Vol. 128 (2015) ACTA PHYSICA POLONICA A No. 4

Proceedings of the International Symposium on Physics of Materials (ISPMA13)

Dislocation Substructure Evolution

during Hydrostatic Extrusion of Al�Mg�Si Alloy

W. Chrominski*and M. Lewandowska

Warsaw University of Technology, Faculty of Materials Science and Engineering,

Woªoska 141, 02-507 Warsaw, Poland

Hydrostatic extrusion is a technique which allows to produce rods with ultra�ne grains and unexpectedlyenhanced mechanical properties caused by grain re�nement. However, the mechanism of such a re�nement is notfully understood at this stage. 6xxx aluminium alloys series are usually processed by extrusion. In this study,commercial 6082 aluminium alloy was extruded at ambient temperature in a cooled die in two stages to the truestrain of ε = 3.2. Such a processing results in a not fully re�ned microstructure which allows to study di�erent stagesof grain re�nement. The texture, dislocation substructures and grain re�nement were investigated using electronbackscatter di�raction and transmission electron microscopy techniques. The results revealed that two main texturecomponents are present in the extruded rods � 〈111〉 �ber texture and 〈001〉 recrystallized grains. Transmissionelectron microscopy inspection revealed dislocation structures that can be associated with di�erent stages of plasticdeformation according to the low energy dislocation structures hypothesis proposed by Kuhlmann-Wilsdorf.

DOI: 10.12693/APhysPolA.128.585

PACS: 81.05.Bx, 61.72.Ff, 81.20.Hy, 81.40.Ef, 81.40.Lm

1. Introduction

Plastic deformation of metals usually results in a sub-stantial increase in dislocation density which arrangethemselves into di�erent structures, in particular low en-ergy ones. The structure formed depends primarily onthe imposed strain, crystal lattice and stacking fault en-ergy (SFE). In the case of Al (high SFE), the size ofdislocation cells decreases with increasing strain [1, 2].At su�ciently high strain, they rotate around a commonaxis and form new high angle boundaries [3, 4] which alsoresults in a sharp texture [5�8]. As a consequence of sucha structural evolution, the grain can decrease below 1 µm.

Ultra�ne grained (UFG) materials are attracting agrowing attention due to their superb mechanical prop-erties [5, 9�15]. This recognition resulted in the develop-ment of their fabrication methods, in particular severeplastic deformation (SPD) techniques, in which grainre�nement occurs as a consequence of extremely highstrains [5]. However, it should be noted that grain sizereduction to UFG regime in metals can also be achievedby means of conventional deformation techniques, suchas rolling [16]. The microstructure evolution as a func-tion of imposed strain was well described for rolling [17]and equal channel angular pressing (ECAP) [4]. The aimof this work is to discuss microstructural evolution dur-ing hydrostatic extrusion (HE) which has been alreadyproven to be an e�cient method of grain size re�ne-ment in a number of metals and alloys, including techni-cally pure aluminium [15, 19]. It has been shown previ-ously that for technically pure aluminium, a true strain

*corresponding author; e-mail: wichr@inmat.pw.edu.pl

of ε = 2.77 is su�cient to obtain re�ned microstruc-ture [19]. However, it should be noted here that puremetals are susceptible to recrystallize dynamically dur-ing plastic deformation.

2. Material and methods

A commercial 6082 Al�Mg�Si alloy was used in thisstudy. The material was supplied in a rod form with a di-ameter of 50 mm in T6 hardened condition. The sampleswere solution annealed at 520 ◦C for 2 h and quenchedinto water in order to obtain supersaturated solid solu-tion. Such a condition allows cold plastic deformation.HE was performed at ambient temperature. The un-wanted warming of the specimen was reduced by a cool-ing system. Two stage extrusion resulted in an accumu-lative strain of ε = 1.8 after �rst pass and ε = 3.2 afterthe second. The �nal product was in a form of a rodhaving 10 mm in diameter.Samples for electron backscattered di�raction (EBSD)

and transmission electron microscopy (TEM) inspectionwere in the form of thin discs of cross-sections taken fromthe center of the extruded rod with spark erosion machineand wire saw. Surface of the specimens for EBSD analysiswas prepared electrochemically with �nal ion polishing.Electron transparent regions for TEM observations wereobtained by electrochemical thinning.EBSD measurements were performed on a Hi-

tachi SU70 scanning electron microscope (operation volt-age of 20 kV) with the Schottky emitter. The datafor texture analysis were taken with 0.5 µm step whichresulted in orientation maps with dimensions of 100 ×100 µm2. Results were used to built inverse pole �g-ures and calculate volume fraction of each of the texturecomponent as a ratio of the area related to a particu-lar orientation to the whole examined region. 0.5 µm

(585)

586 W. Chrominski, M. Lewandowska

step is too coarse for providing a detailed microstructureanalysis of severely deformed aluminum so discussion oforientation maps is omitted in this study.TEM observations were performed on JEOL JEM1200

EX II microscope with accelerating voltage of 120 kVand high double tilt range for setting desired di�rac-tion conditions. TEM investigations were focused on thedislocation structure dependence on the grain orienta-tion relatively to extrusion direction. General observa-tions were performed with bright �eld mode. Disloca-tion structures were investigated in terms of number ofdi�erent Burgers vectors b (determined with invisibilitycriterion g · b = 0) participated in a speci�c dislocationwall. Images of dislocation structures were recorded us-ing g − 3g weak beam dark �eld imaging condition withslightly positive deviation parameter s for sharp imagesof dislocation lines.

3. Results and discussion

The �rst HE pass of supersaturated 6082 aluminiumalloy results in sharp double texture with 〈001〉 and〈111〉 components parallel to extrusion direction (Fig. 1).The texture components fractions equals to 22% and 78%for 〈001〉 and 〈111〉, respectively. After the second pass,the fraction of 〈001〉 component did not change signi�-cantly.

Fig. 1. Inverse pole �gure taken from 6082 aluminiumalloy hydrostatically extruded to the true strain of ε =1.8 shows sharp double texture.

According to literature, deformation substructurestrongly depends on orientation [20], i.e. in 〈111〉 grainsdense dislocations walls form whereas in 〈001〉 grains sta-ble cell dislocation structure exists. This implies signi�-cant di�erences in di�erently oriented grains in HE pro-cessed sample. To provide a better insight into structuralvarieties, TEM study was performed.A bright �eld image of dislocations con�guration in

grain with 〈001〉 parallel to extrusion direction (orienta-tion con�rmed with di�raction pattern presented as in-set) after the �rst HE pass is presented in Fig. 2a. Onecan see dislocation tangles which can be considered asearly stages of dislocation cell structure formation. Oneshould also note di�erences in di�raction contrast be-tween the cells` interior and the regions with dislocations

Fig. 2. Images of dislocation structure in grains with〈001〉 parallel to extrusion direction in 6082 aluminiumalloy, ε = 1.8: (a) bright �eld image showing disloca-tion arrangement typical for early stages of plastic de-formation (b) weak beam dark �eld image with exciteddi�raction vector g = [020].

tangles at the bottom of image. The former are charac-terized with relatively uniform contrast (see area in thecenter of Fig. 2a), while the latter features signi�cantchanges in contrast (bottom of Fig. 2a). Cells, whichare visible in Fig. 2b, are the very early stage of lowenergy dislocation structure (LEDS) formation by dis-locations with di�erent Burgers vectors (con�rmed bydi�raction contrast experiment). The basic feature ofLEDS is that the range of the stress �eld does not ex-ceed the wall due to the superposition of stress �eldsarising from dislocation cores with di�erent Burgers vec-tors [1, 2]. The dislocation structure visible on the bot-tom of Fig. 2a is not ordered in energy lowering structuresalthough it also contains dislocations with di�erent Burg-ers vectors. As a result the local �uctuations of the Braggdi�raction condition di�raction contrast inhomogeneitiescan be observed.

Fig. 3. Images of dislocation structure in with 〈001〉parallel to extrusion direction in 6082 aluminium ε = 3.2(a) bright �eld image showing dense dislocation walls(b) weak beam dark �eld image with excited di�rac-tion vector g = [020] of dislocation subgrain with singleBurgers vector dislocations arrangement inside.

Further plastic deformation, to a true strain of 3.2,brings about the evolution of dislocation cells which be-come more developed as presented in Fig. 3a. Meanequivalent diameter of such cells is 360 nm. Besides welldeveloped LEDS, some dislocations can be noticed withincells as presented in Fig. 3b. Tilting to excite di�erentdi�raction vectors g showed that invisibility criterion was

Dislocation Substructure Evolution. . . 587

satis�ed for g = [2−20] which means that they are asingle b = [−110] structure which according to LEDShypothesis is not stable.

The formation of such a microstructure can be eluci-dated as follows. Plastic deformation results in the gen-eration of dislocations which rearrange themselves intoLEDS, which are known to be stable. One of the exam-ples of LEDS are dislocation cells which separate graindomains in which di�erent slip systems operate. Ac-cording to the model of structure development in heavilyworked materials dislocation cells can accommodate plas-tic deformation until they reach critical dimensions in the�fth stage of work hardening [21]. In our case, the accu-mulated deformation is relatively low and one can con-clude that the dislocation cells presented in Fig. 3 canstill accommodate plastic deformation and evolve into�ner ones.

Fig. 4. Images of dislocation structure in �ber grainswith 〈111〉 parallel to extrusion direction in 6082 alu-minium alloy ε = 1.8 (a) bright �eld image of 〈111〉 ori-ented region, note non-homogenous amplitude contrast(b) weak beam dark �eld image of dislocation structurewithin considered region.

The regions with 〈111〉 parallel to extrusion directiondi�er signi�cantly from 〈001〉 ones discussed previously.Figure 4a presents a typical view of such a region. Firstcharacteristic feature is heterogeneous amplitude con-trast within the observed area which made it di�cult todetermine any microstructure element with bright �eldimaging. Weak beam image of the same area presentedin Fig. 4b reveals dislocation walls and some individualdislocations between them. Contrast on the left side ofthe image becomes weaker in comparison to the rightside because of the residual stresses that cause bend-ing of the lattice planes. Weak beam imaging is verysensitive to the deviation parameter s that strongly de-pends on di�raction conditions. Even small de�ectionfrom perfect imaging conditions results in contrast weak-ening. For comparison, Fig. 2b shows the area with thesame magnitude. The contrast is uniform on whole im-age because of no residual stresses are present in thisregion. This observation implies that observed struc-tures in 〈111〉 grains are not LEDS. During di�ractioncontrast experiment dislocation invisibility criterion wassatis�ed for all dislocations within cell when g = [202].Furthermore, microstructure in 〈111〉 oriented grains ismuch more developed than in 〈001〉 grains (at strain level

of ε = 1.8) as the former possess relatively well devel-oped cell structure with an average size of about 300 nm,whereas in the latter cells are only about to being formed.Figure 5 shows well developed, �ne grains with 〈111〉

parallel to extrusion direction typical for the sample de-formed to larger strain. Di�raction pattern presented asan inset in the �gure is a ring related with (220) planeswhich are inB = [111] zone axis. The mean size of grainsequals to 240 nm and it is slightly smaller than thosemeasured for dislocation cells in the previous HE stagein similarly oriented region. This indicates that cells sizeshrinks together with progression of plastic deformationbefore rotations. As it was already mentioned above, thedi�raction pattern is now a ring which con�rms incre-ment of misorientation angles between cells which trans-form into well developed grains as can be seen in Fig. 5.This microstructure type is the most advanced stage ofgrains development found in the investigated material.

Fig. 5. Image of microstructures in �ber grains with〈111〉 parallel to extrusion direction in 6082 aluminiumalloy ε = 3.2.

4. Conclusions

Hydrostatic extrusion of a single phase (supersatu-rated solid solution) 6082 aluminium alloy results in dou-ble �ber textured grains with various dislocation sub-structures. 〈001〉 oriented grains contain stable cellularstructure which evolves as plastic deformation continues.〈111〉 grains show more advanced structures which re-sult in re�ned, well developed grains separated with highangle grain boundaries.

Acknowledgments

This work was carried out within a NANOMETProject �nanced under the European Funds for RegionalDevelopment (Contract no. POIG.01.03.01-00-015/08).

588 W. Chrominski, M. Lewandowska

Authors would like to thank Dr. W. Pachla andDr. M. Kulczyk from Institute of High Pressure Physicsof the Polish Academy of Sciences for performing hydro-static extrusion experiment.

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