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Materials Science and Engineering A283 (2000) 274 288 www.elsevier.

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An experimental study of the recrystallization mechanism during hot deformation of aluminium


S. Gourdet, F. Montheillet *
Ecole Nationale Supe rieure des Mines de Saint -Etienne, Centre Science des Mate riaux et des Structures, URA CNRS 1884, 158 Cours Fauriel, 42023 Saint -Etienne Cedex 2, France Received 10 February 1999; received in revised form 22 October 1999

Abstract Discontinuous dynamic recrystallization (involving nucleation and grain growth) is rarely observed in metals with high stacking fault energies, such as aluminium. In this metal, two other types of recrystallization have been observed: continuous dynamic recrystallization (CDRX, i.e. the transformation of subgrains into grains); and geometric dynamic recrystallization (due to the evolution of the initial grains). The main purpose of this work was to bring clearly into evidence and to better characterize CDRX. Uniaxial compression tests were carried out at 0.7 Tm and 10 2 s 1 on three types of polycrystalline aluminium: a pure aluminium (1199), a commercial purity aluminium (1200) and an Al-2.5wt.%Mg alloy (5052), and also on single crystals of pure aluminium. In addition, 1200 aluminium specimens were strained in torsion. The deformed microstructures were investigated at various strains using X-ray diffraction, optical microscopy, scanning electron microscopy and electron back-scattered diffraction. Observations of the single crystalline samples conrm that subgrain boundaries can effectively transform into grain boundaries, especially when the initial orientation is unstable. In the case of polycrystalline specimens, after separating the effects of the initial and new grain boundaries, it turns out that CDRX operates faster in the 1200 aluminium compared to the two other grades. Moreover, it appears that the strain path does not alter noticeably the CDRX kinetics. 2000 Elsevier Science S.A. All rights reserved.
Keywords: Hot deformation; Aluminium; Dynamic recrystallization; Single crystals; Subgrain boundaries; Grain boundaries; Misorientations

1. Introduction Aluminium and its alloys exhibit very high rates of dynamic recovery, which is generally expected to completely inhibit dynamic recrystallization. However, the formation of new grains during hot deformation of aluminium has been frequently reported. Three types of dynamic recrystallization are likely to produce such a microstructure: (i) discontinuous dynamic recrystallization (DDRX), i.e. the classical recrystallization, which operates by nucleation and grain growth; (ii) continuous dynamic recrystallization (CDRX), which involves the transformation of low angle boundaries into high angle boundaries; and (iii) geometric dynamic recrystallization (GDRX), generated by the fragmentation of the initial grains.
* Corresponding author. Tel.: + 33-4-77420026; fax: + 33-477420157. E -mail address: montheil@sms.emse.fr (F. Montheillet)

Discontinuous dynamic recrystallization, which is commonly observed in low stacking fault energy metals, remains exceptional in aluminium and aluminium alloys. Nevertheless, it seems to occur in two specic cases, viz., in high purity aluminium and in aluminium alloys containing large particles: 1. Single crystals and polycrystals of 99.999 wt.% aluminium have been subjected to hot deformation in compression by Yamagata [15]. Stress-strain curves exhibit strong oscillations, typical of DDRX, although more irregular. The associated microstructures generally display new grains without substructure. It is therefore not excluded that these grains have grown after deformation, all the more as aluminium of such high purity recrystallizes statically very rapidly, even at room temperature. However, one micrograph [3] clearly displays the presence of several grains containing a substructure, in an initially monocrystalline sample. Moreover,

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the occurrence of DDRX in high purity aluminium has been recently conrmed by Ponge et al. [6]. High purity produces two opposite effects. On the one hand, it favors DDRX by increasing grain boundary mobility. On the other hand, it can inhibit DDRX since the high level of recovery prevents dislocation accumulation, thus reducing the driving force. Experimental results indicate that the rst effect prevails over the second [7]. 2. There is some evidence that DDRX can occur during hot deformation of Al Mg Mn alloys, because a high Mg solute addition raises the dislocation density and thus the driving force for DDRX, while large Al6Mn particles ( \ 1 mm) stimulate nucleation. The presence of small new grains adjacent to large particles has been reported for instance after plane strain compression of Al-1wt.% Mg-1wt.% Mn [8] and extrusion of Al-5wt.% Mg-0.8wt.%Mn [9]. However, the volume fractions of recrystallized grains remained small and no effect on the shapes of the stress-strain curves was detected. This means that DDRX is a possible but limited restoration mechanism in aluminium alloys. Continuous dynamic recrystallization occurs in turn by the progressive accumulation of dislocations in low angle boundaries, leading to the increase of their misorientation and the formation of large angle grain boundaries when their misorientation angles reach a critical value qc (qc : 15). This mechanism has been observed in several high stacking fault energy metals, such as aluminium and aluminium alloys [1013], b titanium alloys [14 16], and ferritic steels [17 20]. The microstructure of a commercial purity (1050 grade) aluminium strained in torsion has been investigated by Perdrix et al. [10], and Montheillet [11]. These authors found that, at small and medium strains (m : 1), the microstructure consists of the deformed initial grains containing subgrains, which is typical of a recovered state. By contrast, strongly strained samples (m : 40) exhibit a completely different microstructure: it is no longer possible to distinguish the initial grains, and the former subgrains now appear as crystallites bounded partly by low and partly by high angle boundaries. Furthermore, the misorientation angles, which display a bimodal distribution at small strains (with subgrain boundaries less than 15 and initial grain boundaries between 30 and 63) become uniformly distributed between 0 and 63 at large strains. Perdrix et al. [10] have explained these results by assuming a progressive transformation of subgrain boundaries into grain boundaries. However, this mechanism remains controversial and some authors have suggested that the increased fraction of high angle boundaries could result from GDRX. Nevertheless, there is a general agreement to consider that the transformation of low angle boundaries into

high angle boundaries effectively takes place when the boundaries are pinned by small particles. This mechanism has been used to promote superplasticity in Zr bearing or high Mg aluminium alloys (Al-6wt.%Cu0.4wt.%Zr [21,22], Al-0.25wt.% Zr-0.1wt.% Si [23,24], Al-10wt.% Mg-0.1wt.% Zr [25,26], Al-10wt.% Mg0.5wt.% Mn [27,28]). These alloys are generally cold or warm rolled, to increase their dislocation density. Under these conditions, subgrains form very quickly during the subsequent hot tension testing. Since the boundaries are pinned by small particles (Al3Zr, (Al8Mg5)b or Al6Mn, according to the alloy composition) and continuously absorb dislocations, the subgrains transform into grains without growing. A ne and equiaxed grain structure is thus obtained in the early stages of superplastic deformation. Finally, geometric dynamic recrystallization has rst been described by McQueen et al. [29] in a commercial purity aluminium. During deformation, the original grains atten (compression) or elongate (tension, torsion), and their boundaries become progressively serrated while subgrains form. Consequently, the grain boundary area per unit volume grows strongly and an increasing fraction of subgrain facets is made of those initial grain boundaries. Ultimately, when the original grain thickness is reduced to about two subgrain sizes, the grain boundaries begin locally to come into contact with each other, causing the grains to pinch-off [29 32]. In the case of Al-5Mg alloys, the tendency to the serration of boundaries is stronger and a secondary process of GDRX by pinching off of the serrations has been reported [33,34]. The rst purpose of this work was to bring forward further evidence for CDRX. The main objection to the results of Perdrix et al. [10] was that the high fractions of large angle boundaries did not necessarily result from CDRX, but could also be due to the evolution of the initial grain boundaries. In order to exclude the latter possibility, single crystalline samples were used. The second objective was to better characterize CDRX. The inuence of the following parameters was therefore investigated: crystalline orientation, by using single crystals of various orientations; purity, by testing three grades of polycrystalline aluminium, ranging from 99.99 to 97 wt.% Al. Impurities and alloying elements reduce the recovery capacity of the material, since they decrease its stacking fault energy (although this effect seems to be relatively weak in aluminium alloys) and solutes as well as precipitates reduce the dislocation mobility; strain path, by comparing the microstructures obtained from uniaxial compression and torsion tests.

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Table 1 Chemical compositions of the three aluminium grades Mg 1199 (mg/g) 1200 (mg/g) 5052 (wt.%) 7 9 2.49 Si 12 1500 0.11 Cr 1 62 0.2 Mn 1 82 0.08 Fe 10 5700 0.3 Cu 45 59 0.01 Zn 4 200

2. Experimental procedure The three selected grades of aluminium, a pure 1199 aluminium, a commercial purity 1200 aluminium and an AlMg 5052 alloy (Table 1), were provided by the Centre de Recherches de Voreppe (Pechiney) in the form of hot rolled plates. The initial structures were fully recrystallized, exhibiting equiaxed grains of 220 mm in the 1199 aluminium, attened grains of average size 200 mm in the 1200 aluminium, and again equiaxed grains of 80 mm in the 5052 alloy (Table 2). The textures displayed a strong cube component, especially in the 1200 grade. Cylindrical compression specimens were machined with their axes parallel to the rolling direction. In addition, torsion specimens were prepared from the 1200 aluminium with the torsion axis parallel to the rolling direction. Finally, single crystals were grown from the 1199 aluminium and sectioned to obtain cubic specimens with a 001, 011 or 111 direction parallel to the compression axis (Table 3). Hot compression tests were carried out at a constant strain rate m; = 10 2 s 1 and 0.7 Tm (i.e. 380, 368 and 333C for the 1199, 1200, and 5052 grades, respectively). The specimens were lubricated with graphite to minimize strain inhomogeneities, and water quenched within 1 s after deformation. The torsion specimens were strained under the same strain rate and temperature conditions, and water quenched within 5 s. The compression specimens were then sectioned parallel to the axis, ground and electropolished (5 ml HClO4, 95 ml C2H5OH, 20 V, 0C, 60 s); some of them were subsequently anodized (10 ml HBF4, 90 ml H2O, 30 V, 20C, 120 s). Since deformation was not uniform, local strains were estimated using a mechanical model [35]. In what follows, the strain values correspond to the center part of each specimen, where all observations were carried out. However, even at large strains, the strain gradient was quite low, e.g. in the compression direction, Dm /Dz : 0.2 mm 1 at m = 1.5 [35]. The torsion cylinders were ground to obtain a at surface, and then prepared the same way. The strain and strain rate undergone by these samples were estimated to approximately 80% of their nominal (surface) values. The deformed microstructures and textures were investigated using polarized optical microscopy (POM) on the anodized specimens, scanning electron microscopy (SEM) in the channeling contrast mode, elec-

tron back-scattered diffraction (EBSD) and X-ray diffraction on the electropolished specimens. POM displays both the initial grains and the new crystallites (subgrains or new grains), whereas only the crystallites are generally revealed by SEM. This is due to the fact that POM colors are related to the crystalline orientations, and the original grains are associated with regions of similar colors. This is not the case in SEM, where crystallites of similar orientations can display quite different grey levels, and conversely. However, POM is known to overestimate subgrain sizes [31,36,37], and is therefore inadequate for quantitative analyses of the substructure. For this purpose, SEM micrographs were therefore used. Moreover, the color contrast in POM is not precise enough to distinguish a new grain from a subgrain and even less to estimate the misorientation between two crystallites. The orientation of each crystallite was thus determined using EBSD and the misorientation associated with each boundary subsequently calculated. On account of detection limitation in hot worked structures, boundaries with a misorientation angle of less than 1 were not taken into consideration. This omission is likely to be of no consequence, however, since the study is focused on the transition from low angle to high angle boundaries around 15. In addition to these local texture measurements, global textures were investigated by X-ray diffraction.
Table 2 Mean intercept lengths of the grains in the hot rolled plates along the rolling (RD), transverse (TD), and normal (ND) directions RD 1199 (mm) 1200 (mm) 5052 (mm) 226 285 78 TD 204 215 86 ND 227 98 59

Table 3 Crystallographic directions parallel to the compression axis (CA) and perpendicular to the lateral faces (TD1 and TD2) of the cubic single crystals CA [001] [011] [111] TD1 [100] [100] ( 0] [11 TD2 [010] (] [011 (] [112

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3. Experimental results

3.1. Pure aluminium single crystals


During the compression tests, the cross-sections of the 001 specimens remain square, as expected since the 001 crystallographic axis and the geometric axis (square cross-section) are both fourfold, and the transverse directions TD1 and TD2 are crystallographically equivalent (Table 3). The 011 (twofold crystallographic axis) specimens lengthen in the 100 direction. It has been shown [38] that this shape change can be explained by the activation of the four octahedral slip ( ], (111)[11 ( 0], (1 ( 11)[1 ( 01 ( ], and (1 ( 11)[1 (1 ( 0]. systems (111)[101 Finally, the cross-sections of the 111 specimens become irregular, which is due to the combination of their threefold crystallographic axis and four-fold geometric axis. Fig. 1 shows that the ow stresses reach a steady state value of about 10.5 MPa in the case of the 001 and 111 specimens (note that the polycrystal ow stress tends to the same value); by contrast, it is much higher for the 011 specimens (about 14 MPa). It will be shown below that these values are closely related to the subgrain sizes. The ow stress drop associated with the 111 crystals can be mainly attributed to the evolution of the Taylor factor: indeed, at m = 0, M = 3
3/2 : 3.67, while at m = 1.5 (101 orientation, see below) M =
6 : 2.45. Global texture measurements show that the 011 orientation is perfectly stable (Fig. 2(b)). The 001 orientation is also fairly stable, since its decomposition only starts at m = 1.5 (Fig. 2(a)). On the other hand, the 111 orientation is very unstable (Fig. 2(c)). At m = 0.3, the compression axis is roughly parallel to 112 and eventually reaches the 011 stable orientation at m = 1.5. These results are in good general agreement with the literature, although the rotation amplitudes are larger than those observed by Me cif et al. [39], after uniaxial compression of aluminium single crystals at the same temperature. This difference can be attributed, to a large extent, to the higher strain (m = 1.5 vs 0.35) and strain rate (10 2 vs. 2 10 4 s 1) applied in the present work. The aspect of the sections perpendicular to the compression axis does not change signicantly with increasing strain for the 100 specimens observed by POM (Fig. 3(a, b)). However, the band structure observed on the lateral sections at m = 0.3 transforms into a subgrain structure at larger strains. It should be noted that SEM reveals the presence of many subgrains within these bands. The 011 specimens exhibit symmetrical mosaic ( ) lateral sections (Fig. 3(c, d)), with patterns on their (011 dislocation walls parallel to the planes of the activated slip systems. SEM also reveals the formation of small subgrains inside the cells at m = 1.5. Such a mosaic microstructure of the 011 specimens (which

Fig. 1. Stress-strain curves of the 001, 011, 111 single crystals and polycrystals of 1199 aluminium.

Fig. 2. Global textures of the monocrystalline specimens strained to m = 1.5. (a) 001; (b) 011; (c) 111. The horizontal and vertical axes are associated with the TD1 and TD2 directions, respectively (Table 3).

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elongate only in the [100] direction) has already been observed in the case of single crystals of various orientations deformed by channel die compression [40]. This suggests that such a particular structure is due to the geometry of the slip systems, which allows a unidirectional strain to take place. By contrast to the previous orientations, the 111 specimens exhibit an inhomogeneous microstructure. Horizontal and tilted bands are displayed on the TD1 lateral sections at m = 0.3. However, this inhomogeneity tends to vanish at larger strains. Misorientation maps were plotted from EBSD measurements for each single crystal strained to m = 1.5. In the 001 specimen (Fig. 4(a)), a large number of boundaries exhibit a misorientation greater than 15, which indicates that subgrain boundaries have transformed into grain boundaries. By contrast, the boundaries in the 011 specimen (Fig. 4(b)) exhibit low misorientations, generally smaller than 6, so that no high angle boundaries have formed. The behavior of the 111 specimen (Fig. 4(c)) is intermediate, since only a small fraction of the interfaces consists of high angle boundaries.

The evolutions of the misorientation distributions with increasing strain are compared for the three orientations in Fig. 5. In the case of the 001 crystal, the average misorientation strongly increases with strain. At m = 0.9, a signicant fraction of misorientations already exceeds 15, which clearly means that part of the low angle boundaries have transformed into large angle boundaries. At m = 1.5, this trend is more pronounced, since almost 20% of the interfaces are now grain boundaries. However, the microstructural steady state is not yet attained, which suggests that a more recrystallized microstructure (with crystallites bounded mainly by large angle boundaries) could form at larger strains. By contrast, for the 011 orientation, all the measured misorientations are lower than 15, even at m = 1.5. Furthermore, no evolution is noticeable between m = 0.9 and 1.5, and thus, the formation of grain boundaries is unlikely, even at larger strains. The behavior of the 111 specimens is more complex. In particular, the specimen strained to m = 0.9 has developed a large amount of very high angle boundaries (3060). This is due to the splitting of the initial orientation into two components (Fig. 6), which was

Fig. 3. POM microstructures of the monocrystalline specimens. (a) 001, m = 0.3; (b) 001, m = 1.5; (c) 011, m = 0.3; (d) 011, m = 1.5.

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Fig. 4. SEM micrographs and associated misorientation maps of the monocrystalline specimens strained to m = 1.5. (a) 001; (b) 011; (c) 111. The vertical and horizontal axes are associated with the CA and TD1 (001 or 011) or TD2 (111) directions, respectively (Table 3).

observed in only one specimen of this orientation. It should also be pointed out that, in the case of this unstable orientation, large angle boundaries are formed in the early stages of the deformation: at m = 0.3, they already represent more than 8% of the boundaries.

3.2. Polycrystalline specimens


The mechanical behavior of the various specimens

obtained from the compression and torsion tests was investigated (see Fig. 1 for the 1199 grade). In all cases, the ow stress seems to reach a plateau at m : 0.3 (although a small decrease of the torsion stress is expected at very large strains [10,11]). The ow stresses reach steady state levels of 10.5, 21 and 77 MPa for the 1199, 1200 and 5052 grades, respectively. Global texture measurements were carried out on the compression specimens. The pole gures of the three grades (Fig. 7

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( : average misorientation Fig. 5. Strain dependence of the misorientation distributions for the three single crystals (N : number of measurements, q angle).

Fig. 6. Formation of deformation bands in the 111 specimen strained to m = 0.9.

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Fig. 7. Global texture of the 1199 polycrystalline specimen strained to m = 1.5. The horizontal and vertical axes are associated with the TD and ND directions, respectively (Table 2).

All the microstructures are quite homogeneous. At m = 0.3, subgrains are well formed in the 1199 and 1200 grades (Fig. 8(a)), whereas they are not visible in the 5052 grade, because their formation is delayed by the strong solute content of this alloy. Note also that at m = 1.5, the grain thickness is still much larger than the subgrain size (Fig. 8(b)), which indicates that the initial grains are far from decomposing into smaller grains by a GDRX process. In Fig. 9, the mean intercept lengths D of the subgrains measured from the SEM micrographs are compared with a theoretical value calculated from the ow stress |, using the relationship | /G = hb / D. The value of h = 28 was chosen here, since it is commonly used for aluminium [34]. In the case of the 1199 and 1200 grades, the calculated subgrain sizes are consistent with the measured ones, although slightly larger. The coefcient 28 seems therefore overestimated, and a better agreement between the two sets of data is obtained by using a value of 24. However, according to Blum et al. [34], this difference is due to the condensation of free dislocations into additional subgrain boundaries between the end of deformation and quenching, which causes a decrease of the average size D. By contrast, the calculated subgrain size is much smaller than the experimental value for the 5052 alloy. This is due to the slow formation of the subgrains in that case, since the presence of regions without wellformed subgrains leads to an overestimation of the mean intercept length. Fig. 10 displays misorientation maps of the polycrystals strained to m = 1.5. In the 1199 specimen (Fig. 10(a)), two initial grain boundaries can still be identied because they form a continuous chain of high misorientation segments ( \ 30), whereas isolated high angle boundaries with lower misorientations (1530) are very probably new grain boundaries. In the case of the 1200 aluminium strained in compression (Fig. 10(b)), the map shows the presence of a large fraction

Fig. 8. POM microstructures of the 1200 polycrystalline specimens. (a) m = 0.3; (b) m = 1.5. The compression axis is vertical.

illustrates the texture of the 1199 aluminium) show that the texture consists mainly of a 011 ber component, which is especially strong for the 5052 alloy. Since a strong cube component was observed in the initial state, this means that the crystallites have strongly rotated during compression.

Fig. 9. | /G versus b /D plot for the single crystals and polycrystals strained to 1.5 (the shear moduli G = 20.6, 20.8, 21.2 GPa for the 1199, 1200, 5052 grades, respectively, at 0.7 Tm, and the Burgers vector length b = 2.86 10 10 m).

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Fig. 10. SEM microstructures and associated misorientation maps of the polycrystalline specimens strained to m = 1.5. (a) 1199 specimen; (b) 1200 compression specimen; (c) 1200 torsion specimen. The compression axis is vertical.

of high angle boundaries, but the original grain boundaries are no longer recognizable. It is likely that subgrains have rotated more in the 1200 than in the 1199 grade, thus leading to a fragmentation of the initial grain boundaries. In the torsion specimen of Fig. 10(c), the fraction of high angle boundaries is very similar, although some chains of segments exhibiting very large misorientations at the top of the map look like initial grain boundaries. The misorientation distri-

butions of the 1199 aluminium are depicted in Fig. 11. For this aluminium, as for the two other grades, there is a progressive shift of the small misorientations towards the larger ones, which leads to an increase of the average misorientation of about 8 between m = 0.3 and m = 1.5. The fraction of subgrain boundaries with small misorientations ( B 6) is strongly reduced; the number of subgrain boundaries with larger misorientations increases at rst, and then decreases, whereas the fraction

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of high angle boundaries continuously increases, reaching more than 30% at m = 1.5. This indicates that the very low angle boundaries ( B 6) are continuously converted into medium angle boundaries (6 15), which in turn transform into high angle boundaries. Such an evolution may be referred to as continuous recrystallization.

3.3. Comparison of the geometric and continuous dynamic recrystallization kinetics


In the polycrystalline specimens, the increase of the high angle boundary fraction is due not only to the formation of new grain boundaries, but also to the expansion of the initial grain boundary area. In order to get a quantitative estimation of the respective effects of CDRX and GDRX, a geometrical model was used. The evolutions of the lengths per unit area of initial grain boundaries, new high angle boundaries, and low angle boundaries were determined from a simple derivation detailed in the Appendix A. Fig. 12(ae) illustrate the GDRX and CDRX kinetics. The strain dependence of the initial grain boundary fraction is not monotonic since it grows due to the attening of the initial grains, whereas the formation of subgrain boundaries makes it decrease. At m = 1.5, the initial grain boundaries represent about 8% of the interfaces for the 1200 and 5052 grades. The 1199 aluminium differs by a much higher fraction, about 17%, which is due to a smaller initial grain size/subgrain size ratio. By comparing the thickness h of the initial grains at m = 1.5 (the latter were estimated by calculation to 68, 80, and 33 mm for the 1199, 1200, and 5052 grades, respectively) and the subgrain sizes D at the same strain (14.3, 6.6 and 3.4 mm, respectively), it appears that the h /D ratios are about 5 for the 1199 grade, and 1012 for the 1200 and 5052 grades. This conrms that GDRX is more developed in the pure aluminium. But this ratio still remains far from 2, which means that the strain achieved by compression is not large enough to obtain a complete GDRX structure.

With regard to CDRX, the 001 single crystal (Fig. 12(d)) and the polycrystal of same purity (and strong initial cube texture, Fig. 12(a)) display similar behaviors: at m = 1.5, roughly 1518% of their interfaces consist of new high angle boundaries. When deformation bands form in the 111 crystal, the fraction of new grain boundaries rises very quickly; if not, it remains rather small, about 58%. Among the polycrystalline specimens, the highest fraction of new grain boundaries is observed in the 1200 specimens (35% in compression, 39% in torsion at m = 1.5), then in the 5052 alloy (about 24%), and last in the pure aluminium (only 15%). This can be explained by the very high recovery rate in pure aluminium, which lowers the accumulation rate of dislocations in the subgrain boundaries. On the other hand, in the Al-Mg alloy, the solute atmospheres impede dislocation movements, thereby delaying the formation of subgrain boundaries [7]. It should be noted that the grain boundaries present in the 1199 aluminium originate in equal parts from GDRX and CDRX, while those present in the 1200 and 5052 grades have mainly developed by CDRX. The present results also indicate that the compression and torsion specimens display quantitatively the same behavior. Therefore, the strain path does not seem to modify the CDRX kinetics signicantly.

4. Discussion

4.1. New grain boundaries and deformation bands


Experiments carried out on single crystals conrm that the subgrain boundary misorientations strongly increase with strain: a maximum of at least 15 is reached for the three investigated orientations at m = 0.9. Moreover, the transformation of low angle boundaries into high angle boundaries is clearly demonstrated for the two unstable orientations, as well as in the polycrystalline specimens where the fraction of high angle boundaries is much larger than expected for the deformed initial grain boundaries.

( : average misorientation). Fig. 11. Strain dependence of the misorientation distributions for the 1199 polycrystals (N : number of measurements, q

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Fig. 12. Strain dependence of the surface fractions pertaining to the various kinds of interfaces, viz. low angle boundaries (LAB), new high angle boundaries (nHAB) [including the deformation band boundaries (DB)], and old initial high angle boundaries (oHAB). (a) 1199 polycrystals; (b) 1200; (c) 5052; (d) 1199 001; (e) 1199 111.

However, the misorientation increase of the subgrain boundaries and their transformation into high angle boundaries has been controversial for a long time, principally on the basis of the work by Kassner and McMahon [30]. These authors studied the microstructural evolution of high purity (99.999 wt.%) polycrystalline aluminium specimens strained in torsion (370C, 5 10 4 s 1). The observations were mainly carried out by transmission electron microscopy, and the misorientations were estimated from either dislocation spacings (subgrain boundaries) or selected area diffraction patterns (grain boundaries). These authors noticed only very limited increases in subgrain misorientations with strain: the mean values varied from 0.5 at m = 0.2 to a saturation value of 1.2 from m = 1.2 to 16. Most of the discrepancies between this prior work and the present investigation can be explained by differences in the experimental procedures. First of all, the aluminium used by the authors was purer, and the strain rate, lower. This means that recovery was more efcient, and thus the increase in misorientation was slowed down. Furthermore, by contrast to the SEM-EBSD technique used here, TEM allowed to account for boundaries with very low misorientations ( B 1), therefore decreasing the average misorientation value. However, some boundaries with medium (about 10), and large misorientations ( \ 30) were also observed by Kassner and McMahon [30]. Since a limited number of measurements (about 20 for each specimen) were carried out, the authors misorientation distributions are not smooth and discontinuous values are observed within the range 515, instead of the continuous distributions displayed here (Figs. 5 and 11). This is a reason why these medium angle boundaries, which were also present in single crystalline specimens strained under similar conditions [41], were interpreted as interfaces between persistent deformation bands (although such bands were not clearly identied), and not as former subgrain boundaries transformed into new grain boundaries. It should be noted that the classication of the various boundary types has been developed in the case of cold deformation and its application to hot worked structures in not obvious. Indeed, at temperatures below 0.4 Tm, several kinds of interfaces are observed. The initial grains decompose into deformation bands separated by a thin (12 mm) transition band containing dislocation cells. Inside the deformation bands, random low misorientation cells are grouped together in cell blocks separated by dense dislocation walls of higher misorientations [43]. However, as temperature increases, dislocation walls become thinner and a much more homogeneous microstructure develops. Generally, above 0.6 Tm, only equiaxed subgrains are observable inside the deformed initial grains. Even when a decomposition occurs, the deformation bands are not easily

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observed on micrographs (Fig. 6). The reason is that they appear bounded by true grain boundaries, instead of the straight above-mentioned transition bands. Differentiation between several types of low and high angle boundaries is therefore difcult in hot worked structures, and the relevance of such a classication even questionable.

4.2. Inuence of crystalline orientation


Results obtained on single crystals conrm that the CDRX kinetics strongly depend on the crystallographic orientation. The fully stable 011 orientation enables only a limited increase of the misorientations. No high angle boundary creation was observed, although some misorientations are close to 15 at m = 0.9. In the case of the quasi-stable 001 orientation, the formation of new high angle boundaries, with 15 30 misorientations, was observed in the specimens strained to m = 0.9 and 1.5. For the 111 orientation, which is fully unstable, new grain boundaries in the same misorientation range were observed, starting even at m = 0.3. Such results are in total agreement with previous work on aluminium single crystals. Theyssier et al. [40] observed, after channel die compression of single crystals of the same purity, that some orientations (e.g., {112}111 or {421}112) led to the formation of high angle boundaries, whereas other ones (e.g. {110}112) did not. More recently, Ponge et al. [6] investigated the misorientations developed during hot uniaxial compression (260C, 4 10 4 s 1) of a very high purity aluminium (99.9995 wt.%), which recrystallized by DDRX. In the unrecrystallized matrix, these authors observed the occurrence of smaller misorientations in the 011 single crystal ( B 9), than in the 112 specimen (up to 26). The misorientation ranges were thus very close to those obtained in the present work.

4.3. Continuous dynamic recrystallization and grain rotations


In order to clarify the origin of the new high angle boundaries, it is interesting to look more closely at the relationship between global texture and local misorientations. In the case of uniaxial compression, the following remarks can be made: 1. Stable orientation. During straining, the global texture of the 011 crystals remains unchanged, except that it becomes slightly less sharp. This is due to strain hardening and dynamic recovery: dislocations accumulate in the subgrain boundaries, thus altering the initial orientation. Misorientations up to 15 have been reported in pure aluminium single crystals. The results obtained on polycrystals indicate that in a less pure aluminium, such as the 1200 grade, the misorientations are probably larger, thus

leading to the formation of high angle grain boundaries. A question still remains open: which mechanism leads to the increase in misorientation? If one considers that dislocations of opposite signs are created in equal densities during straining, each dislocation wall will absorb dislocations of both signs, keeping its misorientation at a low level. A misorientation increase can only occur if a subgrain boundary absorbs an excess of dislocations of one sign, which supposes that the various types of dislocation are not uniformly distributed in the material. This assumption does not seem unrealistic, however, all the more as misorientations between adjacent subgrains will increase such inhomogeneities. Indeed, slip system activities can be affected by small orientation changes. Furthermore, among the various orientations introduced by strain, those belonging to the 011 ber are fully stable and will probably not disappear, thus leading to increased and permanent misorientations. A slight trend towards ber formation in the pole gure of the 011 crystal strained to m = 1.5 can be noticed (Fig. 2(b)). If compression specimens could be deformed to very large strains, a 011 ber texture would certainly be observed. 2. Unstable orientations. New interfaces can be introduced by both strain hardening and lattice rotations. Two cases must be distinguished, according to whether deformation bands occur or not. Let us rst consider the case in which the whole crystal rotates towards the same orientation. In the 111 single crystal strained to m = 0.3, the EBSD local pole gure clearly shows that some orientations still remain close to the initial one, whereas others are already located near the nal one. That is why high angle boundaries are observed at such a low strain. However, at m = 1.5, all the crystallites have reached their nal 011 orientation, which explains the lower fraction of high angle boundaries. The subsequent behavior has been described in (i). In the second case, when the initial orientation splits into symmetrical components, very large and permanent misorientations are rapidly built up. Deformation bands are expected to occur only for specic initial orientations, e.g. 001, 111, or the intermediate uuw orientations, and they are more likely to occur in single crystals than in polycrystals (except for very large initial grains). Lyttle and Wert [23] have formulated three models based on dislocation glide, boundary sliding, and neighbor switching to account for the increased misorientations during straining of superplastic alloys. They concluded that combination of the boundary sliding model and the neighbor switching model most closely reproduced the misorientations measured experimentally. In the case of the dislocation glide model, the

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misorientations tended to decrease rather than increase, therefore reecting texture development. However, it can be inferred from the above discussion that the convergence of the crystallite orientations and the creation of large misorientations are not incompatible. A reason is that strain hardening tends to move the crystallites away from their ideal orientations. This effect was probably very pronounced in this case because of the low recovery level associated with high alloying element content. Moreover, it was experimentally found that, for some reason, the lattice rotation rate varied from one crystallite to another, thus introducing high misorientations during the transient. All these disturbing factors were not taken into account in the model. The increase in subgrain boundary misorientation by accumulation of dislocations was probably predominant in the early steps of straining. However, since the crystallite size was very small, grain boundary sliding and grain switching probably prevailed as soon as large enough misorientations were built up.

parameter of the ow stress. The assumption of McQueen and Blum was based mostly on creep data from specimens deformed to low or moderate strains, which can explain why these authors did not observe any misorientation increase of the subgrain boundaries.

4.5. Elementary mechanisms of the continuous dynamic recrystallization


Continuous dynamic recrystallization has sometimes been labeled extended dynamic recovery, either because some authors restrict the term recrystallization to the classical discontinuous recrystallization, or because the microstructures generally consist of crystallites only partially bounded by high angle boundaries. This terminology is somewhat misleading, however, since dynamic recovery can have detrimental as well as benecial effects on CDRX. Indeed, the above experimental observations indicate that the CDRX process results from the combination of three elementary mechanisms: 1. The formation of subgrain boundaries. These boundaries are created with a very low misorientation angle (about 1), as a result of dynamic recovery. 2. The transformation of subgrain boundaries into grain boundaries. The increase in misorientation of the subgrain boundaries is more or less rapid, according to the material and the experimental conditions. It was shown that it is accelerated by medium recovery levels and when the initial orientation is unstable. If such favorable conditions are brought together, the subgrain boundaries can be gradually transformed into grain boundaries. 3. The elimination of subgrain and grain boundaries. Measurements carried out on a b titanium alloy [13,47] and some aluminium alloys have recently shown that the grain boundaries migrate, even in the absence of classical DDRX, although at much lower rates. All the interfaces present in the volume swept by the migrating boundaries disappear, which certainly plays a major role in the establishment of the steady state, for both GDRX and CDRX. It has been shown for instance that, in compression, the initial grains can reach a quasi-steady state thickness, which is an increasing function of the boundary velocity [13,47]. Moreover, the elimination of interfaces allows the subgrain size and the misorientation distribution to stabilize after a transient period. From the previous experimental observations, a model of CDRX has recently been proposed, in which the above three mechanisms are combined in order to predict the microstructural evolutions [38,48]. The main features are well reproduced: during the transient, the subgrain size decreases while the misorientation grows, and the subgrain boundaries are gradually converted

4.4. Kinetics of the continuous dynamic recrystallization


It is worth noting that the various mechanical and structural parameters tend to their steady state values at different rates. The ow stress remains approximately constant from m = 0.3, except for the 111 crystal. In this case, the crystallographic rotation delays the steady state up to m = 0.9. The subgrain size is generally well established at m = 0.3. However, a subgrain renement is still observed in the 5052 alloy at m = 1.5. By contrast, the misorientations are not yet stabilized at m = 1.5, with the only exception of the 011 crystal. This is due to the combined effects of the increasing misorientations of the subgrains and newly formed grain boundaries on the one hand, and the increasing surfaces of the original grain boundaries on the other hand. Apart from some minor cases, the ow stress and the average subgrain size thus reach their steady state values quite rapidly (m = 0.3), while the average misorientation is still increasing at m = 1.5. These experimental results are thus in contradiction with the similitude principle, which stipulates that the various microstructural spacings are inversely proportional to the ow stress. For instance, McQueen and Blum [42,44] proposed that there is a unique relationship between the average dislocation spacing s in the subgrain boundaries, (or, equivalently, the average subgrain boundary misorientation q : b /s ) and the ow stress. The fact that the average subgrain boundary misorientation increases without affecting the ow stress signicantly can be explained if one considers, as established by several authors [45,46], that the strengthening associated with dislocations inside the subgrains is larger than that due to dislocations in the subgrain boundaries. The former is thus the main controlling

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into grain boundaries; ultimately, the crystallite size reaches a steady state value, as well as the misorientation distribution, although at larger strains.

Acknowledgements The authors are indebted to Professor J.J. Jonas, McGill University, Montreal, for providing access to the torsion facility. They are also grateful to Professor H.J. McQueen, Concordia University, Montreal, for many fruitful discussions. The work of S. Gourdet was supported in part by the Re gion Rho ne-Alpes, France, through a scientic fellowship (Avenir program).

5. Conclusions Various aluminium specimens were submitted to uniaxial compression and torsion testing at 0.7 Tm and 10 2 s 1, up to m = 1.5. The main results obtained after investigation of the hot worked structures are the following. (1) Experiments carried out on 001, 011 and 111 single crystals conrm that the subgrain boundary misorientations strongly increase with strain. For the three investigated orientations, the largest values are close to or beyond 15. In the case of the stable 011 orientation, the increase in misorientation is not sufcient to transform low angle into high angle boundaries. Among the two other orientations, the conversion occurs earlier for the most unstable one: it starts at m = 0.3 in the unstable 111 crystal, but only at m = 0.9 in the metastable 001 crystal. (2) Most of the new high angle boundaries have 1530 misorientations. They originate either from differences in the rotation rate towards the nal orientation, or from uctuations around the average orientation introduced by strain hardening and dynamic recovery. In some cases, the initial orientation splits into symmetrical components, causing the occurrence of deformation bands. In this case, very high misorientations ( \ 30) are rapidly built up. (3) In the case of polycrystals, the high angle boundary fractions strongly increase with strain. Since both continuous and geometric dynamic recrystallization are likely to occur, calculations were carried out in order to estimate the surface fraction of the initial grain boundaries. It turns out that the high angle boundary fraction is much larger than could be accounted for by the expanded initial boundaries, thus conrming the presence of many new high angle boundaries. (4) Continuous dynamic recrystallization is more efcient in the commercial purity aluminium than in the pure aluminium and the Al-Mg alloy. This suggests that the transformation of low angle boundaries into high angle boundaries is faster when the recovery level is neither too high (the accumulation rate of dislocations in the subgrain boundaries decreases), nor too low (the formation of subgrains is very slow or they do not form at all). Comparisons between compression and torsion specimens also indicate that the strain path does not alter CDRX kinetics noticeably.

Appendix A The evolution of the fraction of the various interface types (i.e. low angle boundaries, initial and new high angle boundaries) is addressed here in the case of compression. Similar equations apply for torsion (see Ref. [38] for more details). Since experimental measurements provide interface lengths per unit area, a two-dimensional approach was chosen. Initial grains and subgrains are approximated by ellipses with semiaxes a = y /4 DCA and b = y /4 DTD, where DCA and DTD denote the measured intercept lengths parallel to the compression axis and the transverse direction, respectively. The mean intercept lengths of the initial grains can be accurately measured only at m = 0. Their evolutions with strain are evaluated by taking into account the attening of the grains and the migration of the initial boundaries, which leads to an increase of the average thickness [13,38]. Along the direction parallel to the compression axis: : CA = DCAm; + 26 D (1) where the migration rate 6 = 0.1 mm/s at m; = 0.01 s 1 [13,38]. This yields after integration: DCA = (D0 DS) exp( m ) + DS (2) where D0 is the initial length and DS = 26 /m; , or, for the semiaxis: ag = (a0 aS) exp( m ) + aS (3) where aS = y6 /2m; . Moreover, perpendicular to the compression axis: bg = b0 exp(m /2) (4)

(in the above equations, a0 and b0 are the semiaxes lengths at m = 0). In addition, the initial grain boundary length is affected by the presence of serrations. Measurements from POM micrographs showed that the length ratio k between a serrated and a straight boundary rst increases with strain (as subgrains form) and then remains approximately constant. This evolution can be accurately described by the equation k = 1 + 0.25 [1 exp( 4m )] . The current length per unit

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S. Gourdet, F. Montheillet / Materials Science and Engineering A283 (2000) 274288 [20] P. Cizek, B.P. Wynne, Mater. Sci. Eng. A230 (1997) 8894. [21] R.H. Bricknell, J.W. Edington, Metall. Trans. 10A (1979) 1257 1263. [22] R.H. Bricknell, J.W. Edington, Acta Metall. 27 (1979) 1303 1311. [23] M.T. Lyttle, J.A. Wert, J. Mater. Sci. 29 (1994) 33423350. [24] H. Gudmundson, D. Brooks, J.A. Wert, Acta Metall. Mater. 39 (1991) 19 35. [25] E.-W. Lee, T.R. McNelley, Mater. Sci. Eng. 93 (1987) 4555. [26] S.J. Hales, T.R. McNelley, Acta Metall. 36 (1988) 12291239. [27] T.R. McNelley, E.-W. Lee, M.E. Mills, Metall. Trans. 17A (1986) 1035 1041. [28] E.-W. Lee, T.R. McNelley, A.F. Stengel, Metall. Trans. 17A (1986) 1043 1050. [29] H.J. McQueen, O. Knustad, N. Ryum, J.K. Solberg, Scripta Metall. 19 (1985) 73 78. [30] M.E. Kassner, M.E. McMahon, Metall. Trans. 18A (1987) 835 846. [31] J.K. Solberg, H.J. McQueen, N. Ryum, E. Nes, Phil. Mag. 60A (1989) 447 471. [32] G.A. Henshall, M.E. Kassner, H.J. McQueen, Metall. Trans. 23A (1992) 881 889. [33] W. Blum, Q. Zhu, R. Merkel, H.J. McQueen, Mater. Sci. Eng. 205A (1996) 23 30. [34] W. Blum, Q. Zhu, R. Merkel, H.J. McQueen, Z. Metallkde 87 (1996) 14 23. [35] B. Dumanowski, Thesis, 1997, Ecole des Mines de Saint-Etienne, France. [36] C. Perdrix, F. Montheillet, G. Wyon, F. Weill, Metallography 13 (1980) 289 297. [37] Q. Zhu, H.J. McQueen, W. Blum, High Temp. Mat. Proc. 17 (1998) 289 297. [38] S. Gourdet, Thesis, Ecole des Mines de Saint-Etienne, France, 1997. [39] A. Me cif, B. Bacroix, P. Franciosi, Acta Mater. 45 (1997) 871 881. [40] M.-C. Theyssier, B. Chenal, J.H. Driver, N. Hansen, Phys. Stat. Sol. (a) 149 (1995) 367 378. [41] M.E. Kassner, Metall. Trans. 20A (1989) 2182 2185. [42] H.J. McQueen, W. Blum, ICAA6, Japan Inst. Metals, pp. 99 112. [43] J.H. Driver, 16th Ris Int. Symp., Danemark, 1995, pp. 2534. [44] H.J. McQueen (section 9, R.D. Doherty, D.A. Hughes, F.J. Humphreys, J.J. Jonas, D. Juul Jensen, M.E. Kassner, W.E. King, T.R. McNelley, H.J. McQueen, A.D. Rollett), Mat. Sci. Eng. A238 (1998) 219 274. [45] M.E. Kassner, A.K. Miller, O.D. Sherby, Metall. Trans. 13A (1982) 1977 1986. [46] F.R. Castro-Fernandez, C.M. Sellars, Phil. Mag. 60A (1989) 487 506. [47] A. Girinon, Me moire CNAM, 1999, Conservatoire National des Arts et Me tiers, Saint-Etienne, France. [48] S. Gourdet, C. Chovet, F. Montheillet, in: T. Sakai, H.G. Suzuki (Eds.), 4th Int. Conf. on Recrystallization and Related Phenomena, The Japan Institute of Metals, Tsukuba, 1999, pp. 259264.

area of the initial grain boundaries is then given by kPg/2yagbg, where the ellipse perimeter Pg is calculated numerically from the lengths of the semiaxes ag and bg. Since the subgrain semiaxes asg and bsg can be measured at various strains, the total interface length per unit area is simply given by Psg/2yasgbsg. The total (old + new) high angle grain boundary length is then estimated by multiplying the total interface length by the fraction of high angle boundaries measured by EBSD (see the misorientation distributions). Finally, the length per unit area of the new high angle boundaries is obtained by difference.

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