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J Mater Sci (2012) 47:7719–7725

DOI 10.1007/s10853-012-6507-y

ULTRAFINE GRAINED MATERIALS

Twenty-five years of severe plastic deformation: recent


developments in evaluating the degree of homogeneity through
the thickness of disks processed by high-pressure torsion
Megumi Kawasaki • Roberto B. Figueiredo •

Terence G. Langdon

Received: 8 March 2012 / Accepted: 13 April 2012 / Published online: 28 April 2012
Ó Springer Science+Business Media, LLC 2012

Abstract The processing of disks by high-pressure tor- Preamble


sion leads to an inhomogeneous distribution in strain with
a high strain around the perimeter of the disk and a zero The symposium on Ultrafine-Grained Materials VII, which
strain in the center. Despite this apparent inhomogeneity, formed part of the TMS 141st Annual Meeting in Orlando,
there are now many experiments showing that the hard- Florida, on March 11–15, 2012, was one of a series of
ness values on the surfaces of disks gradually evolve with symposia organized every 2 years within the TMS annual
increasing strain to give a reasonably high level of meetings. However, this meeting was significant because it
homogeneity. Experiments were conducted to determine marked the twenty-fifth anniversary since the first attempts
whether this high level of homogeneity extends also were undertaken to evaluate the microstructures of mate-
through the thickness of the disks or whether inhomoge- rials processed through the application of severe plastic
neities occur in the axial direction. Results are presented deformation (SPD). As reviewed elsewhere [1, 2], the first
for high-purity aluminum and a magnesium AZ31 alloy as detailed scientific studies of SPD processes, and the first
two representative materials showing different hardness incorporating scientific rigor, were conducted by Bridgman
characteristics. [3, 4] in the 1930s and 1940s with classic experiments on
the procedure now known as high-pressure torsion (HPT).
Later, this was followed by the work of Segal et al. [5] in
the 1980s in the development of the principles of equal-
channel angular pressing (ECAP).
However, these early studies were devoted almost
M. Kawasaki  T. G. Langdon (&) exclusively to the mechanical characteristics associated
Departments of Aerospace & Mechanical Engineering
with the HPT and ECAP processes and it was only later,
and Materials Science, University of Southern California,
Los Angeles, CA 90089-1453, USA with the classic work of Valiev and his co-workers in Ufa,
e-mail: langdon@usc.edu that modern microstructural analysis was used to evaluate
the microstructures of the materials processed by SPD and
M. Kawasaki
to investigate their significance. This study began 25 years
Division of Materials Science and Engineering, Hanyang
University, 17 Haengdang-dong, Seongdong-gu, Seoul 133-791, ago, in 1987, and it led very quickly to an extraordinary
South Korea demonstration of low temperature superplasticity in an
Al–Cu–Zr alloy processed by HPT and having an excep-
R. B. Figueiredo
tionally small grain size of 0.3 lm. The report describing
Department of Materials Engineering and Civil Construction,
Federal University of Minas Gerais, Belo Horizonte, this study was submitted for publication on September 28,
MG 31270-901, Brazil 1987, and the paper appeared in the scientific literature in
1988 [6]. This research, and the subsequent detailed
T. G. Langdon
descriptions of experimental results in western journals
Materials Research Group, Faculty of Engineering
and the Environment, University of Southampton, [7, 8], led to a widespread interest in the processing of metals
Southampton SO17 1BJ, UK using SPD techniques and the subsequent development of

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7720 J Mater Sci (2012) 47:7719–7725

SPD facilities in many laboratories around the world. This Although Eq. (1) implies there will be gross inhomo-
area of research has grown over the last 25 years to the geneities in the microstructures developed across the disks
extent that the Ultrafine-Grained Materials VII symposium in HPT processing, early experiments using microhardness
was easily the largest, in terms of the numbers of submitted testing revealed a gradual evolution with increasing tor-
abstracts, of the many symposia held at the 2012 TMS sional straining towards a reasonable level of homogeneity
annual meeting. It should be noted that new developments throughout the disks [11–13]. It was shown also in these
in this area include recent reports describing the innovation experiments that this evolution occurred more rapidly with
potential of SPD processing and the opportunities for increasing applied pressure, P, and/or increasing the
developing new approaches in SPD technology [9, 10]. numbers of revolutions, N, in the processing operation [11,
It was recognized in the earliest research on SPD that 12]. The general evolution towards a hardness homogene-
the strain imposed on the disks in HPT processing varied ity within the planes of the disks was later confirmed in
from a maximum at the outer edge of the disk to zero strain many experiments [27–39] and the evolution was
at the disk center. This recognition led to several evalua- explained theoretically using strain gradient plasticity
tions of the development of microhardness and micro- modeling [40].
structure across the planes of the HPT disks [11–18] but It follows from Eq. (1) that, although the strain may vary
these measurements were taken exclusively on, or very within the sectional plane of the disk, it remains constant
close to, the disk surfaces and there were no parallel along the axial direction within the thickness of each disk.
investigations to determine the degree of homogeneity that Accordingly, it was only very recently that experiments
occurred within the thicknesses of the disks. Investigations were undertaken to make microstructural and microhard-
into the development of homogeneity or heterogeneity in ness observations in the axial direction perpendicular to the
the axial directions of HPT disks have been undertaken top and bottom surfaces [19–21, 41]. The present investi-
only very recently [19–21] and these investigations, toge- gation was initiated to review the information available to
ther with new experimental results, form the basis for the date and to describe new results that provide a compre-
present report. hensive description of the evolution of homogeneity or
inhomogeneity within the through-thickness direction.
Results for high-purity aluminum are described in the next
Introduction section and data for the magnesium AZ31 alloy are given
in the following section.
Processing by HPT is generally undertaken by placing a
thin disk between massive anvils, applying a high pressure
and then rotating one of the anvils so that the disk is Experimental results for high-purity aluminum
subjected to torsional straining. There have been some
limited attempts to apply HPT processing to larger bulk Experiments were conducted on high-purity (99.99 wt%)
samples, in the form of small cylinders [16, 22, 23], but aluminum and some of the results were published earlier
most investigations of HPT processing involve the use of [19]. The material was in the form of a rod with a diameter of
very thin disks. 10 mm and it was annealed for 1 h at 773 K to give an initial
In processing by HPT, it can be shown that the equiv- grain size of *1 mm. After annealing, the rod was sliced
alent von Mises strain, eeq, imposed on the disk during into disks with thicknesses of *1.2 mm and then polished to
torsional straining is given by a relationship of the form final thicknesses of *0.81 mm. These disks were processed
[24–26]: by HPT at room temperature (RT) under quasi-constrained
2pNr conditions [42–44] using an applied pressure of P = 6.0
eeq ¼ pffiffiffi ð1Þ GPa. The disks were processed for selected numbers of turns
h 3
ranging from 1/4 to 20 revolutions and the values of the
where N is the number of turns of the anvil, and r and h are Vickers microhardness, Hv, were then recorded along the
the radius and height (or thickness) of the disk, respec- diameters of the disks. The measurements were taken at
tively. It follows from Eq. (1) that the strain imposed in incremental distances of 0.3 mm with four individual values
HPT varies with the position on the disk so that it is zero at recorded around each separate point at distances from the
the disk center where r = 0 and it reaches a maximum at selected point of 0.15 mm. These measurements were used
the outer edge. This significant variation in strain suggests to plot the variation of hardness across each disk together
that the microstructures introduced by HPT are probably with the calculated 95 % error bars.
highly inhomogeneous and it is reasonable to anticipate In addition, and in order to provide comprehensive
that they will vary significantly as a function of the radial information on the variations of hardness within the
position within each disk. through-thickness of the disks, three separate disks were

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prepared for each condition of HPT processing. These three Figure 1 shows the hardness values recorded over the
disks were used to take separate hardness measurements on surfaces of the disks in the upper, center, and lower posi-
either the central plane of each disk or on planes within tions for HPT through 1/4 turn in Fig. 1a–c and through 1/2
*200 lm of the upper or top surface and the lower or turn in Fig. 1d–f. The results are presented as color-coded
bottom surface after HPT processing, respectively. In the maps with the colors representing values of Hv in incre-
following descriptions of results, the locations for these mental steps of 5 as given by the color key on the right: in
three sets of measurements are designated upper, center, these maps the parameters X and Y are two arbitrarily
and lower, respectively. selected but mutually perpendicular directions where the
For the disks processed through 1/4 and 1/2 turns, the position (0,0) corresponds to the center of each disk.
hardness values were also recorded over the total planar Inspection of these maps shows that the hardness distri-
sections at the upper, center, and lower positions with butions are very similar at the upper, center, and lower
measurements taken following a rectilinear grid pattern positions after 1/4 and 1/2 turns thereby confirming a
with a separation of 0.3 mm between each separate point. general homogeneity in the through-thickness direction.
These measurements were used to plot color-coded contour Furthermore, the close agreement between each plane
maps that provide a simple visual representation of the demonstrates that the HPT processing was successfully
hardness distributions across the disk surfaces. The conducted without the occurrence of any significant slip-
emphasis was placed on producing color-coded maps for page of the disks [45].
the earliest stages of HPT processing because it has been A full set of hardness measurements is shown in Fig. 2
shown that these early stages are critical in determining the for disks processed through (a) 1/4, (b) 1/2, (c) 1, (d) 5,
overall behavior during HPT processing [34]. and (e) 20 turns where the lower lines at Hv & 20 denote

Fig. 1 Color-coded contour maps showing the distributions of the Vickers microhardness values at the upper, the center and the lower positions
of high-purity Al after processing by HPT through a–c 1/4 turn and d–f 1/2 turn [19] (Color figure online)

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Fig. 2 Variation of the average Vickers microhardness recorded on the upper, center, and lower planes as a function of the distance from the
center of the disk after processing by HPT using an applied pressure of 6.0 GPa through a 1/4, b 1/2, c 1, d 5, and e 20 turns

the annealed condition prior to HPT processing and the between the different sectional planes for disks of high-
error bars show the 95 % confidence limits: an earlier purity aluminum processed through a wide range of dif-
report provided detailed hardness measurements in the ferent numbers of turns ranging from 1/4 turn to 20 turns.
unprocessed material and demonstrated there was no It is also apparent that, although there are significant
significant variation in hardness prior to processing by variations in the hardness values as a function of the
HPT [29]. For each plot, separate data are presented for positions on the disks in the early stages of processing,
measurements recorded on the upper, center, and lower these variations are essentially lost for the disks taken
planes in three different disks. From these measurements, through 5 turns and after 20 turns all three disks show
it is concluded that there are no significant variations excellent agreement and a high level of homogeneity that

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J Mater Sci (2012) 47:7719–7725 7723

extends both across each plane and in the through-thick- surfaces of disks of high-purity aluminum after different
ness direction. numbers of rotational turns [19].
The general variations in hardness which are visible in
the early stages of processing in Figs 2a–c are consistent
with expectations based on earlier results showing that Experimental results for the magnesium AZ31 alloy
high-purity aluminum exhibits high values of hardness in
the central regions of disks processed through only 1 turn Magnesium has a hexagonal crystal structure and therefore
[27]. A detailed description of these variations in hardness the numbers of active slip systems are limited. This means
in the early stages of HPT processing is beyond the scope that the processing of Mg alloys is often difficult so that
of this short report but a description may be found else- these and other similar metals are generally termed ‘‘dif-
where [19]. ficult-to-work’’ materials [46].
An alternative procedure for evaluating the through- The experiments were conducted using a commercial
thickness variations in hardness, and therefore in micro- extruded AZ31 magnesium alloy containing 3 % Al and
structure, is to plot color-coded contour maps of one-half of 1 % Zn. An earlier report documented the hardness values
the cross-sections of disks processed under different condi- across an AZ31 disk in the unprocessed condition where
tions. These maps are shown in Fig. 3 and they cover five the average hardness was Hv & 55 and there was no sig-
separate conditions from 1/4 turn (upper) to 20 turns (lower) nificant variation in hardness along the disk diameter [37].
with the center of each disk lying on the left. Inspection of Prior to HPT processing, the grain size was measured as
these plots shows there are no significant variations in *9.4 lm. Disks were prepared for HPT and again these
hardness in the axial directions in high-purity Al. Up to 1 turn disks were processed under quasi-constrained conditions
it is apparent that there are regions of higher hardness but [42–44] either at room temperature (296 K) or at an ele-
these regions extend throughout the disks from the upper to vated temperature of 463 K. All processing was conducted
the lower surfaces. At 5 turns, there is a reasonable level of under an applied pressure of 6.0 GPa and further details are
through-thickness homogeneity and after 20 turns there is an given in earlier reports [20, 21]. Lines were scribed on the
excellent homogeneity throughout the thickness. two surfaces of each disk prior to straining and these lines
The development of homogeneity after 20 turns is were used to check for the occurrence of any slippage [45].
consistent with earlier observations, using optical micros- Using this technique, it was confirmed that there was no
copy, where the flow patterns were recorded on the upper disk slippage in these experiments. Separate disks were
processed through 1/4, 1, and 5 turns and these disks were
then sectioned perpendicular to the upper surfaces for
microstructural observations and detailed hardness
measurements.
The appearance of the vertical sections cut through the
disks after processing at 296 K is shown in Fig. 4 for
torsional strains through (a) 1/4 turn, (b) 1 turn, and (c) 5
turns, respectively [21]. Variations in the grain structures
are visible in these vertical cross-sections and there is
evidence for the occurrence of different amounts of
deformation at different levels between the top and bottom
surfaces. This suggests the development of heterogeneities
within the microstructure after processing by HPT at room
temperature.
These heterogeneities are revealed more directly by
plotting color-coded maps for the one-half cross-sections as
shown in Fig. 5 where the maps correspond to 1/4, 1, and 5
turns after HPT processing at room temperature. These
maps demonstrate the occurrence of remarkable heteroge-
neities during HPT processing with higher hardness values
adjacent to the lower surface of the disk after 1 turn and
Fig. 3 Color-coded maps showing the microhardness distributions with a further enhancement in this heterogeneity after 5
across the one-half cross-sections of high-purity Al disks after turns.
processing by HPT through 1/4, 1/2, 1, 5, and 20 turns (Color figure To check whether these results are also typical of AZ31
online) disks processed by HPT at higher temperatures, Fig. 6

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Fig. 6 Color-coded maps showing the microhardness distributions


across the one-half cross-sections of disks of the magnesium AZ31
alloy after processing by HPT at 463 K for 1/4, 1, and 5 turns [20]
(Color figure online)

Discussion
Fig. 4 Flow patterns visible on the one-half cross-sections of disks of
the magnesium AZ31 alloy processed by HPT at 296 K for a 1/4, b 1,
The results from this investigation show there are signifi-
and c 5 turns [21]
cant differences in the levels of homogeneity achieved in
two separate metals in HPT processing where these dif-
ferences appear to depend upon the crystalline structure of
the material.
Specifically, slip processes are easy in high-purity alu-
minum and the material exhibits excellent homogeneity in
the through-thickness direction at all stages of the HPT
processing. In the early stages of processing, up to 1 turn,
there are variations in the Vickers microhardness at different
positions on the planar sections of the disks but these vari-
ations are not reflected in the through-thickness direction
where, as shown in Fig. 3, there are no significant variations
between the upper and lower surfaces of each disk. Fur-
thermore, the microhardness results for high-purity alumi-
num become essentially homogeneous after 5 turns, as
shown in both Figs 2 and 3, and after 20 turns there is a very
high level of homogeneity throughout the disk. The results
Fig. 5 Color-coded maps showing the microhardness distributions are different for the magnesium AZ31 alloy where the
across the one-half cross-sections of disks of the magnesium AZ31 numbers of slip systems are limited and significant microh-
alloy after processing by HPT at 296 K for 1/4, 1, and 5 turns (Color
ardness heterogeneity is visible after 1 turn and after 5 turns
figure online)
when processing both at 296 K in Fig. 5 and 463 K in Fig. 6.
These results demonstrate that aluminum and magne-
shows a similar set of color-coded maps for disks processed sium represent two extremes in terms of the development
by HPT at a temperature of 463 K [20]. As in Fig. 5, these of homogeneity in the microstructure and the microhard-
maps delineate the development of higher hardness values ness during HPT processing. These differences between
adjacent to the lower surface of the disks after 1 and 5 turns different materials must be considered in any future
with correspondingly lower values of the hardness adjacent attempts to develop a universal plot for the hardness vari-
to the upper surfaces. These results are consistent with ations in pure metals processed by HPT [47].
Fig. 5 and they confirm the development of a high degrees Very recent experiments have revealed the development
of heterogeneity in the through-thickness directions of HPT of unusual shearing patterns in materials subjected to HPT
disks of the magnesium AZ31 alloy. processing including the presence of local swirls and

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vortices that are indicative of the development of shear 14. Hebesberger T, Stüwe HP, Vorhauer A, Wetscher F, Pippan R
velocity gradients between adjacent positions within the (2005) Acta Mater 53:393
15. Sakai G, Horita Z, Langdon TG (2005) Mater Sci Eng
disks [48–51]. However, the significance of these patterns A393(2005):344
is not yet known and therefore it is not possible at the 16. Sakai G, Nakamura K, Horita Z, Langdon TG (2005) Mater Sci
present time to determine the significance of this effect in Eng A406:268
achieving homogeneous microstructures. 17. Zhilyaev AP, Oh-ishi K, Langdon TG, McNelley TR (2005)
Mater Sci Eng A410–411:277
18. Horita Z, Langdon TG (2005) Mater Sci Eng A410–411:422
19. Kawasaki M, Figueiredo RB, Langdon TG (2010) Acta Mater
Summary and conclusions 59:308
20. Figueiredo RB, Langdon TG (2011) Mater Sci Eng A528:4500
21. Figueiredo RB, Aguilar MTP, Cetlin PR, Langdon TG (2011)
1. Experiments were conducted on high-purity aluminum Metall Mater Trans 42A:3013
and a magnesium AZ31 alloy to evaluate the potential 22. Pippan R, Scheriau S, Hohenwarter A, Hafok M (2008) Mater Sci
for achieving a reasonable level of homogeneity in the Forum 584–586:16
through-thickness direction of disks processed by high- 23. Hohenwarter A, Bachmaier A, Gludovatz B, Scheriau S, Pippan
R (2009) Int J Mater Res 100:1653
pressure torsion. 24. Valiev RZ, Ivanisenko YuV, Rauch EF, Baudelet B (1996) Acta
2. For high-purity aluminum, the results show there are no Mater 44:4705
variations in the microhardness in the through-thickness 25. Wetscher F, Vorhauer A, Stock R, Pippan R (2004) Mater Sci
directions in any disks processed between 1/4 turn and Eng A387–389:809
26. Wetscher F, Pippan R, Sturm S, Kauffmann F, Scheu C, Dehm G
20 turns. After 5 turns of HPT there is a reasonable level (2006) Metall Mater Trans 37A:1963
of homogeneity throughout the disks and the overall 27. Xu C, Horita Z, Langdon TG (2007) Acta Mater 55:203
level of homogeneity is increased after 20 turns. 28. Xu C, Horita Z, Langdon TG (2008) Acta Mater 56:5168
3. For the magnesium AZ31 alloy, the numbers of slip 29. Kawasaki M, Langdon TG (2008) Mater Sci Eng A498:341
30. Xu C, Horita Z, Langdon TG (2008) J Mater Sci 43:7286. doi:
systems are limited and the processed structures show 10.1007/s10853-008-2624-z
extensive heterogeneity in the through-thickness direc- 31. Xu C, Langdon TG (2009) Mater Sci Eng A503:71
tions after processing by HPT through 1 and 5 turns. In 32. Kawasaki M, Ahn B, Langdon TG (2010) Acta Mater 58:919
general, there is a tendency for high hardness values to 33. Kawasaki M, Ahn B, Langdon TG (2010) Mater Sci Eng
A527:7008
occur adjacent to the lower surfaces of disks when the 34. Xu C, Horita Z, Langdon TG (2010) Mater Trans 51:2
HPT processing is conducted either at 296 or 463 K. 35. Kawasaki M, Ahn B, Langdon TG (2010) J Mater Sci 45:4583.
doi:10.1007/s10853-010-4420-9
36. Duan ZC, Liao XZ, Kawasaki M, Figueiredo RB, Langdon TG
Acknowledgements This study was supported in part by the (2010) J Mater Sci 45:4621. doi:10.1007/s10853-010-4400-0
National Science Foundation of the United States under Grant No. 37. Serre P, Figueiredo RB, Gao N, Langdon TG (2011) Mater Sci
DMR-0855009 and in part by the European Research Council under Eng A528:3601
ERC Grant Agreement No. 267464-SPDMETALS. 38. Wongsa-Ngam J, Kawasaki M, Zhao Y, Langdon TG (2011)
Mater Sci Eng A528:7715
39. Kawasaki M, Alhajeri SN, Xu C, Langdon TG (2011) Mater Sci
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