Recovery, Recrystallization and Phase Transformations During Thermomechanical Processing and Treatment of Tial-Based Alloys
Recovery, Recrystallization and Phase Transformations During Thermomechanical Processing and Treatment of Tial-Based Alloys
Recovery, Recrystallization and Phase Transformations During Thermomechanical Processing and Treatment of Tial-Based Alloys
48 (2000) 2803±2813
www.elsevier.com/locate/actamat
AbstractÐThe conversion of the cast microstructure of a Ti±45Al±10Nb (at.%) ingot due to extrusion and
subsequent heat treatments was investigated using scanning and transmission electron microscopy. The
starting lamellar microstructure was broken down by dynamic recrystallization into a ®ne-grained duplex
microstructure after extrusion, however, a small amount of remnant lamellae was retained. It was found
that the ®ne substructures in the remnant lamellae varied from one area to another. Recrystallization and
phase boundary bulging were found to be the major mechanisms responsible for lamellar globularization.
The existence of remnant lamellae was ascribed to the anisotropic ¯ow behavior of the starting lamellar
colonies. Microstructural and process variables that in¯uence the scale of remnant lamellae will be eluci-
dated. Annealing in the
a g two-phase ®eld cannot eliminate the remnant lamellar structures. However,
the detrimental eect of remnant lamellae can be minimized after alpha treatments provided that the rem-
nant lamellae are smaller than about 80 mm. 7 2000 Acta Metallurgica Inc. Published by Elsevier Science
Ltd. All rights reserved.
1359-6454/00/$20.00 7 2000 Acta Metallurgica Inc. Published by Elsevier Science Ltd. All rights reserved.
PII: S 1 3 5 9 - 6 4 5 4 ( 0 0 ) 0 0 0 9 3 - 8
2804 ZHANG et al.: RECOVERY, RECRYSTALLIZATION AND PHASE TRANSFORMATIONS
3. RESULTS
lamellae were completely broken down into globu- lamellar structure is nearly completely preserved
larized duplex microstructure (areas A and D). The (just bent slightly), especially the regions consisting
details of these broken-down (BD) microstructure of coarse alpha and thin gamma laths [marked as
are more readily seen in higher magni®cation micro- arrows a and b in Fig. 2(b)]. In area C of Fig. 1(b),
graphs, Fig. 2(a). However, in some regions rem- many recrystallized gamma grains have formed and
nant lamellar (RL) structures can still be seen, areas this has resulted in the lamellae being broken into
B and C in Fig. 1(b) for example. In area B, the fragments, see Fig. 2(c). Note that the remnant
lamellae are mostly closely oriented to the extrusion
direction [Fig. 1(b)] and the length of the remnant
lamellae varies from about 30 to 150 mm.
Figure 3 shows a view of the BD structure using
bright-®eld TEM. The BD areas are characterized
by a microstructure consisting of worked grains
(and subgrains) containing a high density of dislo-
cations and networks plus ®ne equiaxed grains
essentially free of dislocations. The small dislo-
cation-free grains could be the result of static
recrystallization during air cooling after extrusion.
The numerous grains which contain dislocations
must have recrystallized and subsequently under-
gone further working during extrusion; that is they
recrystallized dynamically. This hypothesis was sup-
ported by the ®ne equiaxed gamma grains (that are
recrystallized) observed in the BSE micrograph,
Fig. 2(a). The grain size distribution and volume
fraction of the statically recrystallized grains and
worked grains are presented in Fig. 4(a). The data
given were determined from at least 200 grains. As
can be seen, the mean grain size of the statically
recrystallized gamma grains is small (0.6 mm), but
their volume fraction is as high as 36%. This means
that static recrystallization occurred very fast during
air cooling after extrusion via the nucleation of
many new grains. The ®ne grain size of the worked
grains (0.9 mm) suggested that the BD areas were
deformed severely during hot extrusion.
The typical deformation substructures observed
in the RL areas are shown in Fig. 5. The lamellar
morphology was eventually preserved. As known, adjacent subgrains aA and aB but only of 6 deg
the g and a(a2) phases in perfect lamellar structure between the top subgrain aA and the end subgrain
have the orientation relationships [16, 17] aE. Accordingly, a new recrystallized gamma grain
has formed between aA and aB (marked with arrow
111g ==
0001a and g ==h1120i
h110 a
1 1).
In the adjacent gamma laths (gA and gB), a high
where the {111}g plane is parallel to the lamellar density of dislocations and deformation twins was
boundaries. However, the Kikuchi patterns from observed, respectively. In heavily twinned laths
the adjacent laths (subgrains) gA, aA and gB indi- (that is gA), recrystallization was rarely observed. In
cated a large misorientation of about 9 deg from the dislocation-dominated laths gB, a few new
the perfect relationships given in equation (1). This recrystallized grains were seen. Note that the new
result suggests that the lamellae have been heavily grains gC tend to keep the orientation relationships
deformed during extrusion. In fact, the a laths were given in equation (1).
converted by extensive deformation into ®ne sub- Figure 6 shows a high magni®cation view of the
grains (or grains) which exhibit dierent contrasts ®ne substructure of a gamma lath containing a high
in Fig. 5 because of their misorientations. The de- density of dislocations. The gamma laths were sub-
formation was inhomogeneous as indicated by the divided into domains (gE and gF) by thin transverse
dierence of misorientations between subgrains. alpha laths aL. These alpha laths are likely to be
There is a misorientation of 16 deg between the induced by adiabatic heating due to the defor-
mation during extrusion. In the gamma domains,
recovery has taken place, leading to the formation
of dislocation networks and low angle boundaries.
It is worth noting that the regions 1 ' and 2 ' (in
domains gE and gF, respectively) are almost free of
dislocations. They are neither recrystallized new
grains nor recovered subgrains because no bound-
aries between the dislocation-free region 1 ' and the
main domain 1 were present. The curvature of the
grain boundaries between these regions and the
adjacent a laths suggested that these clean areas
formed by growth of the gamma domains into a
laths after extrusion (during air cooling), that is by
a mechanism of phase (grain) boundary bulging [8].
The progress of phase boundary bulging can lead
to the breakdown of a laths. This eect is evident
in Fig. 5 at the sites marked with arrows 2 and 3.
Consistent with the BSE observations, the extent
of deformation subjected by the RL areas was
dierent at dierent sites. Figure 7 presents an
example of the RL areas which were only slightly
deformed. There were no subgrains in the a laths
and no evidence of phase boundary bulging. The
lamellar interfaces remained ¯at. Dislocation net-
works and low angle boundaries were observed in
the relatively coarse g lath E
00:8 mm but not in
the thinner laths F±H (0.1±0.3 mm), see Fig. 7. It
should be noted that the mean lamellar interspacing
in this area of about 0.2 mm is much smaller than
that shown in Fig. 5 (0.9 mm).
36% in the as-extruded state to 62% after anneal- of worked (recovered) grains to large grain sizes
ing, Fig. 4. The spread of the size distribution curve after annealing suggests that the ®ner worked grains
of the recrystallized grains to large values after were more easily consumed by the recrystallized
annealing [Fig. 4(b)] indicates that recrystallization grains because of their higher stored energies.
proceeds mainly by the growth of existing grains In comparison, static recovery dominated in the
and to a lesser extent by the nucleation of new RL areas during annealing. The rearrangement of
grains. The shift of the grain size distribution curve dislocations leads to the formation of polygonized
Fig. 5. TEM micrograph showing the ®ne structures in a heavily deformed remnant lamellar area; the
inset Kikuchi patterns indicate the misorientation between dierent grains or subgrains. Note that the
prior continuous alpha laths were broken up at the sites marked with arrows 1±3. See text for more
details.
2808 ZHANG et al.: RECOVERY, RECRYSTALLIZATION AND PHASE TRANSFORMATIONS
Fig. 6. TEM micrograph showing the substructures of a gamma lath in remnant lamellar areas. See
text for details.
subgrains, Fig. 8(c). New recrystallized grains can 3.4. Microstructures after heat treatment at 13208C
be occasionally observed like the grain of 9 deg mis-
orientation shown in Fig. 8(c). As a result, the evi- During heat treatment at 13208C (the alpha
dence of the RL regions can still be seen as coarse transus temperature), the g 4 a transformation
elongated g grains plus segments of a laths even takes place in a dierent manner in the BD and RL
after 2 h annealing at 11508C, Fig. 8(d); in contrast regions. In the BD areas, new alpha grains were
the BD areas exhibit a uniform, ®ne-grained dual formed along the grain boundaries and/or on dislo-
structure. cations within the gamma grain interior after 40 s
Fig. 7. TEM micrograph of the microstructure of a slightly deformed remnant lamellar area in the as-
extruded material. Note that dislocation networks and low angle boundaries developed in the coarse
lath E, but are almost absent in the thinner laths F±H.
ZHANG et al.: RECOVERY, RECRYSTALLIZATION AND PHASE TRANSFORMATIONS 2809
at 13208C, Fig. 9(a). It is important to note that the RL areas must therefore have their lamellar orien-
new alpha grains are randomly oriented as con- tations close to such directions, because the g/a
®rmed by the Kikuchi patterns. In contrast, in the laths keep the orientation relationship given in
RL regions the transformation proceeds simply by equation (1) during the phase transformation.
the thickening of remnant alpha laths, Fig. 9(b). Figure 9(c) shows a nearly fully lamellar micro-
Because the segments of the alpha laths within one structure developed after heat treatment at 13208C
RL area have nearly the same orientation, a certain for 5 min followed by furnace cooling. The distri-
RL area is expected to be completely transformed bution of the grain sizes with respect to their lamel-
into a single alpha grain. Therefore, the grain size lae orientations of about 200 lamellar colonies is
of the newly formed alpha grain (or the lamellar presented in Fig. 10. The lamellar colonies are ran-
colony after cooling) will be limited by the size of domly oriented except for a weak tendency of tex-
the RL area. The existence of coarse RL areas will ture around y 108 and 508 (y is the angle between
thus result in the formation of unusually large lamellar boundaries and the extrusion direction).
lamellar colonies. Recall that the RL areas are gen- Moreover, the distribution of grain sizes is uniform
erally oriented nearly parallel to the extrusion direc- with respect to the lamellae orientations. There was
tion. The lamellar colonies descended from prior no preferred alignment of coarse lamellar colonies
Fig. 8. TEM micrographs showing (a) new recrystallized gamma grains and (b) recovered grains
observed in the BD areas and (c) polygonized subgrains formed in the remnant gamma laths after heat
treatment at 11008C for 10 min followed by air cooling. The angles marked in (c) are the misorienta-
tions between the subgrains with respect to subgrain A. (d) BSE micrograph showing ®ne equiaxed
grains developed in prior BD areas and coarse lamellae formed in prior RL areas after heat treatment
at 11008C for 2 h followed by air cooling.
2810 ZHANG et al.: RECOVERY, RECRYSTALLIZATION AND PHASE TRANSFORMATIONS
4. DISCUSSION
the hot work accumulated in the hard areas was comprised preheating high in the a g ®eld, cooling
not large enough to induce any recrystallization as rapidly as possible to an isothermal forging tem-
(Fig. 7), or the recrystallization occurred in a low perature substantially lower within this two-phase
nucleation density which is not suciently eective ®eld, followed by instantaneous forging. The ``alpha
for a breakdown of the lamellar structures (Fig. 5). forged'' pancake contained much less remnant
These areas were ®nally retained as the remnant lamellar structure than that produced by standard
lamellar (RL) regions. This interpretation is consist- isothermal forging practice. Furthermore, the extent
ent with the fact that remnant lamellae mostly have and volume fraction of remnant lamellae in the
their lamellar boundaries parallel to the extrusion pancake conventionally forged at 12508C were
direction [Fig. 1(b)], that is in a hard orientation. found to be smaller than those (conventionally)
This observation agrees with previous studies on forged at 11508C [5]. Oehring et al. [19] also
forged TiAl alloys, which demonstrated that the demonstrated that extrusion at 13008C (in the a g
lamellar boundaries of remnant lamellae are perpen- two-phase ®eld) leads to more homogeneous micro-
dicular to the forging direction [3, 4]. structures as compared with extrusion at 12508C.
In addition to the working temperature, the
strain rate is another critical factor. At higher stain
4.2. How to reduce the remnant lamellar structure? rates, more work is expected to be put into the
hard lamellar colonies due to work hardening of
As shown in Fig. 5, the two mechanisms respon- the soft colonies (and the later BD areas) and thus
sible for lamellar globularization are recrystalliza- bene®t in breaking up the lamellar microstructure
tion and phase boundary bulging (the former being on a broader scale. The reduced amount of remnant
more eective). To achieve more eective recrystal- lamellar microstructure observed in the convention-
lization, it is necessary to impart more hot work ally forged pancakes was attributed by Semiatin et
into the hard lamellar areas as discussed above. al. [5] to the higher strain rates imposed as com-
From a microstructural point of view, a ®ne colony pared with those used for isothermal forging.
size guarantees more uniform deformation. Thus,
the lamellar breakdown must be easier to achieve in
®ne-grained lamellar microstructures as con®rmed 4.3. In¯uence of the remnant lamellae on the ®nal
by previous works [1, 19]. The second factor to be microstructures
considered is the lamellar interspacing. Reducing
the interlamellar spacing will provide more inter- After heat treatment in the alpha plus gamma
facial barriers to deformation in hard oriented two-phase ®eld, the BD areas exhibit a ®ne recrys-
lamellar colonies and thus increases their hardness. tallized duplex structure but the RL areas remained
In this context, ®ne interspacing is likely to be detri- as lamellae consisting of coarse elongated gamma
mental to lamellar structure breakdown. As shown laths plus short alpha segments, Fig. 8(d). The rem-
in Fig. 7, the dislocation density in ®ner gamma nant lamellar structures cannot be eliminated even
laths is much lower than that in coarse laths. after high-temperature heat treatment at 12608C for
Furthermore, the extent of deformation and recrys- 2 h [5]. We believe this is because recovery rather
tallization in the RL areas with relatively coarse than recrystallization dominated in the RL areas
lamellar interspacing (Fig. 5) is higher than that during annealing, Fig. 8(c). Even if recrystallization
with ®ner interlamellar spacing (Fig. 7). The eect occurred in some RL areas, Fig. 5, the nucleation
of lamellar interspacing on globularization has to density of new grains is relatively low and these
be con®rmed by further studies. new grains tend to keep the orientation relation-
Concerning process variables, the preheating tem- ships given in equation (1). Thus, the characteristics
perature seems to be quite important. At higher of the lamellar structure were preserved. Such unu-
temperature (in the alpha plus gamma ®eld), the sual recrystallization behavior was also found in
improved workability of the materials allows the cold-rolled PST crystals of TiAl [7]. During anneal-
imparting of more plastic strain and thus leads to a ing at 9008C, recrystallization occurred in a manner
more homogeneous deformation of the lamellar without disturbing the lamellar orientation relation-
microstructure. Also, the alpha laths formed at ship in the specimens cold rolled to less than 20%.
these high working temperatures are thermodynami- But randomly oriented new grains were formed as
cally more unstable when cooled to low temperature the deformation became greater than 40%.
after processing (because of their higher supersatu- The existence of remnant lamellar microstructure
rated Al concentrations). This results in a larger after annealing is apparently detrimental to the
driving force (chemical energy in addition to strain mechanical properties of the alloys. A strong orien-
energy) for the globularization of alpha laths via tation dependence of fracture toughness with
recrystallization and/or via phase boundary bulging respect to the extrusion direction was observed in
(of gamma grains). The bene®cial eect of higher the studied Ti±45Al±10Nb alloys after annealing at
working temperature was demonstrated by the so- 10308C for 2 h; the fracture toughness KQ measured
called ``alpha forging'' approach [1]. This approach perpendicular to the extrusion direction is higher
2812 ZHANG et al.: RECOVERY, RECRYSTALLIZATION AND PHASE TRANSFORMATIONS
(25.2 MPa/m1/2) than that (17.6 MPa/m1/2) parallel 3. Recrystallized grains were occasionally observed
to the extrusion direction [20]. Such anisotropic in some remnant lamellar areas and these new
behavior cannot be simply explained by the weak grains grew in a manner of preserving the lamel-
textures observed [20], but may more likely be re- lar characteristics. Recrystallization and phase
lated (at least partially) to the remnant lamellar boundary bulging were found to be the major
microstructure. A low fracture toughness was mechanisms responsible for lamellar globulariza-
observed as microcracks propagate along the (rem- tion.
nant) lamellar interfaces [21], which are preferen- 4. The existence of remnant lamellae in wrought
tially aligned parallel to the extrusion direction. TiAl was ascribed to the strong anisotropic de-
After heat treatment in the single alpha phase formation behavior of lamellar colonies. The
®eld, the in¯uence of the RL structure seems not so amount of remnant lamellar structure is expected
pronounced, as demonstrated in Fig. 9(c). As men- to be reduced by decreasing the initial lamellar
tioned earlier, the existence of coarse RL areas can colony size, increasing the interlamellar spacing,
result in the formation of unusually large alpha preheating the work pieces to higher temperature
grains. However, the existence of small RL areas and processing at a relatively high strain rate.
may not in¯uence the ®nal lamellar microstructure 5. The remnant lamellae were dicult to remove by
achieved after alpha treatment. The data in Fig. 10 annealing in the alpha plus gamma two-phase
indicate that the growth of new alpha grains in the ®eld because recovery dominated in these rem-
wrought materials is very fast during the ®rst few nant lamellar areas during annealing. However,
minutes of alpha treatments. After 5 min at 13208C, the detrimental eect of remnant lamellae can be
most of the alpha grains have a grain size larger minimized by alpha treatments provided that the
than 80 mm. Consistent with this fact, the ®nest remnant lamellar areas are smaller than a size of
fully lamellar microstructure obtained in wrought about 80 mm.
TiAl alloys up to date has a mean colony size of
about 120 mm [2]. Thus, the presence of RL areas in
wrought TiAl may not coarsen the ®nal lamellar
AcknowledgementsÐThe authors acknowledge helpful dis-
microstructures provided that the remnant lamellae cussions and assistance from Drs J. Paul, U. Brossmann
are kept smaller than a critical size of about 80 mm. and M. Oehring. One of the authors (W.J.Z.) would like
The growth of the RL areas is considered to be to thank the Alexander von Humboldt Foundation for
marginal during the ®rst few minutes of alpha treat- ®nancial support. He is also in debt to the support from
ments because the conversion of remnant g a Professor R. Wagner (JuÈlich Research Center, Germany)
and Professor G. L. Chen (University of Science and
lamellae into alpha grains (which is a slow ledge- Technology Beijing, P.R. China).
controlled process) will not be completed within
such a short time [22].
Finally, the present investigation demonstrated REFERENCES
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