Acta metall, mater. Vol.43, No. 12, pp.

42134225, 1995
Pergamon ElsevierScienceLtd
Copyright ~ 1995Acta MetallurgicaInc.
0956-7151(95)00126-3 Printed in Great Britain.All rights reserved
0956-7151/95 $9.50+ 0.00

IN SITU STUDY OF THE SELF-ACCOMMODATING

PROCESS D U R I N G THE MARTENSITIC
TRANSFORMATION OF A Cu-Zn-A1 SINGLE CRYSTAL
BY SYNCHROTRON X-RAY TOPOGRAPHY--I.
CRYSTALLOGRAPHIC STUDY
C. J O U R D A N l, J. GASTALDP, V. ROQUES l, G. GRANGE t, S. BELKAHLA 2
and G. GUI~NIN 2
rCRMC2-CNRS, Campus de Luminy, Case 913-13288, Marseille Cedex 9 and 21NSA-GEMPPM,
URA CNRS 341, B~it. 502 20, avenue A. Einstein-69621 Villeurbanne Cedex, France

(Received 16 February 1994; in revised form 26 March 1995)

Abstract--The thermoelastic transformation of the CuZnA1 shape memory alloy has been studied in situ
and in real time by synchrotron X-ray topography. The white nature of the beam leads access to
crystallographic relations between crystals in ]~ and 9R phases. From our original method deduced from
the Kajiwara theory the experimental and simulated orientations have been compared and the self-accom-
modating character of the transformation has been shown.

R~sum6--La transformation thermorlastique de l'alliage CuZnA1 a 6t~ 6tudi~e par topographie en

rayonnement X synchrotron. La nature polychromatique de ce faisceau a 6t~ exploitre pour d~terminer,
exprrimentalement, les relations d'orientation entre les phases ,8 et 9R, A l'aide d'une mrthode inspir~e
par le travail throrique de Kajiwara, nous avons simul~ les orientations respectives et montr~ le caract~re
self-accommodant de cette transformation.

1. INTRODUCTION ation are usually calculated for one martensite vari-

For some years, considerable attention has been
given to martensitic transformation and more
specially to alloys of noble base metals, with a certain
composition range, which transform thermoelasti-
cally from the fl phase (b.c.c.) to the 9R structure
(monoclinic near by the orthorhombic structure) with
a stacking sequence "ABC BCA C A B . . . " . The
mathematical base theory of martensitic transform-
ations proposed by Wechsler et al. [1] and Bowles and
Mackenzie [2] has been applied in several attempts
to predict the crystallographic features of the fl to
9R transformations [3-5]. Suzuki [6] has developed
a simpler method to calculate these crystallographic
relations assuming the same strain condition (no
average distortion at the matrix-martensite interface
which must remain unrotated during the transform-
ation) than the previous attempts. More recently,
he has published a revised approach, easily applicable
to any system of martensitic transformation [7}.
Afterwards the Suzuki mathematical approach was
applied tO the transformation of the fl to the 9R
close packed structure and analytical equations
for the magnitude of the lattice invariant shear and
habit plane indices were derived by Kajiwara [8].
So, the crystallographic properties of the transform-
ant [4, 5, 8] and exceptionally for two variants [9, 10].
In a generalized mathematical model De Vos et aL
[11, 12] calculated all relevant crystallographic
characteristics for all the appearing variants and
especially the relationship between them. Because of
the symmetry of the parent ~ phase, 24 variants can
easily be deduced from one b.c.c, crystal. The 24
martensite plates do occur in a self-accommodating
manner, forming six variant groups, each of them
contains four cooperating martensite variants which
combine to produce a quasi zero net macroscopic
shape change.
The experimental verification of the validity of the
self-accommodating process is not an easy task. The
crystallographic relationships between the transform-
ation variants but also between the variants and
the matrix must be known. Owing to their great
number, such a characterization on polycrystalline
materials is difficult even impossible. Single or large
crystals were mainly studied. The relationships were
determined usually a posteriori optically from the
traces of the interphase boundaries at the crystal
surface, locally by electron microscopy or by X-ray
diffraction (Laue diagrams). Cu [5, 13-18], Fe [19]
and Ni [20] base alloys were studied by these
methods.

4213
4214 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-A1 SINGLE CRYSTAL--I
The self-accommodating process consists in the
grouping of four martensitic variants in order to
cancel the stresses resulting from the transformation
and to obtain a zero net macroscopic change. All
experimental methods cited previously were not able
to display these stresses. On the other hand, owing to
the reduced observation field of the electron micro-
scope, it is difficult to obtain information on the
nucleation centers. These are generally localized in
the thicker part of the sample. The relations between
the crystal structure of the parent phase and the
transformation variants are unexplored. For
example, no information is available on the relations
existing between the nucleation, the variant growth
and the crystalline defects of the parent phase and on
the formation and the growth out of a self-
accommodating group. Since some years ago, the
thermoelastic transformation has also been studied
by X-ray topography with conventional X-ray gener-
ators [21]. Two difficulties have made impossible the
in situ study of the transformation: a very long
exposure time ( > 24 h) due to the low intensity of the
X-ray beam and the impossibility, resulting from the
monochromaticity of the X-ray beam, to record
the diffracted beams of the low temperature phase.
The in situ and real time Synchrotron White Beam
X-Ray Topography (SWBXRT) technique is well
adapted to the study of the evolution processes of
bulk crystalline materials submitted to various treat-
ments. Its possibilities were used in several studies:
recrystallization [22], growth from the liquid phase
[23] and solid-solid phase transition [24]. It has been
shown in a first paper that this technique should be
applied successfully to the in situ and real time study
of the thermoelastic transformation of the shape
memory alloy [25].
In addition to the high flux of the beam which
reduces the exposure time to 1 s allowing the in situ
study of the transformation, two fundamental prop-
erties of this method have been exploited: the white
beam nature of the X-ray beam which allows one to
record simultaneously, on a same film, the diffraction
diagram of the two phases during the transformation
and the property of the topographic method which
visualizes at once the crystalline defects of the crystals
either in parent or transformed phases and so allows
one to establish the relations existing between them.
This last method has been used to study in situ and
in real time the thermoelastic martensitic transform-
ation of single crystals of Cu-Zn-AI shape memory
alloy. The results are presented in two papers. In this
paper, the crystallographic results are discussed. The
nucleation and the growth of the self-accommodating
variants have been analyzed by means of an original
method derived from the Kajiwara theory. In the
second paper, the topograms are analyzed in order to
show the connections between the crystal defects
structure during the fl to 9R transformation.
tL.U.R.E. Bat. 209 D. 91405 Orsay Cedex.
2. EXPERIMENTS
2. I. Crystal preparation
The appropriate alloy composition CuT~Znl6Als is
obtained by induction melting of electrolytical Cu,Zn
99.96% and AI 99.99% in an evacuated chamber
under a nitrogen rich atmosphere. Cylindrical ingots
were obtained by in situ pouring of the liquid alloy
into molds. The preoriented single crystals of /~
Cu-Zn-A1 were obtained by a modified Bridgrnan
method. Homogenization was carried out at 1123 K
in evacuated quartz tubes subsequently quenched in
water. In order to simplify the crystallographic analy-
sis, the atomic order is not taken into account: /~
phase is supposed b.c.c. (instead of DO3) and the
martensite is supposed 9R (instead of 18R). The M~
martensitic transformation temperature (M~ -~ 263 K)
was determined by Differential Scanning Calorimetry
(DSC).
The lattice parameters of the/~ and 9R cells are the
following [26]:
b.c.c./~ phase: aft = 0.2923 nm
monoclinic 9R phase: a = 0.440 nm
b= 0.2670 nm
c= 1.913 nm
fl0 = 1.54235 rad (88.37~
The fl and 9R terms are systematically used in this
paper to designate the parent and martensitic phases,
respectively.
Disk-shaped specimens of selected orientation for
X-ray diffraction were cut from the crystal ingot by
a diamond wheel cutter, mechanically polished with
fine grinding paper and finally electropolished. The
disks have a diameter of 10 mm and a thickness of
0.1 mm to provide the conditions of good contrast on
topograms are approached.
2.2. Synchrotron beam
The white synchrotron beam characteristics are
4 x 1 0 - 2 < 2 < 4 0 x 10-2nm with 2max= 1.6 x 10 -l
when the power of the D C I t ring is 2.9 x 10-1o j and
the intensity 3 • 10-I A. The cross-section of the
beam is circular with a diameter of 10-2m. The
diffracted beams can be recorded using either a TV
camera or films or nuclear plates. In the latter case,
the exposure time is the order of 1-5 s.
The large sections of the incident beam is an
important property of the synchrotron radiation. In
opposition to the one of the electron microscope, this
beam allows the study of the whole crystal submitted
to the temperature cycling.
2.3. Experimental technique
Experiments were made in a regulated ( + 0 . 2 K )
Peltier cell whose temperature can change from 233
to 323 K. To avoid the water condensation, during
the temperature variations, the cell is put inside a
chamber with a primary vacuum of 10-1 Pa. This cell
 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-AI SINGLE CRYSTAL--I
is built in such a way to allow the incident and
diffracted X-ray beams crossing.
Due to the high flux of the incident X-ray beam
in situ and real time studies are possible. The exper-
imental technique is such that, when the first nuclei
of the low temperature phase are detected, the tem-
perature is slowly decreased in steps of 0.2 K. To
follow the crystal structure evolution and the marten-
site plate growth, topograms are recorded at each
step on films or nuclear plates. The reverse transform-
ation is studied in the same manner as the direct one.
A computer program (Orient Express) has been
used to determine the crystal orientations from the
experimental Laue diagrams and conversely to simu-
late, from the crystallographic data, the diffraction
diagrams of crystals in 9R phase.
3. RESULTS
3. I. Diagram description
Figure 1 shows the diffraction diagram given by the
disk-shaped fl single crystal of CuZnA1. This diagram
is in fact a Laue diagram with the following
peculiarities: the Laue spots have the size of the cross
section of the incident beam which has been limited
to the size of the disk-shaped crystal with the aim to
obtain in the diffraction spot information on the
structure of the whole crystal. According to the fact
that the synchrotron beam is a parallel beam, as a
matter of fact each diffraction spot is a topography.
In Fig. 2 a succession of Laue diagrams is shown
which is recorded in the vicinity of the martensitic
start (Ms) point. According to the polychromatism of
Fig. 1. Diffraction diagram given by the single crystal in 13phase.
4215
the X-ray source, the diffraction diagrams of the fl
and 9R phases are recorded simultaneously on the
same film. In Fig. 2(a) (262.7 K) a single transform-
ation variant is present; in Fig. 2(b) (262.5 K) a
second variant appears; in Fig. 2(c) (262 K) four
variants are present. The diffraction spots of each
phase are easily identified: the spots of the fl phase
(initial state) are circular while the spots of the 9R
phase, given by the martensitic plates, are linear.
Moreover, in the fl spots, the white trace (lack of
diffraction) corresponds to the part of the fl crystal
which is transformed into 9R phase, therefore it is
possible to localize the nucleation of the plate and its
interactions with the fl structure. This fundamental
point will be treated in the second paper. Figure 2(d)
(261.5 K), at a further stage of the transformation
(however, less than half of the crystal is transformed),
shows the complexity of the diffraction diagram.
This paper is restricted to the crystallographic
study of the transformation.
3.2. Experimental results
From the crystallographic data (structure and size
of the unit cells), experimental parameters and coor-
dinates of the diffraction spots, it is possible with the
assistance of the computer program "Orient Express"
to determine the crystal orientations. With the same
software, the validity of the solutions can be checked
by the simulation of diffraction diagrams and their
comparison with the experimental ones. This data
processing is easily applied to the fl phase. In Fig. 3
the stereographic projection of the fl parent single
4216 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-A1 SINGLE CRYSTAL--I

Fig. 2. Diffraction diagrams realized during the /~--*9R transformation. This sequence displays the
appearance order of the transformation variants.

crystal is given. The determination of the orientations
of the 9R martensitic plates is not so easy. In the
direct beam, it is difficult to determine what part of
the incident beam has been diffracted by the marten-
sitic plates. This difficulty is increased by the fact that
the trace of the direct beam on the film is surrounded
by a diffusion blurring (see Figs 1 and 2). The
resulting dubiousness in the determination of the
coordinates of the fl diffraction spots involves an
uncertainty in the orientation determination. This
difficulty has been overcome by development of an
original method using together the experimental
tThe traces of V3 and V~ are practically parallel and
apparently intermixed on this topogram.
topographic results and the theoretical work of
Kajiwara.
In Fig. 3, the stereographic projection relative to
the orientation of the crystal in fl phase and the
photographic enlargement of the 231 reflection have
been placed together and positioned in order to
respect their relative positions. In the 23T reflection
the traces of the transformation variants are clearly
visible; they are parallel to the intersections of the
habit planes of the variants (V~ . . . . . V4) with the
surface of the sample. The habit planes in the 9R
structure are close to the { 110}/~ planes therefore the
{011 } poles corresponding to these habit planes must
be close to the direction of the normal to these traces.
It is seen in Fig. 3(b) that the direction of the normal
 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-AI SINGLE CRYSTAL--I 4217

Fig. 3. Stereographic projection of the single crystal in fl phase and 231 reflection. The relative positions
have been respected and the normals to the variant traces have been drawn: (a) 23]" diffraction spot;
(b) stereographic projection.

to the VI, 112 traces [Fig. 3(a)] are close to the (10i)
pole and for V3,V4t close to the (0ii) pole.
3.3. Theoretical analysis
In this paragraph, the results of the theoretical
analysis of the crystallography of the/~ to 9R trans-
formation of Kajiwara [8] will be applied to our
experimental case. The crystallographic orientations
of the transformed variants from the/~ single crystal
will be calculated and their diffraction diagrams
simulated. The results of this simulation will be
compared to the experimental diffraction diagrams.
All the orientations of the 24 variants will not be
calculated but the research will be limited to the two
groups of four variants for which habit planes are
close to the (10T) and (01i) poles of the/~ phase.
The Kajiwara treatment allows one to calculate
the crystallographic characteristics of a variant, VAt
for example, with respect to the /~ parent phase.
The 9R unit cell is taken as an orthorhombic cell.
This treatment has been applied to the /~ to 9R
martensitic transformation of the CuZnAI alloy
tin VA 9I'D, the A ... D subscripts are used only in the
theoretical approach while the a ... d subscripts are
relative to the experimental results.
tested in this study. With the crystallographic data
given in the previous chapter, the direction cosinus
of the habit plane normal (h.p.) and of the shear
vector d parallel to this plane have been calculated.
They are h.p. VA: X =0.133, y =0.673, Z =0.727,
dVAX = 0.022, y = -0.134 and z = 0.121.
It is seen that the (xyz) habit plane is close
to (011)~ for the VA variant. Using the symmetry
properties of the lattice, the three other self-
accommodating variants, VB, Vc and VD, around the
(011) pole can be determined. They are (Yyz)VB,
( x z y ) V c and (Yz)')VD, then ( - 0 . 1 3 3 0.673 0.727)VB,
(0.133 0.727 0.673)V c and ( - 0 . 1 3 3 0.727 0.673)V D.
dVB, dV c and dV D are calculated in the same
manner. (0.022 - 0.134 0.121 )dVA, ( -- 0.02 -- 0.134
0.121)dVB...
From Kajiwara, with the matrix MA relative to the
variant VA, it is possible to index in the initial fl phase
any lattice plane of the 9R martensite
(hkl)~ = (hkl)gR[MA]. (1)
Therefore, if the (001)9R, (100)9R and (010)9R planes
of the variant VA are positioned with respect to the
initial orientation of the crystal in/~ phase, the relative
positions of the two unit cells (/~ and 9R) will be
known.
4218 J O U R D A N et al.: TRANSFORMATION OF A Cu-Zn-A1 SINGLE CRYSTAL--I
Table 1
(10i)a Va Vb Vc Vd
y x f y s f z x fi z s f
(0019R)~ 6 w 91 ~ 99 91 91 99 6 91 99 6
(0109R)# 99 ~ 9 w 2 9 w ] 99 w 2 99
(oii b vc vr vg vh

(0019R)# ~9 6 91 99 6 w w w 6 99 91 6
(0109R)# ~ 99 9 2 99 9 ~ 9 99 2 9 99

The MB, Mc and MD matrices which give the
relative orientations of the orthorhombic unit cells of
the VB, Vc and VD variants with respect to the same
initial /~ cubic unit cell are obtained from the
symmetry operations previously described.
Such a mathematical approach can be generalized
to the self-accommodating variants groups around
any {110}/~ plane.
3.4. Application
The numerical values of the matrix [MA] are the
following
to be grouped either around the (10T)B or (0]'T)~
planes. Using the previous results, the (001)9R and
(010)9 R indexes of the planes of the four self-
accommodating variants around (10i)~ are calculated
in order to calculate in fl phase the poles of these
planes. This is done keeping in mind that indexes xyz
correspond to the (011)~ plane. Using the relation (3)
the corresponding numerical value has been
attributed to these indices (Table 1).
The indexes of the four self-accommodating vari-
ants grouped around the (0Ii)p determined by means
of the same method are given in the same table.

(hkl9R )~ = (hkl)9 R 3.5. Simulation

-0.434839 0.051786 -0.498906
x -0.017931 - 1.09026 -0.097539.
-0.112577 -0.007375 0.10314
Then we are able to index in fl phase the (001)9 R
and (010)9R planes. However, to simulate the theoreti-
cal solutions found, we must enter in the "Orient
Express" program indexes with "integer" lower than
100. The values are normalized in such a way that the
greatest is equal to 99. Then
(0019R)# = (-0.112 -0.007 0.103)a # (99 ~ 91)a
• (0109R)a = (--0.017
-- 1.090 --0.097)B ~ (2 ~9 9)p.
The validity of the numerical values of the matrix
[MA] can be verified. From the phenomenological
theory, it is known that the (114)9R plane is parallel
to the (011)a plane. Then, if (1T4)9R is indexed in/~
phase by means of the matrix [MA], the (011)~ plane
must be found
(ll4)gR[MA] = (0.00246 1.00897 1.009006)a
which is very close to (011)a. The angle between the
two planes is given by
cos(011)~(1149R)t~ = 0.999998.
In our experiments, it has been shown that the 9R
habit planes of the transformed variants are supposed
t l f the numerical values of the indexes are exact, their
algebraical sign can be wrong. Indeed, during the differ-
ent crystallographic operations (x to x, y to y . . . and
rotations), the modifications of the reference axis have
not been taken into account in Table 2.
The method used to simulate the diffraction
(2) diagram of the self-accommodating variants is
illustrated for the lib variant.
(1) In the stereographic projection relative to the
initial orientation of the single crystal in fl phase, the
position of the (0019R)~ and (0109R)~ planes of the Vb
variants have been indicated, Fig. 4(a). Indexes
of these planes are respectively: ~ 99 w and w 2 9
(Table 1).
(2) By means of rotations, the poles of these planes
are respectively led to the center and to the intersection
of the y axis with the sphere of the stereographic pro-
jection. With the conventions indicated in the Fig. 4,
X = 80~ Y = --33 ~ and Z = - 5 8 ~ [Fig. 4(b)].
(3) (3) With the Orient Express program, the stereo-
graphic projection of the 9R unit orthorhombic cell
is simulated in such a way that the (001)9 R and (010)9R
poles are, respectively, positioned at the center and at
the intersection of the Y axis with the sphere of the
stereographic projection [Fig. 4(c)].
(4) The superposition of the Figs 4(b) and
(c) shows that the (0019R)p and (0109R)/~ poles are
respectively superimposed with the (001)9 R and
(010)9R poles.
(5) The relative positions of the 9R and/~ unit cells
in this experimental study are found in submitting the
unit 9R cell, which orientation is given in Fig. 4(c),
to reverse rotations to the upper ones. The orien-
tation of the lib variant given in Fig. 4(d) has been
obtained after reverse rotations Z = 58 ~ Y = 33 ~ and
X = - 8 0 ~ The orientation relationships between the
two phases are given by the superposition of the two
stereographic projections [Figs 4(a) and (d)]; the
0"14)9R'~ plane is superimposed to (10i)~ and (001)9 R
basal plane is close to (0ii)p plane.
 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-Al SINGLE CRYSTAL--I 4219

X>O

Z>O

1 Y>O

a b

100

C d
Fig. 4. (a) Stereographic projection of the initial single crystal. The (0019R)# and (0109tt)t~poles have been
added. (0019R)# = ~ 99 w and (0109R)# = w 2 9; (b) stereographic projection of Fig. 4(a) after rotation
so as to (0019R)# pole should be at the center of the projection and (0109R)# at the periphery. X = 80~
Y = - 3 3 ~ Z = -58~ (c) stereographic projection giving the orientation of the unit orthorhombic cell
with (001) pole at the center and (010) pole at the periphery; (d) stereographic projection giving the
orientation of the Vb variant in accordance with the fl parent phase. Habit plane has been indicated by
a star.

(6) The crystallographic orientation of the Vb
variant known, its Laue diagram has been
simulated and compared to the experimental
diagram to verify the validity of the solution
found.
Each variant (Va . . . Vd and Ve . . . Vk) has
been studied in a same way. The results are gathered
in Figs 5 and 6. Figure 5 is relative to the self-
accommodating group which habit planes are close to
the (10T)p pole and Fig. 6 is relative to the self-
accommodating group which habit planes are close to
the (0TT)p pole.
In Figs 5 and 6, Figs 5(a) and 6(a) give the
experimental orientation of the parent crystal of fl
phase, Figs 5(b) and 6(b) give the simulated stereo-
graphic projections of the self-accommodating vari-
ants and Figs 5(c) and 6(c) give their simulated Laue
diffraction diagrams.
 4220 JOURDAN et al.: T R A N S F O R M A T I O N OF A C u - Z n AI SINGLE C R Y S T A L - - I

C
- ~ ~ ~ ~ ~ ~ ~
~ ~ ~ ~176 ~ ~176 ~ ~
~ ~ ". ~ . 9 . ~ ~

.
9 . . . . . - : "o~"
..
: . : - - ~"o~:
- "": ~ ..":~.
,"-
": ".2"t~'r~
" a . r .". "
.... " " : ~ - '-:" k;-" "" .o'
9 .. "'- .eli-s,.. 9 -
" " " " 9 001 ....... ::7"-.. ~ ':.:..-'-'...'-'-
. . . . . .~ 1 7 6 . . ... -" ' . "~- . -~
o~,~,~-.'..
9 - -
114 + 9
9 9 1~- . 9~ .-- , , - . ~. ,~ .. . . ~ ."- . - ..'- .. . ' :" %. ~L ~ .7 ."
- _ .- .::..::-...: ..-- ~,,

9 . ~ ~ ~ .~149
9 ~ . ~
. ~ r.

9 . .~

:. .:i - . .-
001
"'-..
".i:."-i
-.-.-'.. ! -_.:3-"
eQ
- . . 9 ~. "'. 9 .~e--"
9 " ~ 1 7 6 1 7 6 1 7 6~114499 1 4"9 ~ ...

i'14 +
111 r
1, 9 . ~ 1 7 6 1 4a 9. ~ 1 7 6 ~ , %~ 9

101
% 9 ....;.,.-- - \
- . . ? - \
001
~'
011
~149
...

110 ~t
o~o
Va

IO0
9 9

~ 82
9 -o......-"

O01
k. Q Q
0 OO

Vc

1OI

9 9

O go

114 ~ 9
001
~t .... ~"" ( ~ ~ 1 7 6 . N ~ .....

- X
OO0 9 9 -'" .-" \ .
Vd
Fig. 5. Simulated results relative to the Va, lib, Vc and Vd variants grouped around the (10i)p pole.
(a) Stereographic projection relative to the orientation of the single crystal in/] phase; (b) simulation of
the stereographic projection of the self-accommodating variants grouped around the (101")~ pole, Va, Vb,
Vc, Vd; (C) simulation of their diffraction diagrams.
 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-A1 SINGLE CRYSTAL--I 4221

b c
9 o 9 ca4 9 9 9 41 4# 9 ~

e e o e e 4 e ~ o ==~6~ ~ ~ ,%~
e'~ ee e~ ~eee 9 oj 9

001

.. : - ' : . . . . " .

..
,0 9 114
-\ ,.

./ ,,
i

ve o.
9 o

9 ~176 ~ 9 9

9/ - ~

- ".'."-"..::.':'"- t .- -.
. - .o . ' . % o .
6
"-. .,-- ":" . ' , P ." - ' - : ' 2 - "
9 . . - ...:::,, ..,,,.
: 514 9
.-...,.--,:~:!i~:i
- :.'-:..-:" . . . .'.-':---
or .-. -. ~ ; .- . . - . ~
* . ;.;. %. % . t 4 t .." ~ ' . " 9176
o
111
. -. ... "~ ! -...'.." ...
O
101 ~ ~ o .. ~176 9 ~ .9 .- -.

~ . ., .

.
.

.
9
..-
9
."
j
]
4 ~'- ~ 9
.~.
","
9 .
-

. .
-
"

~
9 ~ . | ,- . 9 ~
~176

oo~ o]1-~"" 9 r .9 "

~o~ _ ~ ~o
9 0
110

,oo
9
~ \ / O0 ~

:i:7-'::'.:-".. 9 . oo,
041

9 9 9 9 9 9 q /
W'!" ..............
~
". . . . . o
~ . 9

"-- .. Z"
". " - 2 ...... ' " @ "" .,-.-!~
""-.";:'7!:::-.-...':" :.: : :
......

. o . ,
9 t :'~ ~-.
.. * o'. ". " ,

o . 9 # "-o
. . . . '. 9

Fig. 6. Simulated results relative to the V~, Vf, Vg and Vh variants grouped around the (0]T)~ pole.
(a) Similar to Fig. 5(a); (b) simulation of the stereographic projections of the self-accommodating variants
grouped around the (oIr)~ pole. v~, vf, Vg and Vh; (C) simulation of their diffraction diagrams.
4222 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-AI SINGLE CRYSTAL--I

Fig. 7. Topograms in white beam realized during the fl---~9R transformation: (a) 262.7K one
transformation variant; (b) 262.5 K two transformation variants; (c) 262 K four transformation variants;
(d) 261.5 K.

The comparison with the experimental results in unambiguously. The crystallographic relationships
Fig. 7 indicates that it is possible to make the connec- between parent and transformed martensite plates are
tion between the experimental and simulated results. deduced from Figs 5 and 6.
The transformation variants are grouped by self-
Figure 7(a): Vl is similar to Va [Fig. 5(c)] accommodating pairs. Indeed, the habit planes of V~
Figure 7(b): V2 is similar to Vd [Fig. 5(c)] and V2 are close to the (10i)a plane and the habit
Figure 7(c): V3 is similar to Vg [Fig. 6(c)] planes of V3 and V4 are close to the (0ii)8 plane. For
Figure 7(d): V4 is similar to Ve [Fig. 6(c)] convenience in the discussion to verify if the vari-
R e m a r k : To detect easily the diffraction diagram
ant-variant and variant-parent crystallographic re-
given by a same variant in Fig. 7, the diffraction spots lationships found in our experiments and if their
given by other variants have been masked. Therefore morphologies are consistent with the previous obser-
in Fig. 7(c) the diffraction spots relative to the V1-V 2 vations, in the standard stereographic projection of
variants have been masked to display the diffraction the fl phase (Fig. 8) which reproduces the notations
spots relative to V3. Their visibility is also increased by used by Saburi and Wayman [13], the numbers 1 ~
the crystallographic indices. To highlight the variant specify the parent close-packed planes which generate
considered the center of the diffraction diagram has the basal planes of the martensite variants. Each
been intentionally shifted [Figs 7(c) and 7(d)]. number can appear with or without prime symbols
when the transformation variants have a common
4. DISCUSSION OF RESULTS basal plane but opposite transformation shear-direc-
tions. The positive or negative sign differentiates two
According to the cross-checking of the experimen- crystallographic equivalent habit planes [13, 14].
tal and theoretical data, the crystallographic charac- A self-accommodating group has habit plane
teristics of the fl to 9R transformation can be given normals clustered about one of the six {110} poles of
 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-AI SINGLE CRYSTAL-- !
~OO
~. 5+ 6"-
5"-4~ 4~- 6 -
0"1~ ~ i - Gall 2+ "-
". 101, ' 4 .
100
Fig. 8. Standard stereographic projection of the single
crystal studied. The habit planes of the transformation
variants have been noted with the Saburi notations. The
arrows indicate the microscopic deformations induced
by the transformation variants after Schroeder and
Wayman [16].
the parent phase [16]. Among the four variants in
a group, there are three types of twin relations
which are well described by the diamond-shaped
self-accommodating plate group [16].
From the phenomenological crystallography the-
ory, the (xyz) indices of V A variant have been calcu-
lated. They are respectively equal to (0.13, 0.67, 0.72).
Then the (yxz-) habit plane indices of the V, exper-
imental variant are (0.67, 0.13, - 0.72): Table 1. The
comparison of these indices with the habit planes
indexes for 24 martensite variants, relative to parent
phase given by Saburi [13] (Table 2, Saburi, p. 18),
shows that the Va variant corresponds to the 2(+)
variant. In a same way the indices of the Vd exper-
imental variant which are (0.72, -0.13, -0.67),
indicate that this variant is the 6 ' ( - ) variant of
Saburi. These two variants 2(+) and 6 ' ( - ) belong to
the same II self-accommodating group (Table 3,
Saburi, p. 19), with their self-accommodating habit
planes grouped around 701 (or 107), Fig. 8 (Table 1,
Saburi, p. 17) gives the original basal planes of the
2(+) and 6 ' ( - ) variants which are respectively,
(011)# (or 077) and (110)~ (or 770). These last
results are in full agreement with our experimental
observation where Va = Vl and Vd = V 2.
Figure 9 shows the diamond-shaped diagram rela-
tive to the four self-accommodating variants clus-
Table 2
Experimental Habit plane 9R
variants close to basal plane {011}~
V~ (10I)#//(114)9 R * (001)9 R
V2 (10I)6//(114)9a (001)911
V3 (0iT)a//(11_~)9 R (001)9 R
V, (0I'T)B//(114)9a (001)9a
4223
(loV)s
!OlO
/
Fig. 9. Diamond-shaped diagram applied to VI-V2 trans-
formation variants.
tered around the (i01)a (or 10i)t~ pole [141 (Saburi,
Fig. 3, p. 981) in which the 2(+) and 6 ' ( - )
experimental variants appear.
The variants Ve and Vg have been studied in a same
manner. Only the results are given
h.p. Vo: (xyz)=O.13, -0.67, - 0 . 7 2 ) - - , 4 ' ( + ) - - * V4
h.p. Vg: (x~f) = 0.13, -0.72, -0.67) ~ 6 ( - ) ~ 1/~.
4 ' ( + ) and 6 ( - ) belong to group III with their
self-accommodating habit planes grouped around
(011) (or 0ii) Fig. 8. (10De and (110)/~ (or i0i and
110) are the basal planes of 4'(+) and 6 ( - ) , respect-
ively, which is in agreement with the experimental
observations. The diamond-shaped diagram relative
to group III is given in Fig. 10.
From these diagrams, we can foresee the mor-
phology of the variants and their crystallographic
relations.
The diamond-shaped diagram is divided in four
parts labelled A, B, C and D. When the variant A (or
D) appears, it is followed by the nucleation of the
variant C (or B). These variants are in twining
position, the twining plane being the symmetry plane.
A spear morphology characterizes the A C or D-B
pair. Our observations indeed confirm these phe-
nomenological approach. Vl, //2 are the variants 2
and 6 or D and B and their morphology, Fig. 3, is a
spear morphology. They are twin-related with respect
Close to to the (T01)r plane (or 10i).
A similar analysis applied to V3, V4 variants shows
(01]')#
(110)# the presence of the C-D pair. This result confirms the
(110) 8 difficulty found in their differentiation from the fl
(TOT)a diffraction spot because, in the wedge morphology,
4224 JOURDAN et al.: TRANSFORMATION OF A Cu-Zn-A1 SINGLE CRYSTAL--I
100)/3
Fig. 10. Diamond-shaped diagram applied to V3-V4 trans-
formation variants.
the two variants are joined side by side. They give, in
the fl diffraction spot, a single trace, Fig. 3. In the
opposite way, the 9R diffraction spots are well separ-
ated, Fig. 7. A careful examination of the diffraction
diagrams does not allow one to determine with
certainty the apparition sequence: V3 followed by V4
or V4 and I/3. These variants are related with respect
to a plane close to the (011)~ (or 0T1) plane.
The four variants observed do not belong to the
same self-accommodating group but they are clus-
tered by pairs round (T01)~ and (011)~ poles. If the
scheme of the microscopic deformation, indicated
through the rotation of a vector during the defor-
mation [12-16], is drawn for each pair of V,-V2
and 1/3-114 variants, Fig. 8, we see that for V~-V2 or
V3-V4 the compensating rotation of the (100) axes
illustrates the self-accommodating character of each
pair.
The self-accommodating theory does not take
into account the reality of the experimental case:
the CuZnA1 matrix is not isotropic, the sample has
finite dimensions and several crystalline defects are
present. So, it is not surprising that when the trans-
formation starts the four self-accommodating vari-
ants clustered round the (10T)a pole should not be
observed.
The geometrical approach shows that the [101;]~
and [01T]p normals make, respectively, 34~ and 28 ~
with the great surface of the sample. Therefore, if the
surface influences the variant formation, it can be
accepted that the two self-accommodating groups are
activated. On the other hand, the Saburi notation
indicates that V2 and V3, respectively, 6 ' ( - ) and
6 ( - ) have a (001)9R common basal plane with oppo-
site transformation shear directions. It can be sup-
posed that local crystalline heterogeneities have
activated these opposite shear directions. As soon as
1/3 has nucleated, the self-accommodating process
starts also round the (oTT)B pole. This remark
indicates that the apparition sequence for V3-V~
must be II3 followed by V4. The result is the division
of the single crystal in two parts with different
self-accommodating groups.
The role of the crystalline defects will be discussed
in the second part of this paper.
5. CONCLUSION
The /3 to 9R transformation of a single crystal
of CuZnA1 has been followed in situ and in real
time by synchrotron X-ray topography. The white
nature of the beam permits one to register, on a same
film, the diffraction diagrams of the fl and 9R
phases and leads access to different crystallographic
relations (variant and parent phase and vari-
ant-variant).
An original method deduced from the theoretical
work of Kajiwara has been used to simulate theoreti-
cally the diffraction diagrams of the four transform-
ation variants clustered round each of the two {011 }a
poles. The comparison between the simulated and
experimental diagrams has permitted one to deter-
mine unambiguously the crystallographic orientations
of the transformed variants and to show that the
transformation proceeds by nucleation and growth of
self-accommodating variants associated by pairs.
From previous works [13, 14, 16], it has been
shown that when a single crystal is fully transformed
in low temperature phase it is divided in several
regions. Inside each region a self-accommodating
group is prevailing. In this study, it has been shown
how the first variant can activate a self-accommodat-
ing group in one region of the crystal and another
self-accommodating group in another region. The
role of the crystalline defects of the parent phase must
be taken into account in this action. This last point
will be discussed in the second part of this study.
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