Contents lists available at ScienceDirect Materials Science & Engineering A ELSEVIER journal homepage: www-elsevier.com/locate/msea The influence of deformation path on strain characteristics of AA1050 aluminium processed by equal-channel angular pressing followed by rolling @: MCV. Vega*, RE. Bolmaro®, M, Ferrante, V.L. Sordi’, AM. Kliauga** "tnt de sce Roser IER) FCEIACUNR, CONICET, B27 de Frere 210 Bx, S20002” Reva, Argentina ARTICLE INFO ABSTRACT Deceped 27 uly 2015 festa ering 28 fay 2015 ‘The present investigation reports on the microsructure evolution, texture development, the nature of the grain Boundaries and th tensile and deep drawing behaviour of commercial AAIO50 AI processed bY Equal Channel Angular Pressing (ECAP) plus rolling Although in terms of final mechanical strength ECAP and rolling are indistinguishable, the deformation pat is substantially different, and this has important Consequences on both microstructure and texture. From the spatial distribution of high angle grain boundaries (HAGE) and low angle grain boundaries (LAGE, the fine microstructure and the crytal= femede Ioguphicerare ws cone rhe micestucte ote scorns the eet nosed Severe plastic deformation flow: a spin movement in the ECAP process, which promotes the rotation of the cells inside the original ssn fran flowed y's sing moenen ese 8 te lle eang tran onan. Te EAP he Froese or cae nse se tion of A ah ee eens he sang [nensy oft ul cpraogapi ete Ara conequne an en ofthe peat dg and Aleformation strain, as meastred by the Erichsen test, was observed in saraples processed by 8 ECAP passes, characterized by low texture intensity and a high degree of dynamic recrystalization. ‘© 2015 Eleevier BV. Al ights reserved 1. Introduction It is well known that severe plastic deformation (SPD) is very, effective to achieve exceptional grain refinement because of the development of dense dislocation walls and simultaneous storage of less dense dislocation arrays, and thereby producing significant increase in the mechanical strength of metals and alloys (1,2) There are several SPD techniques, such as high-pressure torsion, ECAP, and accumulated roll bonding (ARB) among many others, ‘and all have been used successfull to refine the grain size down to submicrometer range in metals such as Al, Cu, and Ti (12). A umber of investigations [3-5] have also shown that ECAP de- formation can be combined with conventional forming processes, ssuch a5 cold rolling, to develop materials with properties, shape and dimensions suitable for a number of technological applications, In plastic deformation processes, with increasing strain the average dislocation density increases while the individual erys- talline size becomes smaller with increasing strain. For Al and ~Feerresponding autos mal edie: kiaugavseabe (AR Kiang} ther {ec metals at room temperature this two quantities reach their saturation at an imposed strain value of about 3-4 Grain size, for low alloy aluminums, usually does not decrease below the limit where Hall-Petch relationship has to be taken in account. Only dislocation density is correlated co the saturation of yield stress and hardness observed during SPD obeying the Taylor re- lationship [5) 29+ Math ie a ‘where ao is the yield strength of the annealed material, M is the ‘Taylor factor (usually 3), eis a constant (0.33 for pure AD), Gis the shear modulus, b is the Burgers vector and p is the disiocation density. This relationship is independent of the applied deforma- ‘tion process; for example for ARB |7,5], ECAP (9, multidirectional forging [10], oF HPT [1], the literature indicates a saturation value of 160-165 MPa for AATOSO, achieved alter a von Mises strain between 2 and 3 and a dislocation density atthe saturation point of about 15-3 x 10" m4, this last figure having been confirmed by x-ray diffraction [12,13]. This indicates that strength is basically determined by the interaction between dislocations. and in the case of high Stacking Fault Energy (SFE) metals, (Which isthe case of Al), operates mainly by the overall deformation of the cell blocks within the grain [14]. At a certain strain, the microstructureMCN. Wega ecal / Mater cence & Engineering A648 (2015) 154-162 15 ‘may sinmultaneously contain both low-angle cel (or grain) bound- aries (LAGBs) and high angle grain boundaries (HAGBs) equally contributing to the hardening behaviour, in which LAGBS form by random trapping of dislocations and HAGBs form between regions of different strain patterns to accommodate the accompanying diflerence in lattice rotation (15) The final grain size that can be achieved by SPD decreases at lower homologous processing temperatures and high strain rates [16.17], The grain size is also finer in low SFE, planar-glide, ma- terials and in alloys that contain elements that have a strong effect fn inhibiting recovery, such as Mg in Al [18] On the other hand, grain refinement by SPD. ic, the actual amount of HAGBs formed during deformation, is influenced by the deformation process and route. For instance, regarding ECAP a recent study by Li et al. 19] showed that grain refinement is most efficient when employing route A (no rotation of the sample be- tween passes) for dies having either 90 or 120° at the channels Intersection. Although the efficiency of grain refinement was lar ger forthe 90°, no difference in inal grain size was observed when {Al samples are processed by six or eight passes employing 90 or 120° angles. These observations confirmed prior reports by other authors [20}, For conventional rolling. in practical terms the amount of strain, imposed is limited by the occurrence of unreasonably small final thicknesses, and usually the process is operated at strains up to 2~ 2. Higher strains can be obtained by ARB or by 2 combination with another SPD process prior to rolling. As for the micro- structure produced in the latter process, Hurley and Humphreys 21] observed dislacation cells oriented within elongated micro- shear bands inside deformed grains, These bands, separated by LAGB, initially are approximately parallel to the Al planes of ‘maximum shear, hence they make an angle with the rolled di- rection, which decreases with accumulated strain, At high strains (eg. 2-3) all the HAGB were approximately parallel to the rolling direction, although low misorientation cell structures were found between the HAGB. Deformation route also has a substantial influence on texture, meaning that ECAP and rolling textures are very different. Thus, for ECAP the sample deforms in shear within a small area at the channels intersection. During the first deformation pass the slip planes tend to be oriented with their normal directions perpen- dicular to the shear plane and theie slip directions point towards the shear direction. For fec materials, the preferential textures are the (hkl) < 110> fibre when the < 10> direction is oriented in the shear ditection and the (111) fibre when the (111) plane is parallel to the shear plane and represents a rotation around the transverse axis of the die. The strength of a texture alter ECAP also depends on the orientations of the initial texture: the closer their components are to the predicted ones (after the rigid body rotation) the stronger they will be, because small fur- ther plastic spin will not highly perturb the texture. However the rule starts vanishing after various ECAP steps and the texture fi- nally smoothers out and decreases. Rolling on the other hand promotes strong textures; thus fee materials such as Al alloys develop a a-fbre texture, which is composed by the (112) < 111 > (Copper), (123) <634> (S) and {011} < 2M > (Brass) components ‘Within the SPD techniques a new trend is underway, thats, the association of different SPD methods, and the majority of such investigations is centred on conventional rolling following ECAP processing [22-24]. The here performed literature review clearly shows that these two deformation mades are very different in term of strain path, texture formation, and ultra-fine grain for- ‘mation mechanisms. However, there is a lack of studies on these phenomena when ECAP and rolling are sequentially performed. ‘Therefore, the alm of this paper is the study of microstructure evolution, texture development, the nature of the grain bound- aries and the tensile and deep drawing behaviour of commercial ‘AA1050 Al processed by ECAP plus rolling. 2. Experimental ‘The intial material, a commercial AA1050 alloy, came from roll, casting (Caster) process with an initial thickness of 7 mm and was deformed in the As Received (AR) condition without prior annealing ‘The SPD processing: took place in an ECAP die with @=120°, y=20" (curvature angle atthe channels intersection) and channel dimensions equal to 7 x 25 mm?, The equivalent strain per pass in this condition was 0.67 (25. The plates were cut into strip 7 mm. thick 25 mm wide and 70 mm long, maintaining the length par allel (o the rolling direction, which is also the deformation direc tion. ECAP processing was conducted employing route A (ie no sample rotation between passes). In order to determine the amount of strain induced by the CASTER process, samples were annealed at 350 °C 1 and subsequently rolled down to 30%, 50% 170% and 90% reduction. Another group of samples were deformed by ECAP up to 8 passes and ECAP up to 4 passes plus rolling to a final thickness of 2 mm (70%). Sample identification is as follows: “E" for ECAP processed samples followed by the number of passes and the letter "X’, °R’ for the rolled samples followed by the thickness reduction and “E+R" for the ECAP plus rolled samples. ‘The microstructure was revealed by conventional polishing techniques followed by anodizing (2.5% HBP solution, 20.V/3- 5 min); optical microscopy was performed under polarized light The deformed billets were also observed in a FEI Quanta scanning lection microscope (SEM) equipped with automatic orientation imaging mapping (OIM) and EDAXITSL software for Electron Backscatter Diffraction (EBSD). The scans were performed in the ND x ED plane of the metallographic prepared samples. Texture ‘was determined by x-ray diffraction on a Philips X-Pert MPD dif Jeactometer using Cu Ket radiation by the Schulz method. Samples for transmission electron microscopy (TEM) were prepared by electrolytic polishing (25% HCI0, in alcohol, 20V ~ 30°C) and ‘observed in a CM120 FEI microscope. The accumulated strain (e) was assessed by Vickers hardness ‘measurements and the tensile behaviour after deformation was evaluated by tensile tests performed in an INSTRON universal testing machine on miniature samples with a gauge length of 7 mm and 3 x 2.mm? cross section, Elongation was monitored by an optical extensometer, The tests were performed at room tem- perature at a nominal srain rate of 1 107? s', Finally, in order to evaluate the deep drawing capability of the ECAP-processed samples. Erichsen tests following ASTM E643 were performed on 2 mam thick plates cut by spark evosion. 3. Results AAs shown in fig. 1a, the AR material contains some dispersoids, (volume fraction~0.03), originated from segregation during the CASTER process. The plate centre grains are elongated in the rolling disection (see Fig. 1b) and exhibit an average hardness ‘equal to 39 HV. ‘The average hardness and the yield strength measured on the rolled, ECAP and ECAP plus rolled samples are summarized in Table 1. For calculating the total equivalent strain, the hardness of the AR material was intespolated in between the hardness values of the annealed and rolled materials, which gave an approximate value for the accumulated strain of 0.85, This figure was added to the calculated values for equivalent deformation given for rolling156 (MW Wego eal Materials Science & Bngeerng A 45 2015) 154-162 Fig. 1. Fae cents in the AR condiin: a) dspetsld dstsbuton,(b) pole image showing elongated grains Tablet Hardbess, led strength, elongation and equiaent sain Deformation Sample Hardness Yield Total lon- Equivalent process (HY) strength gation (x) stain ea) neal Ametee ASD Reling = OSG SS telling EX 2 EAXR 2 and ECAP deformations, respectively [26] a= trl Bl eB ty @ ‘where hy and hy ate the inital and final plate thickness in rolling and, after the Iwahashi equation 27) (+ s}erom(5+5)) a ‘where N is the number of passes, @is the angle of the channels intersection and y is the curvature angle at said intersection Fig, 2 shows that the microstructures of samples, having. ‘otherwise similar strain level and yield stress but differently pro- ‘essed, viz. by ECAP or by rolling, ae radically diferent. A lamellar structure characterizes the latter samples (Fig. 2c and d), revealing that the thickness reduction was accommodated by boundary sliding, whereas in the ECAP samples the deformation takes place within shear bands, se Fig. 2a, “Table 2 summarizes all ideal texture components produced by ECAP processing and rolling deformation, when applied to fec systems. The sample reference system is parallel to the rolling, normal and transverse directions. Triclinie symmetry was con sidered for the Orientation Distribution Function (ODF) calcula tion, since the ECAP process destroys the orthorhombic sample symmetry usually assumed for the conventional rolling process, ODF maps for g» sections at 0° and 45°, 0°<$<90° and (0° =; < 360° are shown in Fig 3. The as-rolled material exhibits ‘ahat rolled texture with a mixture of Cube (100) < 001 = Copper (12}<1t>, Goss (110) <001> and Brass (110)'= 112> orientations, ‘The texture of the ECAP samples was characterized by low in- tensities for samples E4X and EBX and by a reorientation cowards a shear-fibre < 111 >/[ND and a fibre going trom Rotated Cube {001} <110> to rotated Goss (O11) <011 >. These two orienta- tions exhibit the higher intensities and Fig. 4 shows how this feature changes with the ECAP number of passes, For all rolled samples, independently of their initial condition, texture was ‘characterized by rolling orientations and a tendency to increase the Copper component and reduce Brass and Goss components When prior ECAP deformation is present, as shown in Fig. 5. ‘The spatial distribution of HAGB and LAGB obrained by EBSD, plus the TEM images of the ECAP samples are shown in Fig. 6, Dark areas in the EBSD maps correspond to intermetallic dispersoids. At an equivalent strain of 3.3 (Fig. Sb and d) grains are divided in shear regions having a low angle character and dislocation cells further subdivide these regions. Normally, in Al the amount of dislocation inside the dislocation cells is very low, due to the high SFE, LAGB are progressively rotated into HAGB by the shear pro- cess, and Fig. Ge and e shows that after €¢,=5.8, more than hall (65x) of the boundaries are of the latter type, The structure is 1a- ‘mellar and oriented in the shear direction. From TEM images the average subgrain size was estimated as equal to 15 um, see Fig. 7. ‘The spatial distribution of HAGB and LAGB in rolled and ECAP rolled samples is shown in Fig 8. The spatial arrangement of the former type of boundaries was also lamellar with most of the lamellae oriented along the rolling direction Comparing ECAP samples with rolled samples. see Fig. 9. the amount of HAGBS in the former was always higher (60-65% against ~50%), regardless the equivalent strain, ‘The results of the Erichsen tests, that is, load versus penetration epth achieved before rupture, are shown in Fig. 10. There is an increase in the elastic strain range due to the increase in yield strength promoted by the plastic deformation and an initial de- crease in ductility, which is evident for samples E1X, OXR and EIXR. However, as the accumulated strain increases and the re- covery process advances, the ductility also increases, In Table 1 ‘this was perceived as a slightly increment in the total elongation values. In the Erichsen test, samples F4X and EBX exhibited higher strength while their penetration depths are ofthe same order than ‘the annealed sample, which benefits the deep drawing operation, 4. Discussion It is common knowledge that yield strength and hardness are properties connected with the dislocation density and grain size; thus it would be possible to fit these mechanical properties to @