The Early Stages of GP Zone Formation

in Naturally Aged AI-4 Wt Pct Cu Alloys

R. J . RIOJA AND D, E. LAUGHLIN
The e a r l y s t a g e s of the r o o m t e m p e r a t u r e decomposition of s u p e r s a t u r a t e d solid solutions
of A t - 4 wt pct Cu a l l o y s have been i n v e s t i g a t e d . Diffuse s a t e l l i t e s have been found to flank
fundamental r e f l e c t i o n s in e l e c t r o n diffraction p a t t e r n s p r i o r to the formation of the
p t a t e l i k e GP zones. These a r e h e r e i n i n t e r p r e t e d as evidence for the o c c u r r e n c e of
spinodal decomposition at r o o m t e m p e r a t u r e . The development of GP zones f r o m the
modulated m i c r o s t r u c t u r e is documented by the bright field and weak beam d a r k field
techniques, This continuous formation of GP zones is then i n t e r p r e t e d in t e r m s of Cahn's
l a t e r stage spinodal theory.

THE decomposition p r o c e s s in A1-Cu a l l o y s is one m i s s i o n e l e c t r o n m i c r o s c o p y , and if so to a s c e r t a i n if

which has r e c e i v e d an unusual amount of attention.
The independent works of Guinier I and P r e s t o n 2 were
the f i r s t to show that coherent p l a t e l e t s of copper
(now called GP zones) f o r m on the {100} planes of
the aluminum m a t r i x p r i o r to the formation of the
m e t a s t a b l e 8" and O' p h a s e s .
The sequence of these r e a c t i o n s has been r e v i e w e d
frequently (see e.g. Ref. 3). In this p a p e r we s h a l l
only consider the p r o c e s s e s which occur b e f o r e and
during the formation of the GP zones during n a t u r a l
aging (viz room t e m p e r a t u r e aging).
After Cahn published his initial work on spinodaI
decomposition, 4 w o r k e r s in the field began to s p e c u -
late that the GP zones may f o r m v i a the spinedal
m e c h a n i s m . Indeed, the final m i c r o s t r u c t u r e was
o b s e r v e d to be somewhat s i m i l a r to that p r e d i c t e d
by the theory, 5 having p a r t i c l e s that w e r e aligned
along the e l a s t i c a l l y soft d i r e c t i o n s , and somewhat
p e r i o d i c a l l y spaced. However, the composition p r o -
f i l e s for GP zones a r e step functions of n a r r o w
width (about one atomic plane thick), w h e r e a s the
e a r l y s t a g e l i n e a r t h e o r y of spinodal decomposition
p r e d i c t s r a t h e r diffuse, p e r i o d i c modulations.
C l e a r l y , the GP zone f o r m a t i o n could be p r e c e d e d
by spinodat decomposition. However, t h e r e was no
e x p e r i m e n t a l evidence that it was. If spinodal d e c o m -
position does p r e c e d e the formation of the GP zones,
s a t e l l i t e s in r e c i p r o c a l space (or sidebands on Debye-
S c h e r r e r diffraction p a t t e r n s ) p r e s e n t because of
modulations of composition in r e a l space, should be
o b s e r v e d . Until r e c e n t l y , no such o b s e r v a t i o n s
were reported.
N e v e r t h e l e s s , w o r k e r s continued to r e p o r t " h i n t s "
that the f o r m a t i o n of GP zones may occur in a con-
tinuous manner. Asana and Hirano ~ for example found
anomalies in electrical resistivity measurements at
and below 40~ (313 K). Some calorimetry work7
showed that abnormal changes occurred in the rate
of release of heat below the coherent GP solvus. And
finally, the recent X-ray work of Naudin%9and co-
workers has shown that satellites apparently occur
near the fundamental reflections in AI-Cu alloys.
This work was undertaken to ascertain if satel-
lites in the A1-Cu system are observable by trans-
R. J. RIOJA is a Graduate Student and D E. LAUGHLIN is Assis-
tant Professor, Department of Metallurgyand MaterialsScience,
Carnegie-MeltonUniversity,Pittsburgh, PA 15213.
Manuscript submitted November 24, t 976,
they a r e due to composition modulations or if they
a r e due to the i n t e r s e c t i o n of the Ewald s p h e r e with
diffuse (110> r e l - r o d s , as has been r e p o r t e d in the
Cu-Be s y s t e m . 1~ F u r t h e r m o r e , the m e c h a n i s m and
sequence of the development of GP zones from the
modulated m i c r o s t r u c t u r e was to be investigated.
EXPERIMENTAL PROCEDURE
High purity aluminum 4 wt pct copper a l l o y s were
solution t r e a t e d in an argon a t m o s p h e r e in a tube
furnace at 540~ (813 K) for 5 h. The s p e c i m e n s
were quenched in water at r o o m t e m p e r a t u r e and
aged for v a r i o u s t i m e s at r o o m t e m p e r a t u r e ,
D i s c s 3 mm d i a m were punched out of the sheet,
and thin foils w e r e p r e p a r e d by the double ]et e l e c -
t r o p o l i s h i n g technique, using a o n e - t h i r d n i t r i c acid,
t w o - t h i r d s methanol solution a t - 25~ (248 K).
A J E M 100B e l e c t r o n m i c r o s c o p e equipped with a
double tilt stage was used to o b s e r v e the a l l o y s . The
s h o r t e s t aging t i m e p o s s i b l e at r o o m t e m p e r a t u r e
was about ten minutes, b e c a u s e of the time needed to
t r a n s p o r t the s a m p l e to the polishing solution, and
from the polishing solution to the m i c r o s c o p e .
Weak b e a m photographs u w e r e taken by satisfying
the (020) B r a g g r e f l e c t i o n , and tilting the r e f l e c t i o n
into the axis of the column. This r e s u l t e d in the
(060) r e f l e c t i o n being s a t i s f i e d . The s value for this
condition, in A1-Cu alloys is about 0.9 • 10"l nm -1.
Throughout the p a p e r this condition will be r e f e r r e d
to as the (020), (060) weak beam condition. Exposure
t i m e s v a r i e d from 15 to 60 s. Diffraction p a t t e r n s
w e r e taken with a well defocused condenser tens,
for t i m e s of 30 to 150 s.
RESULTS
The as-quenched, solution-treated samples showed
no evidence of decomposition. Strong two-beam
bright field microscopy as well as weak b e a m dark
field microscopy (g = (020), (060)) failed to detect
G P zones or modulations. The diffraction patterns
consisted only of spherical fundamental reflections.
No s a t e l l i t e s or <100> s t r e a k s were detected (see
F i g . 1).
Aging at r o o m t e m p e r a t u r e caused the s u p e r s a t u -
r a t e d solid solution to d e c o m p o s e , The f i r s t evidence
of this decomposition o c c u r r e d a f t e r five hours of
aging, and was detected by the o b s e r v a t i o n of diffuse

METALLURGICALTRANSACTIONSA VOLUME 8A, AUGUST I977-I257

s a t e l l i t e s at a l l f u n d a m e n t a l r e f l e c t i o n s . T h e s e a r e
shown in F i g . 2. T h e s e s a t e l l i t e s in r e c i p r o c a l s p a c e
i m p l y t h e e x i s t e n c e of r e a l s p a c e m o d u l a t i o n s . The
s a t e l l i t e s a r e a b s e n t f r o m r e f l e c t i o n s when g . Ss = 0,
w h e r e Ss is the v e c t o r f r o m g, the f u n d a m e n t a l r e -
flection, to the s a t e l l i t e p o s i t i o n in q u e s t i o n . T h i s
m e a n s they a r i s e f r o m s t r a i n m o d u l a t i o n s 'e which
a r e p r e s e n t b e c a u s e of c o m p o s i t i o n m o d u l a t i o n s .
T h e i r d i f f u s i v e n e s s c o r r e s p o n d s to m o d u l a t i o n s of
wavelength v a r y i n g f r o m 4.0 to 8.0 nm. T h e l a c k of
a (t00) s t r e a k in r e c i p r o c a l s p a c e , a s w e l l a s the
l a c k of o b s e r v a t i o n of GP z o n e s in b r i g h t f i e l d and
w e a k b e a m mode shows that the z o n e s a r e a s y e t not
present.
T h e f a c t t h a t t h e r e l a t i v e i n t e n s i t i e s of t h e s a t e l -
l i t e s i n c r e a s e with g (cf t h o s e at (040) to t h o s e at
(020) in F i g . 4) i s a l s o i n d i c a t i v e of t h e i r o r i g i n , a s
only s a t e l l i t e s which a r i s e f r o m m o d u l a t i o n s in
s t r a i n follow t h i s p a t t e r n . C a r e m u s t be taken how-
e v e r when i n t e r p r e t i n g r e l a t i v e i n t e n s i t i e s s i n c e the
i n t e n s i t y of the s a t e l l i t e s is a l s o s o m e w h a t d e p e n d e n t (a)
on the c r y s t a l o r i e n t a t i o n .

002

/.;,," ,- : . t
., , r

*b " J "'
o " ', ,t
e
"r
000 020
",
,I |
*. ~ ,oo nm
I III I

9 t 9
Fig. 1--The [100] diffraction pattern of an as-quenched At-4
wt pct Cu alloy, The fundamental reflections are round, show-
ing no evidence of s a t e l l i t e s or (110} t e l - r o d s . (100) s t r e a k s
are also absent.
(b)
Fig. 3--The m i c r o s t r u c t u r e of an A1-4 wt pet Cu s a m p l e aged
for 168 h at room t e m p e r a t u r e . (a) Bright field, g = (020),
showing (110} tweed; (b) weak beam dark field, s = 0.09
nm -1 ((020), (060) case). The GP zones show up as bright r e -
gions in the weak beam photographs. Zone axis near [1001.

B
000 020 0 4 0
020 000 020

Fig. 4--The [100] diffraction p a t t e r n of an A1-4 wt pct Cu alloy

Fig. 2--A section of the [100] diffraction pattern of an AI-4 aged for 672 h at r o o m t e m p e r a t u r e . The intensity of the
wt pet Cu alloy aged for 5 h at room temperature. Notice s a t e l l i t e s has i n c r e a s e d . See the (020) reflection and c o m -
diffuse satellites at the (030) reflection. p a r e with the (020} of Fig. 2.

t258-VOLUME 8A, AUGUST t977 METALLURGICAL TRANSACTIONS A

 Another s t r i k i n g f e a t u r e of the s a t e l l i t e s is t h e i r
m a r k e d i n t e n s i t y a s y m m e t r y (cf the two s a t e l l i t e s
flanking the (040) in Fig. 4). T h i s can be explained
by noting that the Cu depleted r e g i o n s p r o b a b l y con-
t a i n m o r e s t r a i n than the Cu e n r i c h e d r e g i o n s . Since
the i n t e n s i t y of a s t r a i n - i n d u c e d s a t e l l i t e is p r o p o r -
t i o n a l to the value of the s t r a i n s q u a r e d , the r e g i o n s
with the g r e a t e r s t r a i n (viz Cu depleted ones) should
give r i s e to the m o r e i n t e n s e s a t e l l i t e . T h e s e Cu
depleted r e g i o n s have a g r e a t e r a v e r a g e l a t t i c e
p a r a m e t e r ; hence the low angle s a t e l l i t e s a r e m o r e
intense.
After aging for one week at r o o m t e m p e r a t u r e faint
(110) tweed is o b s e r v e d i n the b r i g h t field mode
(Fig. 3(a)). T h i s c o n t r a s t has b e e n s a i d t o a r i s e f r o m
e l a s t i c i n t e r a c t i o n s due to t e t r a g o n a l l y d i s t o r t e d
it
J
(a)
|loonm |
(b)
Fig. 5-The mierostructure of A1-4 wt pct Cu aged at room
temperature 672 h. (a) Bright field, g = (020), showing small
(~ 3 nm) GP zone platelets. Notice the black-white contrast;
(b) weak beam dark field, s = 0.09 nm-1 ((020), (060) case).
GP zones show up as bright lines9 Zone axis near [100].
METALLURGICAL TRANSACTIONS A
r e g i o n s (as of GP zones) a l i g n e d in a s t a i r s t e p
fashion. ~3 The 3.0 n m GP z o n e s a r e shown in F i g .
3(b), as i m a g e d by the weak b e a m technique. The
white r e g i o n s c o r r e s p o n d to the z o n e s .
Aging four weeks at r o o m t e m p e r a t u r e r e s u l t e d in a
l a r g e i n c r e a s e in i n t e n s i t y of the s a t e l l i t e s (see F i g .
4). Also, GP z o n e s b e c o m e m o r e r e a d i l y o b s e r v a b l e ,
for e x a m p l e at the a r r o w s of F i g . 5(a) and (b). T h e
zones a r e v e r y s m a l l , ~3 to 8 n m i n d i a m . They a r e
b e s t s e e n by the weak b e a m technique (Fig. 5(b)).
Yoshida, Cockayne and Whelan ~4 have r e c e n t l y shown
that GP zones 3.5 to 10 n m a r e v i s i b l e by this tech-
nique. T h e s e r e s u l t s r e a f f i r m t h e i r c o n c l u s i o n s . Our
r e s u l t s d i f f e r e d f r o m t h e i r s s o m e w h a t though, i n that
the GP zones a p p e a r e d a l m o s t e x c l u s i v e l y as s i n g l e
b r i g h t l i n e s , w h e r e a s in t h e i r work, p a i r s of b r i g h t
l i n e s were m o r e f r e q u e n t l y o b s e r v e d .
The (100) s t r e a k s in the d i f f r a c t i o n p a t t e r n for the
alloy also show the GP zones a r e p r e s e n t . They are
diffuse, b e c a u s e of the s m a l l GP zone d i a m e t e r . The
a,.
f 020
0 Ca)
J
k~.e' "
(b)
Fig. 6--[1001 diffraction p a t t e r n s of A l - 4 w t pet Cu alloy.
(a) Aged 1128 h at r o o m t e m p e r a t u r e . Notice diffuse (100)
s t r e a k s ; (b) aged la0 ~ for 16 h. Notice s h a r p (100} s t r e a k s .
VOLUME 8A, AUGUST 1977-1259
broadening exists in the reciprocal lattice directions
which correspond to the radial directions of the real
space zones~ that is in {100} planes. These diffuse
streaks a r e best observed in Fig. 6(a) which is a dif-
fraction pattern of a sample aged for 1128 h at room
temperature, The diffuseness should be compared
with the sharp streak observed in samples aged at
130~ (403 K). See Fig. 6(b) and discussion below.
Extra reflections appear in the diffraction pattern
shown in Fig. 6(a). The diffuse reflections at the (011)
positions a r e intersections of the [100] streaks with
the reflection sphere. The other two diffuse reflec-
tions are from A1203 oxide, which forms epitaxially
on the surface of the specimens.
With further aging at room temperature the satel-
lites remain, and for times up to four months the
well known transition phases of 0" and 0' do not ap-
pear in bulk samples (i.e. samples of thickness on
the o r d e r of 0.01 in. (250 pro) thick).
The samples were carefully examined for the exist-
ence of <110) r e l - r o d s in r e c i p r o c a l space. They were
not observed, giving support to the conclusion that the
diffuse satellites are indeed present because of diffuse
composition modulations in real space, and not be-
cause of the intersection of the Ewald sphere with
(110) t e l - r o d s , as is the case in the similar C~-Be
system)~
DISCUSSION
These results show that at room temperature the
A1-4 wt pet Cu alloy decomposes into a modulated
m i c r o s t r u c t u r e before the formation of GP zones,
This implies that the alloy may have decomposed by
the spinodal mechanism. This initial decomposition
p r o c e s s may be written as:
where
a ' is the supersaturated solid solution,
nat is the Al-enriched regions of the matrix and
OtCu is the Cu enriched regions of the matrix.
Following this process, the GP zones f o r m .
The details of the composition profiles in the Cu-
enriched regions (viz C~Cu) can not be obtained by
conventional TEM techniques. Thus the regions may
be similar to the "Guinier zones ' ' ~ (not to be con-
fused with GP zones), or they may have a continuous
composition variation throughout (as in spinodal de-
composition). In either case, however, the regions
are periodically arranged in real space as shown by
the manner in which the GP zones form (e.g. Fig.
5). Thus it appears that spinodal decomposition has
occurred.
The appearance of the platelike GP zones after"
the initial decomposition process can be accounted
for by two distinct mechanisms, namely by nucleation
and growth or by the continuous evolution of the
plates from the existing composition modulations.
These two mechanisms will now be qualitatively dis-
cussed.
Clearly the solute enriched regions could act as
sites for easy nucleation of the pure Cu platelet G P
zones. The build-up of solute in the regions mini-
mizes the need for solute diffusion to the sites. This
1260-VOLUME 8A, AUGUST 1977
mechanism is fairly straight-forward, and does allow
for the existence of the "semiperiodic" array of G P
zones that results.
However the diffuseness of the (100) s t r e a k does
suggest that the zones could be forming continuously
from the initial modulated structure. GP zones that
f o r m at 130~ (403 K) give r i s e to v e r y sharp <100>
streaks in r e c i p r o c a l space. This is to be expected
if they form above the spinodal, where they nucleate
directly as plates. However, if the modulated micro-
structure continuously t r a n s f o r m s to the GP zone
m i c r o s t r u c t u r e , we would expect the (100> streaks
to appear gradually, their initial appearance being
rather diffuse. Such is the case. (See Fig. 6(a),
which is the diffraction pattern which corresponds to
a sample aged for 1128 h at room temperature, cf
Fig. 6(b).) We conclude therefore that such a mecha-
nism is the m o r e likely.
This continuous change of the early stage micro-
structure into the later stage GP zone m i c r o s t r u c -
ture, can not however be explained by the linear
theory of spinodal decomposition. This theory pre-
dicts 5 that the final m i c r o s t r u c t u r e wilt consist of
particles of the solute-enriched phase that a r e more
or less cuboidal in nature. The previous studies on
C u - N i - F e 1%17 and Ni-Ti 18-~~follow this v e r y closely.
One exception is found in the Cu-Ti case, where the
particles of Cu.,Ti terminate as " e l o n g a t e d "
cuboids. 21-23 This however is a coarsening effect,
and is related to the fact that the Cu4Ti has tetragonal
symmetry, as opposed to the cubic s y m m e t r y in the
Ni-Ti and Cu-Ni-Fe cases. 24 The particles elongate
along their c-axis in o r d e r to minimize the coherency
strains.
In A1-Cu, however, the exception is more pro-
nounced. The cuboidal regions collapse to platelike
regions during the later stages of the spinodal de-
composition process. In t e r m s of Cahn's later stage
solution to the nonlinearized diffusion equation, 25
the higher o r d e r anharmonic t e r m s have an exag-
gerated effect on the final m i c r o s t r u c t u r e . Specifi-
cally, the second and third harmonics, which come
about by expanding the expression (Eq. [3] of Ref.
15)
iv-- 7 + I-,.{
about the average composition are of great importance
in the A1-Cu system. In the above expression, a2f/~c2
is the second derivative of free energy with respect to
composition, q is the fractional change in lattice
p a r a m e t e r per unit composition change (viz (l/a)
• (da/dc)). E is Young's modulus (assumed iso-
tropic), v is Poisson's ratio, M is the diffusional
mobility and Nv is the number of atoms per unit vol-
ume.
The second harmonic amplifies the composition of
the GP zones at the expense of the matrix, and limits
their spatial extent. ~ The third harmonic sharpens
the interface between the zone and the matrix, e~ ul-
tinmtely yielding the one atomic layer thick GP zone
(often called GP I). The reason for the unusually strong
composition dependence of Expression [2] is not
certain. It probably is related to the fact that A1 and
Cu have a large atomic disparity (about 9 pct). This
makes it energetically unfavorable to build up 3-
METALLURGICALTRANSACTIONSA
d i m e n s i o n a l r e g i o n s o f p u r e Cu i n t h e A1 m a t r i x . H o w -
e v e r , t h e d e t a i l s of t h i s r e l a t i o n s h i p h a v e n o t y e t b e e n
worked out.
T h u s , w h i l e t h e d e c o m p o s i t i o n p r o c e s s s t a r t s out a s
p r e d i c t e d by the l i n e a r t h e o r y of s p i n o d a l d e c o m p o s i -
tion, the h i g h e r o r d e r h a r m o n i c t e r m s s o o n take on a
p r e d o m i n a n t r o l e in t h e d e v e l o p m e n t of t h e m i c r o -
s t r u c t u r e . It m u s t b e e m p h a s i z e d t h a t t h e s e c o n -
c l u s i o n s a r e b a s e d on r o o m t e m p e r a t u r e aging ex-
p e r i m e n t s . A t h i g h e r t e m p e r a t u r e s ( e . g . 130~
(403 K)) t h e z o n e s n u c l e a t e d i r e c t l y f r o m t h e s u p e r -
s a t u r a t e d s o l i d solution without any p r i o r d e c o m p o s i -
t i o n . S a t e l l i t e s a r e n o t o b s e r v e d p r i o r to t h e f o r m a t i o n
of G P z o n e s a t 130~ (403 K).
CONCLUSIONS
F r o m the r e s u l t s and the d i s c u s s i o n we conclude the
following:
1) A 1 - 4 w t p c t Cu i n i t i a l l y d e c o m p o s e s i n t o s o l u t e
enriched and solute lean regions. We interpret this
to show that s p i n o d a l d e c o m p o s i t i o n o c c u r s at r o o m
t e m p e r a t u r e . T h i s i s f i r s t o b s e r v e d a f t e r 5 h.
2) G P z o n e s w e r e f i r s t r e s o l v e d a f t e r a b o u t 1 w e e k
at room temperature.
3) T h e G P z o n e s f o r m c o n t i n u o u s l y f r o m t h e e a r l y
s t a g e m o d u l a t e d m i c r o s t r u c t u r e a s a r e s u l t of t h e
d o m i n a n c e of the s e c o n d and t h i r d h a r m o n i c t e r m s
of the s o l u t i o n to the n o n l i n e a r i z e d d i f f u s i o n equation.
ACKNOWLEDGMENTS
T h e a u t h o r s w o u l d l i k e t o t h a n k N. T . N u h f e r a n d
L. A. Nesbit for technical assistance throughout the
c o u r s e of the i n v e s t i g a t i o n . We a l s o thank P r o f e s s o r s
J . W. Calm and D. de F o n t a i n e f o r helpful d i s c u s s i o n s .
METALLURGICAL TRANSACTIONS A
R . J . R i o j a w a s s u p p o r t e d by a g r a n t f r o m C O N A C Y T
(Mexico), and D. E. L a u g h l i n w a s p a r t i a l l y s u p p o r t e d
by a R e s e a r c h I n i t i a t i o n G r a n t f r o m the N a t i o nal S c i -
e n c e F o u n d a t i o n , D i v i s i o n of M a t e r i a l s R e s e a r c h ,
75-10618.
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