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The effect of the retrogression and reaging treatments (RRA) on the microstructure of AI-7075 in the
T651 temper, both in the matrix and on grain boundaries, was studied using transmission electron
microscopy. The processes occurring in the matrix during the retrogression treatment are principally
the dissolution of small particles of the ~?' transition phase, transformation to 77of the larger particles
of r/', coarsening of the three commonly observed variants of the 77phase precipitates 031, ~72,and rh),
and precipitation of new rt phase particles, particularly the rh variant. The main process occurring
during the reaging treatment is either growth of partially dissolved r/' particles or precipitation of the
rt' phase. These lead to a microstructure containing many fine "q' precipitates and some larger ~71and
~?zpanicles with a smaller amount of coarse 94 particles, resulting in a broad particle size distribution.
The high strength of the 7075 alloy in the RRA temper is believed to arise from the relatively high
overall concentration of particles in this dispersion. The retrogression treatment produces rapid initial
coarsening of the grain boundary particles, which are primarily 77 phase precipitates, resulting in an
increase in their volume per unit grain boundary area, Va. The beneficial effect of the RRA treatment
on the susceptibility of 7075-T651 to SCC is believed to be due, at least partially, to the increased value
of VA produced by the RRA treatment.
(a)
~ _ 0.1 iJ m....A
(a)
(b)
Fig. 2--Bright-field micrographs of AI-7075 in the (a) RRA 30 and
(b) R 30 conditions. A line-of-no-contrast perpendicular to the diffraction
vector ~ = [1]1] is visible at the particles indicated by arrows in (a).
Table I. Characteristics of the Precipitate Dispersions in the Matrix of 7075-T651 Resulting from the Various
Retrogression and Reaging Treatments. The Dimensions (d = diameter, t = thickness, 1 = length) Are in nm.
The Particle Concentrations, Nv, Are Represented Qualitatively by vl = very large, I = large, m = moderate, s = small.
,o
Z
w
30
o
w
LI.
(c) RRA 10 (d) RRA 60
20
10
I~r,? ~ I
5 10 15 20 25 30 0 5 10 15 20 25 30 35
the r/l variant, compared to that in the RRA 30 structure are (7a) is a dark-field image taken using the (00.10) 7,
(Table I). The second is that considerable coarsening of all and (24.0)~4 reflections, and Figure 7(b) is a dark-field
the rt variants occurs as the immersion time increases from dislocation image taken using g = (1]-1) with g = (333)
30 to 60 seconds, shifting the peak in the histograms from strong (fine particles are also seen in the background of
5 to 10 nm to 10 to 15 nm (Figure 6). The sizes of the r/ Figure 7(b), due to the fact that the (00.6),, reflection super-
variants are very comparable to those in the T7 structure. 27 poses on the (1]l)a~ spot). The examination of various
However, the RRA 60 structure still shows the presence of images of these kinds suggests that the extent of hetero-
some fine r/' particles. geneous nucleation of r/' particles is generally small com-
It is interesting to note that no appreciable increase in the pared with that in the T651 structure. 27
overall average particle size, d, is found during the initial
period (up to 20 to 30 seconds) of the retrogression treat- B. Microstructure of Precipitates on Grain Boundaries
ment, although significant coarsening of the r/ particles, The microstructures of regions near grain boundaries, in
particularly the rt~ and '1'74types, occurs during that time. particular the width of the PFZs and the size distributions
General coarsening occurs rapidly afterwards. The rela- and dispersions of grain boundary particles, were studied in
tively constant value of d is due to the partial dissolution an attempt to correlate them with the SCC properties of A1
of/he r/precipitates, which compensates for the growth of 7075 in the T651, T7, and various RRA conditions. Ex-
the r/particles. truded 7075-T651 typically contains grains highly elongated
On the examination of various thin foils in both bright- in the extrusion direction. The L-ST orientation, which is
and dark-field, it appeared that some fine r/' particles nucle- the most susceptible to SCC, contains PFZs along the length
ate along dislocation lines. These particles were usually of these elongated grains. On the other hand, the L-T orien-
visible in dark-field images taken using the r/' reflection. tation, which is the least susceptible to SCC, contains PFZs
Dark-field dislocation images were examined to confirm distributed randomly among the boundaries of the equiaxed
this observation. Careful comparison of various dark-field grains. The results of PFZ width measurements made from
images of the r/' particles with dark-field dislocation images samples in the T651, RRA 30, and T7 conditions (Table II)
indicated that some of the r/' particles in fact nucleate along indicate that no significant difference can be found, consid-
dislocation lines. An example is seen in Figure 7; Fig- ering the scatter in the data, although the PFZ width in the
(c) (d)
Fig. 8--Bright-field micrographs of precipitates on the grain boundaries in samples of AI-7075 in various temper conditions: (a) T651; (b) T7;
(c) RRA 30; (d) RRA 10.
was taken as dg. More than 100 particles in five different paring them with the particles in the matrix adjacent to the
grain boundary areas were generally measured in each case. grain boundary.
NA was measured directly from micrographs in which the A a w a s measured from the micrographs using lines drawn
projected areas were about 0.15/zm 2. This projected area parallel to the intersection of the grain boundary and the foil
was also used for the measurements of AA. It was hard to surfaces. The spacing of the parallel lines was 0.01 /xm and
measure the exact angles of tilt between the grain boundaries their length was typically 0.9/xm. Ten lines were typically
and the plane of projection. However, it was estimated that used in each analysis and more than five grain boundary
the maximum error arising from the differences between areas were examined in each case. The potential major
tilting angles from one sample to another is less than sources of error in the measurement of AA are twofold. The
13 pct. Errors can also arise from the projected images of first is associated with the problem of overlapping particles
matrix particles onto the grain boundary, although the grain in the projected area. This problem was avoided by choosing
boundary precipitates are in general easily distinguishable proper grain boundary areas. The second is the orientation
from matrix particles because of their considerably larger dependence of the projected particle shape due to the pos-
sizes (Figure 8). Nevertheless, the sizes of some of the sibility of different aspect ratios of the particles in the
smaller grain boundary particles are sometimes comparable different conditions. It was assumed that the aspect ratios of
to those of the larger particles in the matrix, particularly the particles in all conditions are the same.
in samples in the T651 temper. Special precautions were From Table II it is seen that the mean particle size, dg, in
taken in such cases to differentiate those matrix particles the T7 structure is significantly larger than that in the T651
possibly projected onto the grain boundary area, by com- structure, and that dg in the RRA 30 structure is comparable
10
0 i Ihi I I
20
(c) RRA 30 (d) R 30
o
>-
Z
ug 10
D
uJ
t~
0
, , i i lJ Illll Hl"il
20
10
r~RRA 10
(f) RRA 60
1 I I ~ / _ l I J
20 40 60 80 100 120 0 20 40 60 80 100 120 140
Fig. 9 - - S i z e distributions of the particles on the grain boundaries in AI-7075 in the T651, T7, RRA 30, R 30,
RRA 10, and RRA 60 temper conditions. The size of the particles refers to their diameters. Note the bimodal
size distribution in the RRA 30 structure.
to that in the T7 structure. As seen in Figure 9, however, the 60 25 ~.~ ~" 500 100
size distribution of the grain boundary particles in the RRA -\
30 structure appears to be broader than those in the T651 and
T7 structures. In the T651 structure, the sizes of most of the 50 20-k.,.,,~.,~_i 400 80
particles are in the range 20 to 40 nm, while they are in the
range 40 to 60 nm in the T7 structure. In the RRA 30
structure, however, some grain boundaries exhibit particles "~ 40 _ v 15 300 ~ 60 -
of small size (ranging from 20 to 40 nm), which are compa-
rable in size to those in the T651 case, while other grain !,," I
boundaries show large particles, comparable in size to those 30 ~o 6/ I o~-,,( .... ) 200 40
in the T7 case, resulting in a bimodal size distribution. The r- IzxN,,.*.- --)_ ,
[o v,,,/vA(-. l ( " - = ' - )
reason for that is not known at the present time, but further
investigation is in progress. It can be seen in the particle size 20 - 5 , , I , , ,~ 100 ~ 20
distribution characteristic of the RRA 10 structure that the 30 60 T7
proportion of large particles increases, indicating that IMMERSION TIME (s)
particle coarsening has already occurred. Fig. 1 0 - - Variation of the parameters characterizing the dispersion of grain
Figure 10, summarizing the effect of the RRA treatment boundary precipitates in AI-7075-T651 as a function of immersion time
on the dispersion of grain boundary particles, shows the at the retrogression temperature, 240 ~ AA is the areal fraction covered
variation of de, AA, and NA as a function of immersion time, by particles on the grain boundaries, d~ is the mean particle size, Na is
the number of particles//zm ~, and VA is the volume of particles//zm 2.
together with the corresponding values in the T7 structure.
The values of Va are normalized to that in the T7 structure. Note the
AA and d Rincrease rapidly, while Na decreases rapidly in the rapid increase in de, Aa, and VA during the initial period of the retrogres-
initial period of the retrogression treatment and very slowly sion treatment.
a f t e r w a r d s . AA reaches --80 pct of its value in the T7 struc-
ture within 30 seconds of the retrogression treatment, and is
already significantly larger than that in the T651 structure The volume of grain boundary precipitates per unit grain
( - 5 7 pct of its value in the T7 structure) after a retro- boundary area, VA, can be calculated using the measured
gression treatment of only 10 seconds (--75 pct of its value parameters AA and NA, assuming that the plate-shaped par-
in the T7 structure). ticles are randomly oriented on the grain boundary area and
METALLURGICAL TRANSACTIONS A VOLUME 15A, AUGUST 1984--1539
that the aspect ratio of the particles, k = t/r, (where t is the solvus temperature can survive during up-quenching to
plate thickness and r the plate radius) is small. The mean above its solvus temperature and transform to a more stable
projected area, which is given by 7rr2/2, can be calculated phase if their sizes exceed a critical size, de, at the higher
by the integral of the projected area at a given orientation temperature. Meanwhile, smaller particles, the sizes of
times its probability over all possible orientations. As- which are less than d,., dissolve during the up-quench.
suming that k is constant (-0.18), VA is given by VA = Thirdly, coarsening of the r/particles occurs. On com-
1.6k AA3/Z/NA1/2. Values of ga/k for the various heat treat- paring the RRA 30 and T651 structures, 27 it is seen that the
ment conditions are also summarized in Table II. Figure 10 RRA treatment causes a significant increase in the sizes of
shows the variation of VA as a function of retrogression time, the r/ particles, particularly the r/l and TI4 variants. This
normalized to its value in the T7 structure. It is seen that VA occurs mostly during the retrogression treatment, since the
in the T651 structure is small compared with that in the T7 sizes and distributions of the r/ particles in the RRA 30
structure ( - 3 5 pct). VA increases rapidly during the initial structure are similar to those in the R 30 structure. The
period of the retrogression treatment (as does AA), reaching results on the RRA 10 structure indicate that some coarsen-
--65 pct of its value in the T7 structure within 10 seconds ing of the r/particles has already occurred after only a few
immersion time and - 7 0 pct of its value in the T7 structure seconds of the retrogression treatment. As the retrogression
within 30 seconds immersion time. time increases from 30 to 60 seconds, significant coarsening
of all the r/variants occurs.
Finally, examination of the RRA 60 structure shows that
IV. DISCUSSION as the retrogression time increases from 30 to 60 seconds,
the number of r/ particles, particularly the T]I variant, in-
A. Effect of the RRA Treatment on the Microstructure of creases. An appreciable increase in the number of the "1"/4
Matrix Precipitates particles occurs as well. This suggests that the precipitation
The processes occurring during the retrogression treat- of r/particles, particularly the rh variant, occurs during the
ment in the matrix can be summarized as follows. Firstly, retrogression treatment. It is concluded that the r/' particles
comparison of the RRA 30 and R 30 structures leads to the in the T651 structure, the sizes of which are smaller than dc
conclusion that a significant fraction, -V3 of the total par- corresponding to the retrogression temperature of 240 ~
ticles, either partially or completely dissolves and that the become unstable on up-quenching to the retrogression tem-
dissolving particles are mainly r/' precipitates, since the perature and gradually dissolve during the initial period of
concentration of each r/variant is found to be comparable in the retrogression treatment. All the unstable particles will
both structures. The presence of a significant amount of very tend to dissolve. If the proportion of unstable particles is
fine 7' particles in the R 30 structure suggests that many of very large and the overall concentration of the solid solution
the dissolving particles remain incompletely dissolved near resulting from the dissolution of these particles exceeds the
the minimum hardness condition of retrogression. It is evi- solubility limit of the stable phase at the retrogression tem-
dent that the drop in hardness observed during the early perature, the solid solution can become supersaturated with
stages of retrogression is due to precipitate dissolution, as respect to the stable phase. When the degree of super-
surmised by Danh et al.25 The dissolving precipitates are not saturation becomes sufficient to drive the nucleation of the
GP zones, however. They are instead r/' particles. Coarsen- equilibrium phase at a reasonable rate, the precipitation of
ing of the r t phase precipitates at this early stage was appar- that phase will occur. We believe that this happens in the
ently not observed by them. present case, since examination of the R 30 structure shows
Secondly, the phase transformation r/' ~ rt appears to that a significant portion of the r/' particles dissolves during
start in the early stage of the retrogression treatment. The the retrogression treatment.
results show that the concentration of ~ particles, particu- Mondolfo et al.,32 in their X-ray study of a pure AI-6Zn-
larly the 172 variant in the RRA 30 structure, significantly 2Mg alloy, found that the r/and T phases form together at
increases while the concentration of the 77' particles de- temperatures between 200 and 300 ~ Within the aging
creases, compared to those in the T651 structure. The con- times (up to 60 seconds) at 240 ~ investigated in this study,
centration of the 774 particles also increases appreciably. no appreciable formation of the T phase was observed,
Even the number of the r/2 particles in the RRA 10 structure although small amounts were occasionally detected. The
increases significantly. These observations can be inter- reason for this is not well understood, but the observation
preted as an indication that some of the more stable large r/' suggests that the nucleation of the T phase is more difficult
particles transform to r/particles, particularly the r/: variant than that of the rt phase when the alloy is subjected to the
which has the same orientation relationship with the matrix multistage heat treatment used in the present study.
as r/', i.e., (10.0)II (110)al; (00.1)II (1]l)a~. This agrees with The process occurring during the reaging treatment ap-
the observation of Gjonnes and Simensen z9 and DeArdo and pears to be either the growth of the partly dissolved r/'
Simensen, 3~who studied two-step aging of pure A1-Zn-Mg particles or the reprecipitation of the 77' particles. Since the
alloys, that some of the r/' particles formed at a lower aging results show that a significant fraction of the dissolving r/'
temperature transform to '/72 particles during up-quenching particles still exhibits faint contrast after the retrogression
to a higher aging temperature. It is also possible that some treatment, it appears that the growth process contributes, to
of the r/particles transform to the "04 variant, since 774 has a significant extent, to the presence of many r/' particles in
the same habit plane, {111}, as r/'. the RRA structure. Some of these are nucleated hetero-
These results may be explained by the theory of two-step geneously, although this is a minor effect. Nevertheless, this
aging of Lorimer and Nicholson. 3~ They proposed that par- result is of interest because the original intent of the RRA
ticles of an intermediate phase formed during aging under its treatment of Cina and Ranish 2~ was to dissipate localized