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CELLULAR
PRECIPITATION
COARSENING
AND
IN
PRECIPITATE
A Mg-Al
ALLOY
Abstract-The
of Metallurgical
morphology
Engmeering,
and growth
lndtan
kinetics
Institute
of Technology,
of the cellular
precipitate
OptiCdl
Kanpur-208016,
India
subsequent coarsening stage, has indicated that the transformation is controlled by diffusion of aluminum
through the cell boundaries.
ResumePOn a ttudie, g des temperatures allant de 440 a 580 K. la morphologie
croissance
et de grossissement
discontinu
du precipite
cellulaire.
On a utilise
et les cinetiques de
la microscopic
optique
et la
diffraction de rayons-X pour caracteriser la transformation cellulaire. On a observe quun alliage mttastable
de Mg-7 at.% AI rapidement solidifie. se decompose completement en une structure lamellaire constituee
de phases j et 7, pour toutes les temperatures de vieillissement utilisees darts cette etude, via un processus
appelt precipitation cellulaire. La structure lamellaire fine de cellules primaires sest ensuite decomposee
en une structure lamellaire grossiere comprenant les memes deux phases. Les mesures des parametres de
mailles ont indiquees que la matrice appauvrie de la phase 6 associte avec les cellules initiales Ctait plus
riche en solute que le point dequilibre du solvus 6!(6+y). La concentration en solute de la matrice
appauvrie. associee avec le materiau gross,. etait moindre que celle du point dtquilibre. Lanalyse de
la cinetique des croissances, en premier lieu des reactions cellulaires. puis des etapes consecutives de
grossissement, indique que la transformation est contrBlee par la diffusion daluminium
au travers des
joints de cellules.
1. INTRODUCTION
been carried out to study the kinetics of discontinuous coarsening of the cellular precipitate and compare the results with those
for the primary cellular precipitation in the same alloy.
2. EXPERIMEIVTAL
The Mg-7 at.% Al alloy was obtained in the as cast condition
in the form of rods 1 cm in diameter and approximately 9 cm
long. The rods were lightly cold deformed and annealed at 650
K for one day in a sealed quartz tube under vacuum. A number
of specimens, 2 mm thick, were cut from the rod. These were
ground flat and cleaned.
The disc specimens were encapsulated in a quartz tube under
vacuum, annealed for 1.5 h at 650 K and quenched in a mixture
of ice and water mainmined at 277 K. In order to prevent
possible room temperature transformation,
the quenched specimens were stored in a refrigerator. All aging treatments were
carried out in a salt bath maintained within k 2 K of the desired
temperature. In order to prevent oxidation and direct salt corrosion of the Mg-Al
alloy, each specimen was wrapped in
aluminum
43
foil
before
aging.
A number
of specimens
were
aged
44
Q. M. AMIR
and S. P. GUPTA:
CELLULAR
PRECIPITATION
AND
PRECIPITATE
COARSENING
3. RESULTS
AND DISCUSSION
3.1. Microstructure
Time,
Fig. I. (a) Growth distance vs time of aging, primary cells. (b) Growt
distance vs time of aging, secondary cells.
rate
The growth rate for both primary cells and secondary coarsened patches at each temperature was determined from average
growth distance vs time data. The growth distance was measured as the perpendicular
distance from the original position
of the grain boundary to the leading edge of the cell. About 40
measurements were made on each specimen and the average
growth distance determined. For the measurement of the coarsening rate, only those patches which originated at the grain
boundary position were considered for evaluation. Again,
about 40 measurements were made. The growth distance values
were multiplied by a factor 7114 to be consistent with the bulk
averaging technique of Gust et al. [I 31. Growth distance vs time
plots are shown for both primary and secondary features at a
few temperatures in Fig. 1(a) and (b). respectively. Growth rates
as determined from the best straight lines drawn through the
points are shown in Fig. 2 and Table I as a function of the
absolute temperature. The growth rate of the primary cells
reported by Frebel et al. [2] for a Mg-7 at.% Al alloy is also
shown in Fig. 2 for comparison. The growth rates of the primary
g lo-lo
6
10-l
10-12I
450
500
550
T, K
Fig. 2. Growth rate vs temperature of aging.
Q. M. AMIR
Table
I,, m
T(K)
and S. P. GUPTA
I. Composition,
S-I
440
460
480
500
520
550
570
580
(x
growth
lO-y)
: CELLULAR
PRECIPITATION
P2, m SK (x lo-)
0.84
2
4.8
7.31
10.33
15.16
11.00
9.84
AND
PRECIPITATE
1.092
2.58
6.84
10.91
14.76
18.47
36
40.41
46.95
56.42
71.04
93.87
115.4
163.94
45
COARSENING
and secondary
52.82
62.84
72.69
90.09
141.37
209.65
cells
X;
X;
X;
0.0225
0.028
0.0345
0.039
0.0465
0.051
0.0555
0.058
0.0115
0.0125
0.018
0.255
0.028
0.045
-
0.018
0.0215
0.026
0.03 1
0.0363
0.045
0.0525
0.0555
1 o-5
E
800
700
M
+
600
Equilibrium
solvus
500
400
I
3001 11 12
0
lF7-
550
T,
spacing
10
Al, atom%
Fig. 4. Composition
Fig. 3. Interlamellar
vs temperature.
superimposed
on the
Mg-
46
Q. M. AMIR
and S. P. GUPTA
: CELLULAR
PREClPITATION
AND
PRECIPITATE
COARSENING
AC:-? = (~)A(;:+(~)AG;.
Table
T(K)
440
460
480
500
520
550
570
580
3.914
3.801
3.661
3.545
3.571
3.319
3.231
3.203
-AC;
(J mol-)
-4.23
23.6
60.99
94.98
1 19.56
171.68
205.08
217.41
-AC:
(J mol78.77
92.78
112.11
132.44
147.71
186.53
213.31
223.74
2.
(7)
(8)
In equation (8) Xz is the composition of the fi phase at the
three phase junction &6,-y. and is given by
-A;+,
I)
(J mol-)
I 18.28
123.6
134.1
147.8
156.18
189.6
213.4
222.95
-6G:
(J molt
122.52
100.0
73.11
52.81
37.2 1
17.91
8.31
5.54
+ AGj
(J mol )
22.42
20.0
17.21
14.32
11.38
8.61
7.0
4.93
-AG,
(J molF)
-A0
(J mol)
10.07
80.0
55.89
38.48
25.83
9.3
1.31
0.61
1.29
2.77
3.71
2.96
5.12
1.22
-(A(;>-AG,,)
(J molF)
7.18
7.13
6.1
5.35
5.66
4.75
- AGz
(J molF)
8.47
9.91
9.81
8.32
10.78
5.97
Q. M. AMIR
and S. P. GUPTA
: CELLULAR
PRECIPITATION
AND
PRECIPITATE
41
COARSENING
above simplification
because values of L, L, and K are not
known, substitution of X$ = XR and Xk as the depleted matrix
composition yields a modified value of s( given as follows :
(13)
I
I
-i
0
E
b
10
20
30
40
Mg
0"
lo-l6 F
c
Petermann
and
flornbogen
-300
xKI
L---X",
1
II
04
20
Al,
Fig. 5. (a) Free energy-composition
composition
Turnbull
is
(a)
30
Dilute
solution
40
atom%
(10)
1 .I
"E
1.8
1.9
2.0
2.1
2.2
2.3
1.8
1.9
2.0
2.1
2.2
2.3
(12)
10-23
,
1.7
1000/T,
Fig. 6. (a) and (b) Diffusivity
K-l
cellular
reaction.
48
PRECIPITATION
AND PRECIPITATE
COARSENING
Table 3. Activation energy data for the glowth of primary and secondary ceils
S
Activation
energy Q
(kJ mol-)
Petermann and
Hornbogen
Cahn
Turnbull
125
68.25
100.35
Sundquist
Hillert
Petermann and
Hornbogen
Livingston
and Cahn
73.25
71.32
120
90.00
Mobility
104
cells occurs
(14)
(15)
Q. M. AMIR
and S. P GUPTA:
Petermann
and
CELLULAR
PRECIPITATION
AND
PRECIPITATE
Hornbogen
4.50
1.7
1.8
1.9
2.0
1000/T,
Fig. 7. Diffusivity
vs I/Tfor
49
COARSENING
2.1
550
600
T, K
2.2
2.3
K-
the secondary
I
500
cellular
vs temperature
of aging.
reaction
boundary migration
lowing relationship:
Examination of the free energies for the growth of secondary
cells (Table 2) reveals that chemical free energies remaining
after the primary cell growth are negligibly small. The major
contribution
to the driving force for the growth of secondary
cells stems from differences in interfacial energies associated
with the primary and secondary cells. The Livingston and Cahn
[31] model of discontinuous
coarsenmg of the primary cells
proposes the difference in interfacial energies associated with
the primary and secondary cells as the driving force. The secondary cell growth kinetics are, therefore, analyzed using the
theory of Livingston and Cahn [31]. Accordingly, the diffusivity
is related to the growth rate, vL, and mterlamellar spacings, S,
and S,, by the following relation :
M, by the fol-
The mobility of the cell boundary for the primary cells is shown
in Fig. 9 as a function of the reciprocal of absolute temperature.
The Arrhenius plot of Fig. 9 describes the kinetics of cellular
precipitation
quite well in the whole range of temperature. The
slope of the straight line yields an activation energy of 104 kJ
molV, which is well within the range of activation energies
obtained for the growth of primary and secondary cells from
the diffusivity vs temperature plot.
4. CONCLUSIONS
10-17
1.7
1.8
1.9
2.0
2.1
2.2
2.3
1000/T,
K-
50
Q. M. AMIR
and S. P. GUPTA:
CELLULAR
PRECIPITATION
REFERENCES
M. Frebel, K. Behler and B. Predel. 2. Metallk.
67. 228 (1976).
M. Frebel and K. Behler, Metall. Trans. 8A, 621 (1977).
D. Turnbull,
Acta Metull. 3. 55 (1955).
B. E. Sundquist,
Metall.
Trans. 4, 1919 (1973).
S. P. Gupta and G. T. Parthiban,
Z. Metullk.
76, 505 (1985).
V. Suresh and S. P. Gupta. 2. Metullk.
77, 529 (1986).
V. V. Balasubramanyam
and S. P. Gupta,
Actu. Metull.
37, 291
(1989).
8. S. P. Gupta, Z. Metullk.
77, 472 (1986).
9. S. P. Gupta, Actu Metall. 35. 747 (1987).
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2.
3.
4.
5.
6.
7.
10.
11,
12.
13.
14.
15.
16.
17.
18.
19.
20.
21.
22.
23.
24.
25.
26.
27.
28.
29.
30.
31.
AND
PRECIPITATE
COARSENING