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Table of contents
1. Effect of strain path change on recrystallisation in copper........................................................................... 1

Bibliography...................................................................................................................................................... 14

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Effect of strain path change on recrystallisation in copper

Author: McDonald, D T; Bate, P S; Hutchinson, W B ProQuest document link Abstract: The effect of different modes of deformation on the subsequent recrystallisation kinetics of copper has been studied. Combinations of uniaxial tension, uniaxial compression and plane strain compression were used to give linear, reversed, and orthogonal strain paths. The rate of recrystallisation, determined using hardness tests and isochronal annealing, did not correlate with any simple strain measure. Correlation with final flow stress was moderate, and was slightly better with as deformed hardness. Deviations from such simple relationships were due partly to an overall effect of strain state, although the largest differences were associated with transient behaviour at small second stage deformations. [PUBLICATION ABSTRACT] Full text: Headnote The effect of different modes of deformation on the subsequent recrystallisation kinetics of copper has been studied. Combinations of uniaxial tension, uniaxial compression and plane strain compression were used to give linear, reversed, and orthogonal strain paths. The rate of recrystallisation, determined using hardness tests and isochronal annealing, did not correlate with any simple strain measure. Correlation with final flow stress was moderate, and was slightly better with as deformed hardness. Deviations from such simple relationships were due partly to an overall effect of strain state, although the largest differences were associated with transient behaviour at small second stage deformations. Keywords: Recrystallisation kinetics, Copper, Tension, Compression, Deformation Introduction The vast majority of investigations into the behaviour of metals during deformation as well as during subsequent annealing have been concerned with linear, or proportional, straining such as simple tension or plane strain compression, e.g. near the midplane in flat rolling. However, for very many practical circumstances the strain paths are far from linear and this can have a major influence on how the metal responds. For example, the strain history during sheet forming affects radically the extent of ductility. It is also an established fact that the kinetics of recrystallisation on annealing and the recrystallised microstructure depend to a large degree on the prior deformation history. In recent years it has become recognised that a better appreciation of the effects of strain path change are necessary, both for the sake of general understanding, and so that they can be accommodated when modelling the behaviour of metals during processing. In fact, this subject is not so new as generally believed. Czochralski1 reported in 1925 that reversed torsion led to a relative reduction in the rate of recrystallisation and this was followed shortly afterwards by work by Sachs,2 including investigations on single crystals. The effect of reversal on mechanical behaviour, the well known Bauschinger effect, had been recognised even earlier than this. More recently3'4 it has become evident that the evolution of microstructure during hot rolling can be modelled reasonably well near the plate centre, where deformation is continuously in plane strain, but not in the near surface regions where a complex pattern of reversed shearing is superimposed. The overall amount of deformation is usually defined in terms of a total strain. In cases where the ratios of the different components of straining, or formally the strain rate, remain constant (proportional deformation) there is usually a monotonie relationship between simple measures such as recrystallisation rate or recrystallised grain size and the total plastic strain. This is not true when the deformation is more complex. Embury et a!.5 working with aluminium deformed by uniaxial compression with a change in compression axis, showed that recrystallisation kinetics correlated well with the final flow stress but not with the accumulated plastic strain. A similar conclusion was reached by Lindh et al.6 working with uniaxial tension and compression of copper. 24 March 2014 Page 1 of 14 ProQuest

Cowan et al.7 using torsion combined with either reverse torsion or axial compression in aluminium, confirmed the profound influence of reversed straining on recrystallisation kinetics but observed almost no deviant effect of torsion+ compression (orthogonal states). More recently, Zhu and Sellars8 showed similar behaviour of reversed straining using tension+ compression for an Al-2%Mg alloy. Previous investigations of the effect of strain path on recrystallisation have been rather sporadic. The aim of the present work was to vary the deformation history in a more controlled and systematic manner in the hope that general relationships could be found that can be included in process models and which also provide a better insight into this subject area. As described by Hutchinson and Davis,9 a change in strain path can appropriately be described by an angle in strain space which may vary from 0 for proportional straining to 180 for fully reversed straining corresponding to the Bauschinger condition. In the present work, three values of path change were chosen; 0 90, and 180, and these were combined with various levels of prestrain and subsequent strain. Although deformation substructures were not specifically examined here, the phenomena investigated are intimately connected to mechanisms of substructure evolution and work hardening that remain significant challenges in physical metallurgy.

Experimental Material The material was hot rolled copper plate approximately 11-4 mm thick manufactured by Outokumpu Oy. It contained 0-025 wt-%P, 0-008 wt-%Ag, and no other significant alloying. This was machined to 10 mm thickness to remove the rolled surfaces. The material was in a recrystallised condition with fairly large equiaxed grains. The mean linear intercept grain size was about 60 m, not including the significant fraction of coherent twin boundaries. The main characteristic of the crystallographic texture, determined from X-ray diffraction data, was that it was very weak. Although it comprised a mix of cube, {001}<100> and the fibre orientations characteristic of the rolling texture of FCC metals, the maximum orientation density was only 1.8 random, and the texture index J was 1.08. Mechanical behaviour Three modes of deformation were used; uniaxial tension, uniaxial compression, and plane strain compression. All tests were carried out using Instron twin screw machines. The tensile specimens had a 12 mm wide parallel section, and were 200 mm long, with the tensile axis along the plate rolling direction. They were deformed at a constant cross-head speed of 0.17 mm s^sup -1^, with a clip gauge extensometer to determine strain during the test. Strain uniformity was determined from 20 mm gauges marked on the parallel section using light scratch marks through a thin layer of black ink. These were measured before and after testing with a travelling microscope. The first specimen was extended to slightly beyond the maximum load, giving a tensile strain of 0.33, and two other specimens were then taken to strains of 0.11 and 0.22. The specimen subjected to the highest strain developed a neck and subsequent tests on material from 24 March 2014 Page 2 of 14 ProQuest

that specimen generally used material with strains close to the extensometer value. For this purpose the large gauge length was invaluable. In specimens stretched to lower strains, the gauge section remained reasonably uniform. Samples for uniaxial compression were taken from tensile specimens such that the compression and tension axes were parallel. An unstrained tensile specimen was used as a precursor, for the sake of uniformity, for these tests and also for plane strain compression. The initial height of the compression pieces was about 11 mm and these were compressed between flat tool steel platens at a rate of 8 10^sup -3^ mm s^sup -1^ using 0-05 mm PTFE film and oil as lubricants. The compliance measured on unloading was used to correct the loaddisplacement data. Stress versus plastic strain results for the uniaxial compression tests are shown in Fig. 1. The prestrained material gave lower stresses than the virgin material for the same accumulated absolute strain, and also showed a characteristic transient behaviour, with a significant amount of 'permanent softening' developing as the reverse deformation increased. Plane strain compression (PSC) used a tool steel channel die, with a channel width of 8 mm. The constrained direction corresponded with the tensile axis and the compression direction with the width direction of the tensile specimens (the transverse direction in the plane of the plate). Extension was accordingly along the thickness direction of the tensile specimen (and plate). As in the case of uniaxial compression, specimens were compressed at a constant rate of 8 10^sup -3^ mm s^sup -1^, with oiled PTFE film as lubricant. It is not reasonable to use directly tensile prestrain offsets to show the effect of prior tensile deformation on the plane strain compression behaviour. According to the von Mises approximation, the tensile strain should be multiplied by a factor of 0-8663 to give the equivalent offset strain. The Taylor model, assuming a random texture and isotropic hardening predicates a factor of about 0-9225. For this part of the analysis an empirical approach has been adopted. The stress-strain results for tension and for uniaxial compression and plane strain compression without prestraining are compared in Fig. 2. The curves for uniaxial deformation in tension compression are very similar and good coincidence with these is achieved by using a factor of 0.89 to multiply the stress and divide the strain for the channel die tests. Applying the same multiplier for the prestrain offsets, the plane strain compression results are shown in Fig. 3. After a small initial transient, the flow stress of prestrained material evolves in much the same way as the virgin material. There is little indication of latent hardening or significant changes in strain hardening behaviour.

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Measurements of cross-section after deformation revealed that the width and thickness strains in uniaxial tests were approximately equal, i.e. the r value was close to unity. Because of transverse compliance in the channel die, there was some expansion in the nominally zero strain direction, though this was relatively small. These features are shown in Fig. 4, where the final strains (i.e. true plastic strains corresponding to the total shape changes of the specimens) for all the tests are plotted in a space of total deviatoric strain ( plane).

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The nominal values of strain are summarised for all specimens in Table 1. In this table, the strain values from tests involving PSC are evaluated in terms of von Mises equivalent strains. Recrystallisation

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Isochronal annealing treatments were used. Specimens, with a volume of about 30 mm^sup 3^, were placed inside an air circulating furnace on a 10^sup 4^ mm^sup 3^ copper block that had been preheated to the required temperature. The annealing time was 1 h (3600 s). Reasonable estimates of repeatability and measurement accuracy were 2C for temperature, measured using a thermocouple in the copper block, and <0.1% for time. The specimens to be annealed were cut from the deformed material using a diamond saw and were pickled to remove about 0-5 mm from each dimension prior to annealing. The hardness indentations were made on the rolling plane.

An example of the effect of annealing on hardness and the JMAK curve fits is shown in fig. 5. These curves are from material deformed only in tension, but are quite representative of the whole set of annealing results. Scatter in the hardness results tends to be greatest when the material is partially recrystallised. In that condition, 24 March 2014 Page 6 of 14 ProQuest

even relatively minor spatial inhomogeneities tend to have an effect because of the large hardness difference between recrystallised and unrecrystallised volumes. The fitting was considered sufficiently good to allow the derived values to be used in assessing the correlation between prior deformation and recrystallisation behaviour. Deformation and recrystallisation

Here the correlation is significantly better than with accumulated strain, but there are deviations from a simple relationship between the final flow stress and recrystallisation kinetics. It is interesting to note that slightly better correlation can be achieved by using the as deformed hardness, rather than the final flow stress, as the determining parameter, as can be seen in Fig. 8.

Discussion It is apparent that neither strain nor stress can be relied on as a simple measure for recrystallisation tendency following complex deformation paths. Nevertheless, there are reasons to pursue further both approaches. Stress is a state function and so may provide a key towards understanding the physical principles that are 24 March 2014 Page 7 of 14 ProQuest

involved here, whereas strain does not possess this characteristic. On the other hand, the stress in a material is not normally known at different stages during its processing, whereas the strain history is generally available. Therefore, from the viewpoint of modelling, a criterion based on strain is to be preferred. Before discussing the correlations between recrystallisation and parameters describing the deformed state, it is relevant to make some comments on the mechanical behaviour in these tests. A significant amount of published research shows that strain reversal generally leads to a regime of reduced flow stress and high strain hardening followed by a regime with reduced flow stress - 'permanent softening'- when compared with continued forward deformation. These are the characteristics of the Bauschinger effect where the initial transient regime is due to the effect of internal stresses in the mechanically inhomogeneous deformation microstructure, and the 'permanent softening' to the partial removal, or dissolution, of that deformation microstructure.11'12 A different type of behaviour is usually observed when the strain paths are not reversed but are more nearly orthogonal in strain space ( ~ 90). Typically, the flow stress rises rapidly to a value higher than that for continued proportional deformation and there then follows a regime in which the strain hardening is lower than for continued proportional deformation. Eventually, the flow stress evolution becomes similar to that of continued proportional deformation. These effects can also be rationalised in terms of changes in the deformation microstructure.13'14

The mechanical behaviour observed here was different. The characteristic orthogonal strain path effect was not observed in the tension PSC tests, where the flow stress in the second stage quickly became similar to that in proportional PSC. Upon strain reversal, there was a small initial Bauschinger effect but this was followed by an increasing level of'permanent softening', leading to a regime in which there was relatively reduced strain hardening more akin to the behaviour after an orthogonal strain path change. Such behaviour has been reported for reverse simple shear of aluminium,15 and assumed to be due to the dissolution of dislocation substructure. The majority of work on the orthogonal strain path effect has used ferritic steel and aluminium. In both those cases, dynamic recovery leads to the formation of a well defined dislocation cell substructure, with relatively condensed high dislocation density cell walls and cell interiors having a low dislocation density. If dynamic recovery is hindered by a lower stacking fault energy or solute, then a more uniform distribution of dislocations occurs. This has a quite significant effect on the orthogonal strain path change effect, which then becomes much less marked. The relatively low stacking fault energy of copper, as compared to aluminium or iron, is known to inhibit dislocation recovery processes involving cross-slip or climb. In fact, the present observations are in quite reasonable agreement with earlier results,16 which compared steel, aluminium, copper, and brass with strain path changes of 120. In addition to the effects of strain path changes on recrystallisation, there is also reason to consider what may be the influence of the strain state itself, for example after proportional loading to the same (equivalent) level. To the authors' knowledge this has not been investigated in any systematic way and, if so, represents a significant omission in the literature. The present results in Fig. 6 suggest that recrystallisation kinetics are comparable for 24 March 2014 Page 8 of 14 ProQuest

the different strain states up to equivalent strains of around 0-2 but that after higher strains, recrystallisation occurs more rapidly - at lower temperature - following simple tension than after uniaxial compression or PSC. One can speculate that this may be related to evolution of different textures or to different tendencies for grain fragmentation by deformation banding. Alternatively, the geometries of grain boundary networks, especially at triple junctions where nucleation of recrystallisation frequently takes place, may vary with the imposed strain state. In any event, such an effect is a complicating factor when attempting to clarify the role of strain path changes. Correlation of the recrystallisation kinetics - as the T^sub 0.5^ parameter - with as deformed hardness was somewhat better than with final flow stress. It may be significant that the recrystallisation kinetics were determined from hardness measurements, and so there is an increased likelihood of consistency, but this only shifts the argument to why there is poor correlation between hardness and final flow stress. The possibility that the orientation of hardness testing could be making a difference, as a result of strain induced anisotropy, was discounted after finding that the hardness measured on different faces of several specimens only varied within 1%. Hardness measurements involve additional straining, and this is a significant factor because the greatest deviations from a fairly simple relationship between recrystallisation kinetics and final flow stress - for uniaxial compression - occur when deformation ended in the transient regime prior to the full development of 'permanent softening'. This is shown in Fig. 9. There is good correlation between T^sub 0.5^ and final flow stress for all but three uniaxial compression tests; those three have low second stage strains and therefore terminate in the transient region of the stress-strain curves. The hardness will sample the stress at higher strains, including the regime of reduced strain hardening, and so the influence of the transient will be reduced. It appears that the results progressively deviate from the results for uniaxial tension as the strain increases, indicating that there exists a contribution of strain state per se in addition to that caused by the change in strain path, as noted above.

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There are several possible reasons why recrystallisation is less rapid following non-linear straining than proportional straining. Calorimetric measurements have shown that the stored energy is actually reduced for certain stages of reversed loading17 due to a reduction in the dislocation density or possibly their rearrangement into lower energy configurations. Such an energy reduction will lower the driving force for both nucleation and growth of new grains on annealing. Relaxation of piled-up dislocations could also remove lattice curvatures that are necessary for nucleation by polygonisation processes. This reduction of lattice curvature could occur during the early stages of compression following tension, i.e. during the transient stage prior to the establishment of permanent softening, and could account for the mismatch between the flow stress and recrystallisation behaviour in specimens with small compressive reverse strains. Hardness tests also involve a variety of straining states and, for this reason, may be a better indicator than flow stress regarding the propensity of prestrained material for recrystallisation.

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Another possible influence is the effect on the geometry of the pre-existing grain boundary network. The specific area of grain boundary after deformation becomes greater in compression than in tension but the difference is very small for low strains18 and cannot be expected to have any measurable influence in the present case. However, the nearly equilibrium grain boundary network is perturbed by deformation and this will tend to reassert itself by local boundary migration, especially at triple junctions, which can lead to formation of strain free nuclei along triple junctions as shown, for example, by Vandermeer and Gordon.19 It has been shown20 that reversed straining can result in an almost perfect reestablishment of the initial grain structure even though an internal substructure remains. For this reason, nucleation at prior grain boundaries is likely to become less prolific after non-linear straining and, accordingly, the final recrystallised grain size should become larger, consistent with previous reports.6 8 Another difference between tension and compression is the effect on grain orientations, i.e. the deformation texture. Compression of FCC tends to give a single [left angle bracket]011[right angle bracket] parallel to the compression axis, whereas tension gives both [left angle bracket]001[right angle bracket] and [left angle bracket]111[right angle bracket] along the tensile axis.21 The generation of two components in tension - and some more high angle boundaries - would superficially suggest that tension would favour recrystallisation, which is clearly not the case. There may also be a difference in strain uniformity between tension and compression, associated with the development of different textures. However, calculations using crystal plasticity finite element modelling indicate that there is little difference in the overall degree of strain heterogeneity between compression and tension - at least up to a strain of 0.4. Perhaps more significant is the occurrence of intragranular deformation banding by subdivision of the crystals which is expected to be much more prominent in tension than in compression. Recrystallisation associated with deformation band structures is well known and this could contribute to the faster recrystallisation kinetics after tensile deformation. Conclusions The recrystallisation of copper following deformation to low overall strains is highly dependant on the strain path involved. There is very poor correlation between recrystallisation temperature and strain, either path integrated 24 March 2014 Page 11 of 14 ProQuest

or based on the overall shape change. A linear combination of those two can give a somewhat better prediction of recrystallisation temperature, but it is still rather poor. Although better than total strain, final flow stress does not give adequate correlation, although as deformed hardness is a somewhat better measure. There are two main reasons for this. The final stress state has an effect, such that strain in compression gives a lower recrystallisation temperature than the same strain in tension. The causes of that asymmetry are not known. The second reason is that small reverse strains give a regime where the permanent softening component of the Bauschinger effect is not developed. It is expected that this will lead to a disparity between directional and nondirectional aspects of the dislocation content. Hardness testing not only samples flow stress in a variety of states, it also introduces significant additional plastic strain which takes the material out of that low strain regime. References References 1. J. Czochralski: Z. Melallkd., 1925, 17, 1-11. 2. G. Sachs: Zeil. Metallk., 1926, 18, 209-212. 3. A. J. McLaren, N. Le Mat, J. H. Beynon and C. M. Sellars: Ironmaking Steelmaking, 1995, 22, 71-73. 4. M. P. Black, R. L. Higginson and C. M. Sellars: Mater. Sc/. Technol., 2001, 17, 1055-1060. 5. J. D. Embury, W. J. Poole and E. Kokcn: Scr. MeIaII. Mater., 1992, 27, 1465-1470. 6. E. Lindh, B. Hutchinson and S. Ueyama: Scr. Metal/. Mater.. 1993, 29, 347-352. 7. J. R. Cowan, R. L. Higginson, W. B. Hutchinson and P. S. Bate: Mater. Sd. Technol., 1995, 11, 1104-1109. 8. Q. Zhu and C. M. Sellars: 'Conference on thermo-mechanical processing in theory, modelling and practise ([TMP]2)', Swedish Society for Materials Technology, 193-200; 1997, Metals Park, OH, ASM. 9. W. B. Hutchison and T. Davis: in 'Proc. 4th Int. Conf. on mechanical behaviour of materials' (ed. J. Carlsson and N. G. Ohlson), 1227-1236; 1983, Oxford, Pergamon. 10. R. Ray: PhD dissertation, University of Birmingham, UK, 1973. 11. P. S. Bate and D. V. Wilson: Acta Metal/., 1986, 34, 1097-1105. 12. T. Hasegawa, T. Yakou and U. F. Kocks: Mater. Sd. Eng., 1986, 81, 189-199. 13. D. V. Wilson and P. S. Bate: Acta Mater., 1996, 44, 3371-3383. 14. B. Peelers, S. R. Kalidindi, P. Van Houtte and E. Aernoudt: Acta Mater., 2000, 48, 2123-2133. 15. E. F. Rauch, J. J. Gracio, F. Barlat, A. B. Lopes and J. Ferreira Duarte: Scr. Mater., 2002, 46, 881-886. 16. W. B. Hutchinson, R. Arthey and P. Malmstrom: Scr. Metal/., 1976, 10, 673-675. 17. A. S. Iyer and P. Gordon: Trans. Met. Soc. AIME, 1959, 215, 729-730. 18. P. S. Bate and W. B Hutchinson: Scr. Mater., 2005, 52, 199-203. 19. R. A. Vandermeer and P. Gordon: in 'Recovery and recrystallisation of metals', (ed. L. Himmel), 211-239; 1962, New York, Interscience Publishers. 20. M. M. Farag, C. M. Sellars and W. McG. Tegard: in 'Deformation under hot working conditions' (ed. P. Moore), 60-67; 1968, London, Iron and Steel Institute. 21. CS. Barrett and T. B. Massalski: 'Structure of metals', 543-549; 1966, New York, McGraw-Hill. 22. H. Ahlborn: Zeit Metallk., 1965, 56. 411-420. AuthorAffiliation D. T. McDonald1, P. S. Bate*1 and W. B. Hutchinson2 AuthorAffiliation 1 Manchester Materials Science Centre, The University of Manchester, Manchester M1 7HS, UK 2 Swedish Institute for Metals Research, Drottning Kristinas vg 48, S-11428 Stockholm, Sweden * Correponding author, email pete.bate@man.ac.uk Subject: Deformation; Recrystallization; Copper; Strain; Hardness testing; Correlation analysis;

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Publication title: Materials Science and Technology Volume: 21 Issue: 6 Pages: 693-700 Number of pages: 8 Publication year: 2005 Publication date: Jun 2005 Year: 2005 Publisher: Maney Publishing Place of publication: London Country of publication: United Kingdom Publication subject: Metallurgy ISSN: 02670836 CODEN: MSCTEP Source type: Scholarly Journals Language of publication: English Document type: Feature Document feature: Graphs Tables Equations References ProQuest document ID: 201117478 Document URL: http://search.proquest.com/docview/201117478?accountid=46437 Copyright: Copyright Institute of Materials Jun 2005 Last updated: 2012-02-07 Database: ProQuest Science Journals

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Bibliography
Citation style: APA 6th - American Psychological Association, 6th Edition D, T. M., P, S. B., & W, B. H. (2005). Effect of strain path change on recrystallisation in copper. Materials Science and Technology, 21(6), 693-700. Retrieved from http://search.proquest.com/docview/201117478?accountid=46437

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