intensity is modified in the
faulted region of the crystal with respect to the unfaulted areas. Whelan
and Hirsch (1957)) using the dynarnical theory of diffraction and neglecting
3x2
 1044 On Defect Sub-structures in the Fe-Cr Sigrnu Phase
absorption, have shown that the transmitted intensity across the fault on
the underside of the foil is given by

where

and
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Fig. 11
rTr--irr I I I i I I Ti- I ' I
1.0-

In
-
-
2 0.8-
I-
z -
0
0.6 -
5
3 -
2
- 0.4-
N -
5
N 0.2-
.-
"7 -
L& I
0
15
PHASE ANGLE a ASSOCIATED WITH h k l
REFLECTION GIVING RISE TO FAULT CONTRAST
Graph showing how fault contrast diminishes as a decreases.

where t is the thickness of the foil, X is a parameter indicating its deviation

from the exact Bragg angle 6, 2 is the perpendicular distance measured
from the centre of the foil, and to is the extinction distance associated with
a particular g. In general, f will consist of periodic variations in intensity
with Z giving rise to fringe contrast across the fault. Whelan and Hirsch
(1957) have shown that the maximum intensity dfference between these
fringes will decrease as either t decreases or as X increases, and finally
vanishes. On the other hand, it is important to realize that when X and t
are held constant, the maximum intensity difference between the fringes
will decrease as 01 decreases from T to 0. This is apparent from eqn. ( 2 )
since the a's appear only in sin terms. For convenience, it is instructive
to write eqn. ( 2 ) for X = 0. Furthermore, by keeping X and t constant
we may express eqn. ( 2 ) as follows :
E' = sin2401cos22.rrZlt0. . . . . . . (3)
 Table 3. Variation of phase angles 01 with both the indices of reflection
h, k, 1 corresponding to the reciprocal lattice point g and the
fault vector f
--
Sequence faults whi-ch Sequence faults which
lie on (100) planes lie on (010) planes
--__-
g fi or f, f3 f, or f, f3
- _ I ~
-

100, 101, 102, 15 4 8

103,104,105
+-i7
- 15
0 +ET +-77
- 15
010, 01 1, 012, 4 8 15
f-77 +-77 +-77 0
013,014,015 15 15 - 15

110,111,112 *-
11
15
i7
8
*-Ti
15
11
F-77
15
5-77
15
8

001, 002 0 0 0 0
8
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200,201,202 0 0 +-rr 14
15 +-TI
8
- 15
14
020,02 1.022 *--a 5-77 0 0
15 15
-4 8 7 14
210,211,212 +-77 +--n +-77
15 7 T - 15 - 15 -- 15
7 14 4 8
120,121,122 +-i7 +-iT +-7i 51571
- 15 - 15 - 15
8 14 8 14
220,221,222 I-i7 i-77 +-77 +-77
15 15 15 15
15 12 6
300, 301, 302 +-i7
15
0 +-77 -
15 15 i7
12 6 15
030,031, 032 f-i7 f-i7 *-77 0
15 15 15
10 B 3 6
310, 311 *-77
15 +--..
15
+-77
15
k-77
15
3 6 11 8
130, 131 *-77 &-TI +-77 2-77
15 15 15 15
7 14 12 6
320,321 k g v +-77 +-77 +GV
15 15
12 6 7 14
630,231 +-i7
15 + -77
- 15
k-77
15 *EX
400,401 0 14 2
0 f-77 *-7r
15 15
14 2
040,041 5-77 +-7r 0 0
15 15
4 8 1 2
410,411 +-77 "7r 5-77 *-77
15 15 15
1 2 4 8
140,141 +-7r *-77 &-77 'C"
15 15 15
3 6 3 6
330,331 +-77 +-77
- 15 15
+-77
- 15
8 14 14 2
420,421
-+ - T15I +-77
- 15 +-7r
- 15 +-?7
- 15
14 2 8 14
240,241 f-77 *---TI 5-77 *iy
- 15 15 15
--
 1046 M. J. Marcinkowski and D. S. Miller on
Specifically t' is that part o f t which varies with 2 and is seen to be of the
cosine squares form. For sufficiently large 8,i.e. Z 2 t o / 2 ,the maximum
change in the cosine square term will be one, i.e. the difference in fringe
contrast corresponding to Z = O and Z = t o / 2 . This function in turn is
modified by the sin2&aterm which may vary between the limits of 1 for
a = 7~ to 0 for a = 0. Thus the maximum digerenee in intensity between
successive fringes and therefore the fault contrast, varies as sin2 801 when
X = O as shown in fig. 11. Whelan and Hirsch (1957) have shown that
a = 3.+r,corresponding to a maximum intensity difference of 0.75 in fig. 11.
I n addition Marcinkowski (1962) has shown that 01 may be r, r j 2 or r / 3
for certain combinations of superlattice reflections and antiphase bound-
aries, thus giving rise to maximum intensity differences according to
fig. 11, of about 1, 0.5 and 0.25 respectively. For convenience, the ordinate
in fig. 11 will simply be referred to as fault contrast henceforth.
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Turning now to the analysis of the various phase angles associated with
faults in the Fe-Cr (T phase, consideration will be given only to the basic
fault vectors fl, f, and f, which are associated with faults lying in the (100)
and (010) planes. Using these fault vectors along with a number of the
lowest-order reflections compiled by Bergman and Shoemaker (1954) for
the Fe-Cr u phase, we have constructed table 3. In this table the phase
angles are listed along a row corresponding to a particular reflection and
along a column corresponding to a particular f vector. Because of their
nature, the fault vectors fl and f,, which lie on the same plane, give identical
values for 01. In addition only positive indices have been listed for the
indices of reflection in table 3 , since any distribution of negative signs
among these indices does not alter the original value of a: associated
with the positive indices. Another interesting feature of this table is
that a: can be expressed in general as + N r / l 5 , where N can be any
integer. It is apparent however that N need be considered only in
the range 0 to 15. One therefore has a discrete spectrum of phase angles
associated with faults in the cr phase which accordingly is expected to give
rise to a wide variation in fault contrast. It is anticipated that this
type of behaviour will become quite common as more complex faulted
structures are examined.
In order to check the hypotheses advanced above experimentally, the
following series of experiments was carried out. Figure 1 2 ( a ) shows
a bright field micrograph of a grain formed as described in fig. 9. Parallel
(T

pairs of faults are seen to lie on (010)planes and to extend from the left-hand
edge of the foil into the thicker regions toward the right. These pairs of
faults are joined by oblique segments to the right of the micrographs which
appear to lie on no specific crystallographic plane, in a manner similar to
what had previously been observed in fig. 7 ( a ) . Since these faults lie for
the most part on (010) planes, they are postulated t o be either of type fl
or f,, or f,, with the latter being less probable because of their higher energy.
In order to verify this prediction, the dark field micrographs shown in
fig. 12 (c), ( d ) and ( e ) were taken of the area shown in fig. 12 ( a ) using the
111, 222 and 333 reflections respectively of the selected area diffraction
 Defect Sub-structures in the Fe-Cr Sigma Phase 1047

pattern (of fig. 1 2 ( b ) . According to table 3, the phase angles for these
reflections associated with either fl or f2 should be +_ 11/15) +_ 8/15 and
+ 3 / 1 5 n corresponding to fault contrasts of about 0-85, 0.55 and 0.1
respectiliely as obtained from fig. 11. This general decrease in fault contrast
is indeed observed in the dark field micrographs of fig. 12 (c) through ( e ) .
On the other hand, the fault vector f3 can be immediately eliminated as
the vector associated with the faults in fig. 1 2 ( c ) through 12(e) since,
according to table 3 and fig. 11, it would give rise to an enhanced fault
contrast in proceeding from fig. 12 (c) through 12 ( e ) ,which is not observed.
During the course of this investigation, it was observed that fauIts
lying on (100) and (010) planes frequently intersected one another. This
can be seen by referring to fig. ( 1 3 a ) and ( b ) . Here again it is assumed
that these faults are of the type fl and f2.
In the region denoted by B in fig. 13 (a),the intersection is simple, and,
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as it should, the fault contrast vanishes along their line of intersection.

Similarly, a small segment of fault in region A of this same microgra,ph
also shows vanishing contrast. The indication in the latter case is that
the two basic faults have combined over the small segment to produce a
+
fault with a resultant vector of fl(loo) f2(010,, f2(100) + fi(olo), fi(lOo)+ fl(010) Or
+
f2(100) f2(010). A dark field analysis of fig. 13 ( a ) showed that the fault
contrast resulted from a 2 2 2 reflection. According t o table 3, the possible
phase angles associated with the resultant fault could be either 0 or 14/15n-.
The former phase angle is obviously the more likely since the combined
segment of fault in fig. 1 3 ( a ) shows vanishing contrast. A slight tilting
of the foil in the electron microscope was sufficient to permit strong contrast
from a second reflection which in turn was able to reveal the short segment
of fault as shown a t A in fig. 13 (6). A large number of intersecting faults
can also be observed in fig. 14 which was obtained from a different region
of the same grain shown in fig. 13. Here again it is seen that at some
intersections, the faults have combined over a small length. However,
this does not occur as a general rule. I n fact, it appears that simple
interseelion without combination is more frequent. It is concluded
therefrom that the energy decrease resulting from such combinations is
small. ii possible explanation for the combinations that do occur, however,
is believed to be as follows. As has been shown earlier, the fl and f2 type
faults hiLve associated with them a certain shear strain E, which normally
acts perpendicular to the fault plane. Assuming this strain to be elastic,
the energy corresponding to the strain is proportional to Ge2, where G is
the shear modulus. If we now combine fault vectors associated with
faults lying on (100) and (010) planes, the shear strain of the resulting
fault is now ~ Z E and , acts in a direction of 45' to both the (100) and (010)
planes. Furthermore, its resultant energy is proportional to 2Ge2. If G is
isotropic:, then the fault combination will involve no change in energy.
On the other hand, if G measured at 45" to [loo] and [ O l O ] is smaller than
G at right angles to these planes, then a decrease in energy can be expected
by combination. From the observations in figs. 13 and 14, however, this
difference in G is apparently quite small.
Downloaded by [University of Montana] at 11:42 09 April 2015

Fig. 12
 012 Defect Sub-structures in the Fe-Cr Sigma Phase 1049

Fig. 12 (continued)
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( a ) Bright field micrograph of faults in the Fe-Cr u phase. 0 phase developed

assdescribed in fig. 9; ( b ) selected area diffraction pattern of area shown
in fig. 12 ( a ) ; ( c ) dark field micrograph of area shown in fig. 12 (a).
111 reflection of fig. 12 ( b ) used to form image; ( d ) dark field micro-
graph of area shown in fig. 12 ( a ) . 222 reflection of fig. 12 ( b ) used to
form image; ( e ) dark field micrograph of area shown in fig. 12(a).
333 reflection of fig. 12 (6) used to form image.

A final interesting observation of the transmission electron micrograph

of fig. 14 shows t h a t steps are observed on faults which in many cases do
not lie on (100) and (OlO),b u t on higher index planes. Preliminary analyses
indicate t h a t some of the steps, specifically those near A a n d B, probably
 1050 M. J. Marcinkowski and D. S. Miller on
lie on (T10) and (110) planes respectively, although this is not always
the case.
4.3. Dislocations in the Fe-Cr u Phase
Bain and Griffiths (1927) have made hardness measurements of the Fe-Cr
u phase and, although in most cases the specimen shattered, preventing
any meaningful readings, they report obtaining ' very proper ' hardness
values of 68-5 Rockwell C in a few cases. In order to obtain some
explanation for this high hardness, the following observations were made.

Fig. 13
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(b)
( a )Intersection and combination of pair of faults in the Fe-Cr 0 phase, producing
the segment at A which exhibits vanishingly small contrast. CT phase
developed by annealing for 9 hours at 7 2 5 " after
~ cold rolling ferrite 20%;
( b ) same area as that shown in fig. 13 (a), only this time foil was tilted
slightly, giving rise t o fault contrast at the segment A,
 Defect Sub -structures in the Fe-Cr Sigma Phase 1051

Figure 15 shows an incompletely transformed Fe-Cr alloy in which the

untransformed a or ferrite grain is located toward the right, while the
u grain is located toward the left side of this figure. The white band A-B
represents a crack which travels through the u phase only. I n general,
very high stress concentrations are generated in the vicinity of an advancing
crack. This can be seen in fig. 15 by noting the high density of dislocations

Fig. 14
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Intersecting sequence faults in the Fe-Cr phase. D phase developed as described

in fig. 13 (a).

which have been generated in the a phase at the tip of the crack which
terminates in the a--0 interface. On the other hand, similar obvious
dislocation generation in the o phase does not occur. There is, however,
some indication of very small dislocation loops originating at the periphery
of the crack in the u phase, but this is not a t all certain. No moving
 1052 M. J. Marcinkowski und D. S. Miller on
dislocations or dislocation traces were ever observed in the cr phase. On
the basis of the similarity in crystal structure alone between p-uranium
and the Pe-Cr cr phase, it would be expected that the latter should show
some ductility and thus dislocation motion. However, as has been
mentioned earlier in this paper, there is strong evidence that the f~ phases
are in general ordered although the details have not yet been worked out.
It appears quite likely that the motion of Kronberg's (1959) zonal
dislocations must do work against these ordering forces, which in the case
of the Pe-Cr cr phase is apparently quite large.

Fig. 15
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Generation of dislocations in ferrite ( a ) at the cr phase interface resulting from

the propagation of a crack in the u phase. u phase formed from 700/,
cold-rolled ferrite by annealing for 2 hours at 7 2 5 " ~ .
 Befeet Sub-structures in the Fe-Cr Sigma Phase 1053

A final important observation of fig. 15 shows quite clearly that the

faults in the u phase lie nearly at right angles to the u-01 boundary and in
many cases terminate thereon thus growing along with it. This can be
seen just above the crack A-B. Occasionally, however, a pair of these
faults become united by an oblique segment as was also observed in fig. 12,
so that they form a closed loop within the grain of the CT phase. It is

Fig. 16
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Sequence fault bounded by sessile dislocations in the 46% Cr-Fe c phase.

u phase developed as described in fig. 15. Direction normal t o foil is [22i].

concluded from these observations that the faults that form, do so

thermally as a result of the transformation of the 01 phase to CT,and not by
the motion of glissile dislocations.
Sequence faults may however end abruptly within a grain of u phase
if they terminate on dislocations. An example of this is shown in fig. 16
where the ribbon of sequence fault lying on a (010) plane lies completely
 1054 M. J. Marcinkowski and D. 8. Miller on
within the grain of (5, so that both ends must terminate on dislocations.
These dislocations are just barely visible in the figure. Figure 17(a)
shows a schematic representation of the fault-dislocation configuration
that is obtained in fig. 16, where for convenience the fault is postulated
to lie on the (100) plane. The fault is believed to be a basic one of either
type fi or f2. We have also for convenience chosen the former. Further-
more, the fault can be formed in two ways. The first involves removing

Fig. 17

L p L * L p L * L p L - L p L * L p L * L p L *
- + - + - + - + - f - f
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R * R p R - R p R * R p R - R p R - R p R * R p

1. L A
1 ' I
I I I
L p L *LI- L p L - L p LI* LI* L p L
- + I + - + - L t L +'t I + - +
R R p Rlp R * R p R * R * R p Rip Rlp R R p
I
I
I
I
Lp
=++I

L - L L Lp- L +- L p-
2GlOO)

+cm,
I R
- + I +
R p RIP R Rp R
I I
I <=
1
T T f'('oo)
L p L * L p L * L p L * L p L * L p L - L p L *
- + - + - + - + - + - +
R - R p R * R p R * R p R * R p R * R p R * R p
(a) (b)
( a ) Basic fl(loo,-sequence in the Fe-Cr u phase bounded by a pair of Frank
partial (sessile) dislocations; ( b ) composite sequence fault which
terminates on three Frank partial dislocations.

planes of atoms parallel to the (100) plane and then bringing the adjacent
faces together. This operation results in the formation of the pair of
partial dislocations shown in fig. 17 (a,) which are termed negative Frank
particles. Furthermore, they are of pure edge type. For illustrative
purposes, the symbolic representation of the arrangement of hexagon
strips on adjacent nets is shown across both the faulted and unfaulted
regions of fig. 17(a). With this notation, it is apparent that the fault
involves the removal of p, L and R strips between the vertical dislocation
 Defect Sub-structures in the Fe-Cr Sigma Phase 1055

pair. The addition of p, L and R strips would create a positive Frank

partial, i.e. fi(loo)+. It is apparent that the Burgers vector of the partial
dislocation does not lie in the glide plane (assumed to be the same as that
for p-uranium if slip could be induced in this alloy, i.e. (110) or (lTO)),
and for this reason the dislocations are not mobile. They are therefore
termed sessile dislocations and can move only by climb.
Fig. 18
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Abrupt termination of sequence faults on sessile dislocations in 46% Cr-Fe

u phase. u phase formed as described in fig. 6. Direction normal to
figure is [OlZ].
A striking transmission electron micrograph obtained from a region
showing a high density of faults which terminate on Frank partials is
shown in fig. 18. For the most part, they are believed to be of the type
shown in fig. 17 ( a ) , although in some cases the faults do not always lie
 1056 M. J. Marcinkowski and D. S. Miller on
on (100) or (OTO) planes. On the other hand, the dislocations appear to
all lie along [ O O l ] directions.
Figure 19 shows another CT phase grain which was formed by a heat
treatment similar to that given to the specimen shown in fig. 18. Here
again many of the faults are seen to terminate abruptly on dislocations,

Fig"l9
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Termination of stepped faults on sessile dislocations in the Fe-Cr u phase.

u phase formed as described in fig. 6. Direction normal t o foil is [1T6].

and are believed to be essentially of the type shown in fig. 17 ( a ) . On the

other hand, however, many of them do not lie on either (010) or (TOO)
planes, but continually change direction via a series of steps. The steps
 Defect Sub-structures in the Pe-Cr Sigma Phase 1057

however do appear to lie on (OTO) and (TOO) planes. They are believed
to arise for reasons similar to those previously discussed in connection with
fig. 8.
Another interesting feature of both figs. 18 and 19 is the segment of
fault lying immediately to the left of the areas labelled A, in which a
dislocation line is contained entirely within the fault. The arrangement
giving rise to this configuration is believed to be that shown schematically
in fig. 17 ( b ) ,and which can be interpreted in a manner similar to that given
in fig. 1 7 (a).Specifically, two identical sequence faults bounded by Frank
partial dislocations have been brought together over only a portion of their
length. One portion of the fault therefore has a vector of 2f1- and must be
separated from that portion of the fault whose vector is fl- by a Frank
partial as shown in fig. 17 ( b ) .
Of final interest in fig. 19 are the two entirely closed loops of fault
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immediately below the area labelled B. Similar observations have been

made in fig. 9, and discussed in terms of a possible mechanism for fault
elimination.
I n closing, we wish to emphasize that in this initial study no attempt
was made to examine the details of the mechanism involved in the
transformation of the cy phase to u. The primary concern has been with
a study of the geometry of dislocations and faults in the u phase structure
only. It is hoped that additional investigations into the transformation
mechanism will be made in the near future. These additional studies will
be necessary, since, as the present investigation has shown, there is little
doubt that both the sequence faults as well as the dislocations observed
in the u phase arise as a result of the transformation of the cy phase to u.
One possibility is that these may be associated with the nature of the strain
at the Ix-u interface due to the difference in structure between the two
lattices.

8 5. SUMMARY AND CONCLUSIONS

The present investigation has been concerned primarily with a trans-
mission electron microscopy study of the defect sub-structures occurring
in the Fe-Cr u phase. These defects are postulated to arise during
transformation of the ferrite to u.
Faults lying on (100) and (010) planes were the most common
defects observed. They have been interpreted as sequence faults as
first described by Frank and Kasper (1959), with fault vectors of the
type f == (a,/30)(15,4, O ) , where the first two terms enclosed within
carets can be permuted with respect to both position and sign. Many of
these facultsform closed surfaces within the 0 grain similar to antiphase
boundaries observed in B2 type superlattices. Because of this behaviour,
certain portions of the surface cannot lie on the lowest energy planes.
The faulted planes in these portions are frequently found to be stepped.
This behaviour has been explained in terms of a possible mechanism
whereby the faults on these unfavourable planes can lower their energy.
P.M.
3y
 1058 &I. J. Marcinkowski and 1). S. Miller on
Frequent intersection of sequence faults lying on (100) and (010) planes
are found to occur, with occasional coalescence of the faults over a small
segment of plane near this line of interaction.
The critical conditions giving rise to fault contrast using transmission
electron microscopy techniques have been considered in some detail.
Of most importance is the observation that the change in phase angle
which the diffracted electron beam undergoes in passing through the fault,
can be expressed in general by a = & N/15n. N can be any integer from 0
to 15, depending on the particular combination of the indices of reflection
of the diffracted wave and the fault vector. The fault contrast in turn
varies from zero for N = 0 to its maximum value for N = 15.
No direct or indirect evidence for dislocation motion was ever observed
in the Fe-Cr u phase. On the other hand, dislocations frequently acted as
termini for stacking faults, from which it has been concluded that they are
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immobile Frank partials of the type f = (15,4, O } which are also formed
during the transformation of ferrite to u. The high hardness and brittleness
of the Fe-Cr 0 phase has been related to the difficulty in nucleating and/or
generating glissile dislocations in this alloy. This difficulty is thought to
arise from the work that the dislocations may have to overcome due to
the ordering forces between the atoms in this alloy.

ACKNOWLEDGMENTS
The authors would like to express their appreciation to R. M. Poliak
and J. C. Raley for technical assistance during the course of this
investigation. I n addition, the helpful comments and criticisms of
N. P. Louat and P. R. Swann are gratefully acknowledged.

REFERENCES
BAIN,E. C., 1923, Chem. Met. Eng., 28, 23.
BAIN,E. C., and GRIFFITHS,W. E., 1927, Trans. Amer. Inst. min. (metall.)Engrs,
75, 166.
BERGMAN, G.. and SHOEMAKER, D. P., 1954, Acta Cryst., 7, 857.
COOK, A. J., and JONES, F. W., 1943, J. IronSt. Inst., 148, 217.
DTJWEZ, P., 1955, Theory of Alloy Phases (American Society for Metals), p. 243.
, and MARTENS,H., 1957, Ductile Chromium (American Society for
D u w ~ zP.,
Metals), p. 322.
FISHER, R. M., DULIS,E. J.,and CARROLL,K. G., 1953, Trans. Amer. Inst. min.
(metall.)Engrs, 197, 690.
FISHER, R. M., and SZIRAME, A., 1959, Special Technical Publication No. 262
(American Society for Testing Materials), p. 103.
FISHER, R. M., and MARCINKOWSKI, M. J., 1961, Phil. Mag., 6, 1385.
FRANK, F. C., and KASPER, J. S., 1959, Acta Cryst., 12, 483.
HOLDEN, A. N., 1952, Acta Cryst., 5, 182.
Hu, H., 1962, Trans. Amer. Inst. min (metall.)Engrs., 224, 75.
INTERNATIONAL TABLESFOR X-RAYCRYSTALLOGRAPHY, 1952 (Birmingham:
Kynoch Press).
KASPER,J. S., 1955, Theory oj* Alloy Phases (American Society for Metals),
p. 264.
KRONBERG, M. L., 1959, J. nucl. Materials, 1, 85.
 Defect Xub-structures in the Fe-Cr Xigrna Phase 1059

I , J., and BROWN,N., 1962, J. appl. Phys., 33, 537.

M ~ C I N K O W S K M.
MARCINKOWSKI, M. J., 1962, Proceedings of the First lnternationl Materials
Conference held at Berkeley, July 5-8, 1961 (Interscience).
MORRIS,C. E., 1949, Metal Progr., 56, 696.
NENNO,S., SABURI,T., TAGAYA, M., and NISHIYAMA, Z., 1960, J . phys. Soc.,
Japan, 15, 1409.
READ,W. T., 1953, Dislocations in Crystals (McGraw-HillBook Co., Inc.), p. 95.
TUCKER, C. W., and SENIO,P., 1953, Acta Cryst., 6, 753.
WRELAN,M. J., and HIRSCH, P. B., 1957, Phil. Nag., 2, 1121, 1303.
WHELAN, M. J., 1958-59, J . Inst. Met., 87,392.
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