Extreme Grain Deformation

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com
Acta Materialia 61 (2013) 782817

www.elsevier.com/locate/actamat
Extreme grain renement by severe plastic deformation: A wealth

of challenging science
Y. Estrin a,, A. Vinogradov b,1
a
Centre for Advanced Hybrid Materials, Department of Materials Engineering, Monash University, Clayton, VIC 3800, Australia
b
Laboratory for the Physics of Strength of Materials and Intelligent Diagnostic Systems, Togliatti State University, Togliatti 445667, Russia
Abstract
This article presents our take on the area of bulk ultrane-grained materials produced by severe plastic deformation (SPD). Over the
last decades, research activities in this area have grown enormously and have produced interesting results, which we summarise in this
concise review. This paper is intended as an introduction to the eld for the uninitiated, while at the same time highlighting some
polemic issues that may be of interest to those specialising in bulk nanomaterials produced by SPD. A brief overview of the available
SPD technologies is given, along with a summary of unusual mechanical, physical and other properties achievable by SPD processing.
The challenges this research is facingsome of them generic and some specic to the nanoSPD areaare identied and discussed.
2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
Keywords: Severe plastic deformation; Ultrane-grained materials; Modelling; Properties
1. Historical overview developed the scientic grounds and techniques for materi-
als processing through a combination of high hydrostatic
Grain size can be regarded as a key microstructural fac- pressure and shear deformation [5,6], which today are at
tor aecting nearly all aspects of the physical and mechan- the core of SPD methods. Bridgman eectively introduced
ical behaviour of polycrystalline metals as well as their the dening characteristics of SPD processing in the early
chemical and biochemical response to the surrounding 1950s. In a strict sense generally accepted in the materials
media. Hence, control over grain size has long been recog- engineering community, an SPD process is currently
nized as a way to design materials with desired properties. dened as any method of metal forming under an exten-
Most of the mentioned properties benet greatly from sive hydrostatic pressure that may be used to impose a very
grain size reduction. As the race for better materials perfor- high strain on a bulk solid without the introduction of any
mance is never ending, attempts to develop viable tech- signicant change in the overall dimensions of the sample
niques for microstructure renement continue. A possible and having the ability to produce exceptional grain rene-
avenue for microstructure renement of metals is the use ment [7]. In this Diamond Jubilee issue of Acta Materialia
of severe plastic deformation (SPD)a principle that is it is appropriate to mention that many of the modern ideas
as old as metalworking itself. Recent essays [14] tell a fas- of thermomechanical processing involved in virtually all
cinating story of the art of ancient swordmaking through SPD schemes were already addressed in the rst volume
SPD. The modern-day history of SPD technology has its of Acta Metallurgica in 1953. Carreker and Hibbard [8]
beginnings in the seminal work by P.W. Bridgman who pointed out that the yield strength of high-purity copper
benets substantially from grain renement and this eect
Corresponding author. Tel.: +61 420822164.
is more pronounced at low temperatures. They also noticed
E-mail address: yuri.estrin@monash.edu (Y. Estrin).
that the eect of the initial grain size vanishes at strains lar-
1
On leave from the Department of Intelligent Materials Engineering, ger than 0.1 and for that reason the grain size has little or
Osaka City University, Osaka 5588585, Japan. no inuence on the strength under monotonic loading. A
1359-6454/$36.00 2012 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.actamat.2012.10.038
Y. Estrin, A. Vinogradov / Acta Materialia 61 (2013) 782817 783
similar eect is well known in fatigue where the grain size the reviews [21,22] and special issues of Advanced Engineer-
of wavy-slip materials has no bearing on the fatigue limit. ing Materials [23], Materials Science and Engineering A [24]
These observations can be associated with the vital role and Materials Transactions [25,26].
of the dislocation substructure, which forms during defor- What makes SPD processing techniques so popular is
mation (be it monotonic or cyclic), and it is the size of the the possibility of using them to enhance the strength char-
substructure which determines the strength characteristics acteristics of conventional metallic materials in a quite
of metallic materials. Gow and Cahn [9] emphasized the spectacular way: by a factor of up to eight for pure metals
signicance of crystallographic texture for the deformation such as copper and by some 3050% for alloys [7,27].
and recrystallization behaviour of metals and the eect of Despite the impressive property improvement achievable
evolving texture on the resultant properties. Bell and Cahn with SPD techniques, their uptake by industry has been
[10] outlined many ne features of mechanical twinning, rather sluggish. However, things are now starting to
which play an important part in plastic deformation when change, and there is a common feeling in the nanoSPD
accommodation by dislocation slip is hindered. Beck [11] community that major breakthroughs in terms of indus-
highlighted the possibility of relieving the work-hardening try-scale applications of SPD-based technologies are immi-
eects by post-processing recovery. As will be seen in the nent. We have been working in this area for more than a
following sections, these ideas have had a great impact decade and have followed its developments closely. In this
on the development of the SPD processing and are pivotal article we present our views on what has been achieved,
to the modern concepts underlying these techniques. Now- what is possibly achievable, and what future trends are to
adays, the subject of SPD processing is represented very be expected from SPD processing technologies. This article
prominently on the pages of Acta, as illustrated by the does not represent a full review of the SPD area (one could
analysis in Ref. [4]. Its revival is due to the work of Segal almost say the discipline of SPD, considering the rm place
et al. [12] in the Soviet Union in the mid-1970s. These this group of material processing techniques has taken in
authors developed the method of equal-channel angular literature). Rather, it is our personal take on the SPD area
pressing (ECAP), which later evolved into what is now and an attempt to foretell its future development. Empha-
the most popular SPD technique. It should be mentioned, sis is placed on the scientically challenging aspects of
however, that in the time between the publication of Bridg- SPD, and not so much on technological issues, although
mans studies and the reintroduction of this subject in the some insights into the promises and limitations of SPD
metal science literature, exploration of the possibilities of technologies will also be given.
changing the properties of materials through combined
high pressure and shear deformation went on both in the 2. SPD methods
Soviet Union and in the West. This less known work has
been reviewed in Ref. [13]. In particular, credit should be Among the procedures devised for grain renement,
given to the work by the group of N.S. Enikolopian con- SPD techniques are of particular interest and are the
ducted mainly on polymers. focus of the present review. These techniques enjoy great
A real appreciation for the new possibilities for improv- popularity owing to their ability to produce considerable
ing the properties of metallic materials provided by SPD grain renement in fully dense, bulk-scale work-pieces,
techniques came with the work of the group of Valiev thus giving promise for structural applications. The
[14,15], which demonstrated the relation between the achievable grain sizes lie within the submicrometer (100
enhanced strength and the extreme grain renement 1000 nm) and nanometer (<100 nm) ranges. SPD-pro-
imparted by SPD processing to a range of metals and cessed materials with such grain sizes are generally
alloys. The seminal work of this group, emphasizing the referred to as nanoSPD materials [7], although only the
great potential of SPD processing with regard to property latter ones can be regarded as being nanostructured
improvement through grain structure modication, has according to the conventional denition. Several compre-
heralded what has been described as the microstructural hensive reviews have focused on various nanoSPD pro-
age of SPD research [4]. Over the last decade, the nano- cessing techniques [22,2833]. We refer the reader to the
SPD community (www.nanospd.org) has grown to an original works for specic details and only briey outline
impressive group of researchers, and thousands of publica- the general SPD methodology underlining the common
tions on ultrane-grained (UFG) and nanostructured features and the most important dierences between the
materials produced by SPD have been published. It is nanoSPD processes. By no means do we claim that our
probably not surprising that in the year of the Diamond list of currently available manufacturing schemes is
Jubilee of this journal, the Acta Materialia Gold Medal exhaustive.
goes to Professor Terry Langdonone of the world leaders After the landmark work by Bridgman mentioned above
in the area of nanoSPD materials. A representative collec- [6,34], Langford and Cohen [35] and Rack and Cohen [36]
tion of the relevant articles on the subject can be found in demonstrated in the 1960s that the microstructure of Fe
the proceedings of symposia on UFG materials [16,18] and 0.003% C subjected to high strains by wire drawing was
nanoSPD conferences [19,20]the most recent ones in a rened to subgrain sizes in the 200500 nm range. These
series of ve such forums. Further useful sources include microstructures could not be regarded as UFG proper in
784 Y. Estrin, A. Vinogradov / Acta Materialia 61 (2013) 782817
Table 1
Schematic illustration of some basic and modern SPD techniques.
Process Schematic illustration Equivalent strain Ref.
Basic processes
(a) Equal-channel angular pressing eeff N p23 cot/ [39]
(ECAP) N, the number of ECAP passes
(b)High-pressure torsion (HPT) eeff N p23 prt [34]

r, the distance from the axis, t, the thickness of the
sample, N, the number of revolutions
(c) Accumulative roll bonding (ARB) eeff N p23 lntt0 [54]

t0, the initial thickness of the sample, t, the thickness
of the sample after rolling, N, the number of passes
(d) Multi-axial forging eeff N p23 lnab [57]

Strain is non-uniform. N, the number of processing
steps
emin max p2
(e) Twist extrusion (TE) eff 0:4 0:1tanc; eeff N 3 tanc [61]
c is the twist line slope; N is the number of passes.
Deformation is non-uniform
Derivative processes
(f) Repetitive side extrusion ECAP equivalent [65]
(continued on next page)

Table 1 (continued)
(g) Rotary-die ECAP ECAP equivalent [66]
(h) Cyclic extrusioncompression eeff N 4 lnDd [75]

(CEC) N, number of cycles
(i) Cyclic close-die forging (CCDF) eeff N p23 lnWH [76]

N, number of cycles
(k) Repetitive corrugation and eeff N p43 lnr0:5t

rt
[72]
straightening (RCS) N, number of cycles
Integrated processes
(l) Integrated extrusion + ECAP [110,111]
(m) Parallel channel ECAP (PC- ECAP equivalent [67]

ECAP)
Continuous processes
(n) ECAP- Conform [37] [120]
Table 1 (continued)
(o) Con-shearing [121]
(p) Continuous conned strip [122]

shearing (C2S2)
(q) Continuous repetitive corrugating [73]

and straightening (RCS)
(r) Incremental ECAP (I-ECAP) [126]
(s) Continuous high-pressure torsion [127]
(t) Continuous manufacturing [129]

of bolts
the sense of the commonly accepted denitions [7], because between nanoSPD materials and more conventional mate-
most of the sub-boundaries were low angle. Indeed, it is the rials with subgrain structures produced by cold rolling or
prevalence of high-angle grain boundaries that is com- other common metal forming techniques. This distinction
monly believed to be a signature of UFG materials manu- notwithstanding, these works opened the gates for micro-
factured by SPD. This constitutes a clear demarcation line structure renement by deformation to gigantic strains.
Imparting large plastic strains to a work-piece is a chal- rst requirement stimulated development of dies with
lenging and technically formidable task. It requires a con- reduced friction by implementing surface hardening of
siderable investment in tool design, which on one hand the channel walls, mobile walls [37,43], etc., as well as the
should be durable enough to sustain repetitive high loads introduction of new eective lubricants [44]. The third
during material forming, and on the other hand be suitable requirement led to the understanding of the signicance
for materials processing without causing damage to the of back-pressure for processing of billets with uniform
work-piece. A distinctive feature of SPD processing, which microstructure and improved mechanical properties
meets these requirements, is that the high strain is imposed [43,45,46]. Segal showed that the performance of a die
without any signicant change in the overall dimensions of may be compromised by perceived simplicity of the die
the work-piece. This is achieved due to special tool geom- design [38]. In particular, he warned against the use of dies
etries that prevent free ow of the material and thereby with a corner arc which leads to the occurrence of a widely
produce a signicant hydrostatic pressure. The presence spread fan-shaped plastic zone. This is equivalent to arti-
of this hydrostatic pressure is a clue for achieving the high cially increased friction that spreads shear and gives rise to
strains required for exceptional grain renement. Many signicant heterogeneity of strain. Unfortunately, this
crystalline materials, including those which are brittle important warning was disregarded in many later studies,
under normal conditions (e.g. tungsten oxide, B2O3 glasses which utilized a simplied die design with a rounded
and amorphous materials), gain substantial ductility under outer corner and had to pay a high price in form of sub-
high hydrostatic pressure and can be deformed to large stantial heterogeneity of the deformed structure. By con-
strains without failure. Nowadays many variants of SPD trast, by following Segals philosophy, samples with
techniques, which expressly or tacitly employ this generic uniform microstructure throughout the billet could be fab-
feature of high hydrostatic pressure, are readily available ricated [47,48]. While standard laboratory-scale ECAP rigs
for fabrication of a great variety of UFG materials. can handle billets with cross-sectional dimensions in the
range of 1020 mm, Segals ideas enabled development of
2.1. Principal processing schemes industry-scale ECAP facilities for processing of billets as
large as 50 50 mm2 in cross-section and 500 mm in length
Equal-channel angular pressing (ECAP), less appropri- [43].
ately referred to as equal-channel angular extrusion High pressure torsion (HPT) refers to processing that
(ECAE) in some publications, is at present the most highly evolved from Bridgmans anvils [6], cf. Table 1b, and
developed SPD processing technique (Table 1a). A simple involves a combination of high (GPa range) pressure with
shear strain is introduced when the billet passes through torsional straining. Today this technique is appreciated
the plane where the two channels meet. The cross-sectional by many researchers as the one that allows the most e-
dimensions of the billet remain unchanged, thereby permit- cient grain renement. A handicap of the method is that
ting repetitive pressing, leading to accumulation of very only small coin-shaped samples, typically 1015 mm in
large strains. For example, the equivalent (von Mises) diameter and 1 mm in thickness, can be processed. The
strain, eeq, introduced per pass in ECAP with a 90 angle readers are referred to a comprehensive review on the sub-
between the channels amounts to 1.15 [37,38]. Dierent ject [30] for details. Because of size restrictions, the samples
ECAP variants involving rotations of the billet about the manufactured by HPT are used primarily for research pur-
pressing axis between the passes are possible, and they gen- poses. An important issue for many SPD processing
erally lead to dierent results in terms of the microstructure schemes, including HPT, is the non-uniformity of deforma-
and texture produced. The denitions of these ECAP tion. For instance, during HPT straining, Table 1b, the
routes to which we refer below can be found in Refs. shear strain at the rotation axis should be zero, increasing
[14,15]. linearly in the radial direction if the geometry of the work-
Against the backdrop of a ood of publications on piece does not change. This means that the material near
ECAP processing, it is easy to forget where it all started. the rotation axis of the sample should stay undeformed.
It is therefore timely to recall that the key advantages This is not supported by numerous microstructural obser-
and fundamentals of ECAP, including the mechanics of vations and microhardness measurements showing a rea-
extrusion, the derivation of the optimal process conditions sonably uniform distribution of grain dimensions and
involving a balance between friction, tool geometry, strain microhardness, provided the compressive pressure and
path and its eciency for grain renement, were formu- the number of revolutions of the anvil are suciently large
lated by V. Segal in a series of early publications [12,38 (as in Fig. 1) [4951]. Vorhauer and Pippan [52] explained
42]. He dened ECAP as a deformation technique to this discrepancy by the fact that it is virtually impossible to
impart intensive, uniform and oriented simple shear for realize an ideal HPT deformation due to the misalignment
materials processing. He also demonstrated that ECAP of the axes of the anvils. Alternatively, the development of
is eective if (i) friction between the billet and the die walls a reasonably uniform strain (Fig. 2) and homogeneous
is kept at a minimum; (ii) the angle between the channels is microstructure was explained in terms of gradient plasticity
close to 90; and (iii) the sharp outer corner is fully lled theory coupled with the microstructurally based constitu-
ensuring that the shear zone is as narrow as possible. The tive modelling [53]. This model will be addressed in the
AlMg alloy AA5083 and interstitial-free steel, and was

also used to process Al- and Mg-based laminated struc-
tures and composites [56]. In addition, ARB can be applied
for the production of metalmatrix composites by sheath-
ing mixed powders and subjecting them to a roll-bonding
process [57]. Similarly to conventional rolling, the UFG
structure formed in the course of repetitive rolling is not
equiaxed but rather exhibits pancake-like grains, irrespec-
tive of the type of metal or alloy processed.
Multi-directional forging (MDF), Table 1d, was proposed
as a technique for structure renement in the rst half of the
1990s [5860]. Multiple free-forging operations include
repeated setting in three orthogonal directions. Since MDF
is commonly performed in the temperature interval of 0.1
0.5Tm, where Tm is the melting temperature, grain renement
during MDF is usually associated with dynamic recrystalli-
zation. The homogeneity of the strain produced by MDF
Fig. 1. Vickers microhardness, Hv, of HPT samples after dierent
numbers of turns, N, as a function of the distance from the specimen
is lower than for ECAP or HPT. However, the method can
centre. After Ref. [53] (reprinted with permission). be used for microstructure renement in rather brittle mate-
rials owing to elevated temperatures and the low specic
following section. Axial inhomogeneities observed in an loads on tooling involved. Furthermore, MDF was demon-
HPT-processed Zr3Al intermetallic [54] were associated strated to be a potent technique for manufacturing large-size
with softening eects related to nanostructuring. billets with microcrystalline (UFG) structures and was suc-
Accumulative roll-bonding (ARB), Table 1c, was intro- cessfully applied to a wide range of materials [61].
duced by Saito et al. [55] as a process which was supposed Twist extrusion (TE), Table 1e, is another variant of a
to overcome major limitations of the ECAP and HPT, simple shear deformation process that was introduced by
namely the low productivity of the former and the small Beygelzimer et al. some ten years ago [6264]. Under TE
work-piece size of the latter. The greatest technological processing, a prismatic billet is extruded through a twist
advantage of ARB is that it makes use of a conventional die. While the advantage of the process is its high upscal-
rolling facility. A metal sheet is rolled to 50% thickness ing capacity, it suers from essentially the same generic
reduction. Then, the rolled sheet is cut in two and both problem as the HPT: deformation is non-uniform, being
halves are stacked together, thus restoring the original smallest near the extrusion axis. Investigation by Orlov
thickness of the sheet. The contact faces are degreased et al. [65] showed that this technique is slightly less eective
and wire-brushed before stacking of the sheets, which are in producing UFG structure than ECAP or HPT.
then rolled together to half the thickness. This sequence
of rolling, cutting, brushing and stacking operations is 2.2. Derivative SPD processes
repeated so that ultimately a large strain is accumulated
in the sheet. ARB was successfully applied to a wide range Inspired by the success of the above classical SPD
of materials, including commercial-purity (CP) Al, the techniques, more exotic methods were developed
Fig. 2. Accumulated equivalent strain as a function of the distance from the torsion axis for the rst-order gradient model [53]. The degree of homogeneity
is seen to increase with the overall strain, i.e. with the number of revolutions.
recently with the aim of processing samples other than sim- diate annealing and/or post-ECAP processing by conven-
ple rod or disk stock and/or enabling a higher throughput. tional rolling, drawing or extrusion. The advantageous
Some of them are illustrated in Table 1. A list of these tech- eect of post-processing was conrmed by many research-
niques (which is admittedly not exhaustive) includes: ers who combined dierent post-ECAP techniques to fur-
ther enhance strength [103105], modify texture [106] or
repetitive side extrusion [66]; improve ductility by subsequent annealing [107109].
rotary die ECAP [67]; Finally, new integrated processing schemes, which adopt
parallel channel ECAP [68]; features of dierent processes and combine them in a sin-
hydrostatic extrusion [6971] and hydrostatic extrusion gle-step integrated processing workow [110112], have
combined with torsion [72]; recently been developed, cf. Table 1l. The use of the inte-
repetitive corrugating and straightening (RCS) for pro- grated semicontinuous processing techniques may be a
cessing of sheets or plates [7375]; promising way of overcoming obstacles to uptake of SPD
constrained groove pressing [76]; techniques by industry.
cyclic extrusioncompression (CEC) [77]; Among the recent developments of SPD methods one
cyclic closed-die forging (CCDF) [78]; can recognize a trend to target thin products, particularly
conecone method (CCM) [79]; thin-walled tubes, and produce grain renement by fric-
cryogenic rolling [80,81]; tion-induced shear. One of the work-piece dimensions used
asymmetric rolling (ASR) [82]; in such processes, namely the thickness, is much smaller
continuous frictional angular extrusion (CFAE) [83,84]; than the other two dimensions. The conecone method
friction stir processing (FSP) [85,86]; [79,113] and high-pressure tube twisting [96] are in that cat-
super short interval multi-pass rolling (SSMR) [87,88]; egory, as is a modied tube-twisting technique suggested in
severe torsion straining (STS) [89,90]; Ref. [114]. Depending on the wall thickness, grain rene-
torsion extrusion [91]; ment can be achieved throughout the tube wall thickness
ECAP with rotation tooling in which the conventional or only within near-surface regions of the wall. This
xed die is replaced by rotating tools [92]; method was also applied for producing bimetallic AlCu
reversed shear spinning [92]; tubes with ultrane grain size (as small as about 140 nm
transverse rolling [92]; near the interface of the two metals) [115].
non-equal channel angular pressing (NECAP) for plate- In a similar vein, Umemoto [116118] made a point that
shaped billets [93]; conventional metal processing techniques, such as shot
tube channel pressing [94]; peening, drilling and wear [119], can be used as an eective
KOBO forming [95]; way to create UFG structure and concomitant strengthen-
high-pressure tube twisting (HPTT) for thin-walled ing in near-surface regions of metals and alloys.
tubes [96];
cyclic expansionextrusion CEEa modied CEC pro- 2.3. Continuous SPD techniques and post-processing
cess [97];
simple shear extrusion [98,99]; Many of the SPD methods presented above involve a
vortex extrusion [100]; large number of discrete steps and are not labour and cost
helical rolling [101]; ecient. Furthermore, they suer from the inability to deli-
high-pressure sliding [102]. ver suciently large work-pieces as required for industry-
scale applications. A number of approaches to SPD pro-
From this list alone one can see that there are really no cessing seek to alleviate these disadvantages. In what fol-
bounds to the imagination and resourcefulness of SPD pro- lows, we touch upon them briey.
cess designers, and more and more new SPD techniques Continuous forming (CONFORM), Table 1m, is a well-
have been emerging recently. From a purists viewpoint, known process, the principles of which were rst formu-
not all of them would qualify to be termed nanoSPD lated by Etherington [120] with the aim of improving the
processing according to the denition in Ref. [6], but most ecacy of materials recycling. They were later adapted
of these techniques are cognate with the principal pro- by Segal and co-workers to continuous ECAP of bulk
cessesECAP, HPT, TE or ARBthey derive from and materials [37]. These principles were implemented by Raab
bear some semblance with. Most of these processes use et al. in a rig for production of Al and Ti rods [121]. In this
shear deformation in conjunction with hydrostatic pressure process, the rod is placed in a groove within a rotating
to produce large strains. The potential benets of these shaft and is driven forward by frictional forces and then
derivative techniques include simplied tool design, extruded through an outlet cannel of the die similarly to
lower loads, reduced material loss, the possibility to pro- ECAP. A modication of this process was proposed by Sai-
cess larger work-pieces, automated handling and/or poten- to et al. [122] as continuous shearing, Table 1o, for process-
tial continuous operation. ing of sheets or strips.
It is broadly recognized that strength and ductility may Continuous conned strip shearing (C2S2), sometimes
greatly benet from a combination of ECAP with interme- referred to as ECA-rolling process, Table 1p, is a
modication of the CONFORM method for processing of

sheets or strips [123,124].
Continuous ECAP for sheet manufacturing was dis-
cussed by Lapovok et al. [125,126]. For the Al alloys tested
it was established that just a single ECAP pass was su-
cient to obtain a signicant reduction of normal and in-
plane anisotropy. A variant of the process is continuous
equal-channel angular drawing [125,126].
Repetitive corrugating and straightening (RCS) has an
obvious advantage of providing a simple modication of
rolling to enable continuous SPD processing, as illustrated
graphically in Table 1q [74,75].
Incremental ECAP (I-ECAP). Rosochowski and co-
authors extended general knowledge of incremental metal
forming operations, such as rolling, swaging or rotary
forging, and adapted it to ECAP by modifying it for pro-
cessing of long billets. This process was dubbed incremen-
tal ECAP (I-ECAP) [127]. The basic version of I-ECAP is
shown in Table 1r. The deformation mode is simple shear,
and it is uniform within the marked zone similarly to the Fig. 3. Steel preform with 100 lm porosity inltrated with Al (seen in red)
as revealed by energy dispersive spectroscopy. A 90 ECAP-like knee is
shear deformation in classical ECAP. Separation of the
seen in the bottom left part of the picture. After Ref. [132] (reprinted with
feeding and deformation stages reduces or eliminates fric- permission).
tion during feeding; this substantially reduces the feeding
force and enables processing of very long or continuous
billets. Concluding this section we would like to note that a great
Continuous manufacturing of bolts by ECAP. The group variety of SPD techniques are now available. Their com-
of Prof. Y.-T. Im at KAIST in Korea developed a method mon features are the high hydrostatic pressure and the tool
[128,129] which overcomes the discrete character of ECAP geometry permitting multipass operation to achieve ultra-
by integrating what they call spring-loaded ECAP in a high strains. Dierences are mainly related to the deforma-
continuous bolt manufacturing process (Table 1t). tion mode, the work-piece shape, the ecacy with respect to
AA6016 bolts produced using this technology were shown the strain imposed per pass and the load involved. All these
to be superior to those manufactured in a conventional way factors aect, to a varying extent, the resultant microstruc-
in terms of their tensile strength and fatigue strength. ture, the properties of the product and the upscaling capac-
Continuous high-pressure torsion. An advanced version ity of the technique used. These aspects of SPD processing
of the HPT technique was proposed by Edalati and Horita will be addressed in the next sections.
[130], who demonstrated its viability as a method to pro- A great advantage of the SPD techniques is that they are
duce sheets 0.6-mm thick and 3 mm wide, which possess based on a top-down approach involving grain rene-
UFG structure, in a continuous fashion, cf. Table 1s. ment through breaking down the microstructure of the
While for most structural applications upscaling of the bulk to the submicron scale. SPD processing is thus free
SPD technologies is required, there may be niche applica- from problems of excessive residual porosity and contami-
tions where downscaling would be desirable. The feasibility nation, which are common in nanostructured materials
of such downscaling was demonstrated for the ECAP pro- manufactured in a bottom-up fashion, e.g. by consolida-
cess [131]. Miniaturized dies with channel diameters in the tion of nanopowders. Furthermore, no health hazards
millimeter range were used to deform Al specimens and potentially associated with handling of nanopowders are
achieve grain renement in a single pass. involved in SPD processing.
An SPD-like process of an entirely dierent type was As will be seen below, perhaps the most important dis-
proposed by Estrin et al. [132]. In this solid-state inltra- advantage of SPD is that the eciency of grain renement
tion method, solid aluminium was forced to ll a porous drops with strain [134]. A way to overcome the problem by
steel preform under high pressure in much the same way suppressing dynamic recovery, e.g. by using SPD process-
vias are lled with metal in fabrication of metallic intercon- ing at cryogenic temperatures, was suggested in Ref. [81].
nects by the force-ll process in microelectronics [133]. The However, the microstructures obtained in this way retain
random paths taken by the plastically owing Al are pretty a large volume fraction of low-angle boundaries, giving rise
tortuous and involve numerous kinks. Some of them may to considerable thermal instability and coarsening of the
be similar to those seen in ECAP channels and induce ultrane microstructure produced.
ECAP-like localized shear zones and ensuing grain rene- Given the rapid progress in the eld, we are condent
ment. Penetration of Al into the porous steel preform is that new processes with higher throughput, upscaling
illustrated in Fig. 3. capacity and greater cost-eectiveness will emerge, meeting
the demand for advanced high-performance structural dq k 0

k 2 q; 1
materials in modern industries. de bL
with the intrinsic length scale L corresponding to a charac-
3. Mechanisms of grain renement by SPD teristic length scale of the cell structure, e.g. the cell size,
that determines the dislocation mean free path. Here k 0 is
The main aim of SPD processing, its ultimate raison a constant or a slowly varying quantity and k2 is a mecha-
detre, is extreme grain renement and the ensuing nism-dependent phenomenological parameter sensitive to
strengthening of the processed material. There is no longer strain rate and temperature. The KocksMecking model
any doubt that this is achievable with most malleable and has been extremely successful in providing a description
even with many hard-to-deform materials, and innumera- of stages II and III of strain hardening. However, an ade-
ble experimental results documented in review articles quate description of stages IV and V of strain hardening,
and conference proceedings (e.g. [1620]) are a convincing which are predominant at large strains [146], requires a
testimony to that. Despite this body of experimental evi- more detailed representation of the dislocation population.
dence, the mechanisms of grain renement, which are piv- It involves treating dislocations in the dislocation cell walls
otal in designing the routes to property improvement, are and cell interiors as separate entities, thus introducing two
far from being understood. In particular, there is no gener- distinct evolving dislocation densities. This was done by
ally accepted scenario of grain fragmentation by subdivi- Prinz and Argon [147] and later by Nix et al. [148] who
sion of grains, and the underlying processes have adopted the approach proposed by Mughrabi [149,150],
remained a riddle for researchers to the present day. in which the cell walls and cell interiors are treated as
two distinct phases of a composite. These models were
3.1. Disclination models of grain fragmentation able to account for stage IV and stage V hardening. More
complex models with three internal variables [151] also
Early attempts at unravelling this riddle go back to the provided an adequate description of mechanical response
work of Honeycombe [135], Rybin [136137], Vladimirov at large strains and were successfully applied for metal
and Kusov [138], Mughrabi et al. [139], Indenbom and forming simulations [152].
Orlov [140] and others. This research has prepared the Estrin et al. [153,154] and Zehetbauer et al. [146,155,156]
ground for models introducing grain fragmentation by dis- proposed constitutive models based on Mughrabis com-
location wall formation, notably in form of rows of dislo- posite principle and detailing the evolution of the disloca-
cation dipoles. These concepts have led to a description tion densities in the cell walls and cell interiors, including
of the grain fragmentation process in terms of disclinations interactions between the two phases of the composite.
[141,142]. The process of grain subdivision is represented While Zehetbauers model postulated constancy of the vol-
by the nucleation and propagation of incomplete disclina- ume fraction of cell walls, Estrin et al. emphasized that this
tions, producing misorientation between the adjacent grain volume fraction must decrease during stage IV of harden-
fragments. Models based on coupled disclinationdisloca- ing in order to account for the nearly constant hardening
tion dynamics were shown to provide a reasonably good coecient commonly found experimentally in stage IV.
description of the microstructures formed at large strains The two-dislocation density models [153,154] have
[142]. A recent review of disclination-based models become a useful platform for modelling SPD processes
addressing, in particular, bulk nanostructured materials (cf. [155,157,158]), and we shall present them in a condensed
can be found in Ref. [143]. form here. The models apply to dislocation cell-forming
materials and address suciently large strains when a cell
3.2. Dislocation density based models structure is already formed. The primordial stage of the
deformation in which this happens is not considered.
The most commonly accepted type of models of grain Understanding the self-organization processes leading to
renement due to large strain, particularly under SPD con- the emergence of a dislocation cell structure is one of the
ditions, are based on the notion that a dislocation cell greatest unsolved problems of the dislocation theory, and
structure, which forms already in the early stages of plastic numerous modelling eorts, including discrete dislocation
deformation, gradually transforms to the nal ne grain dynamics simulations [159], are being devoted to this prob-
structure. This is believed to occur through continual lem. An assumption made in the models [153,154] is that the
decrease in the average grain size accompanied by accumu- average dislocation cell size, d, scales inversely with the
lation of misorientation between neighbouring dislocation square root of the total dislocation density, q:
cells. This type of model goes back to Kocks and Mecking p
d K= q; 2
[144,145] who described the deformation behaviour of met-
als and alloys in terms of a single internal variable: the total where K is a proportionality constant. Eq. (2) goes back to
dislocation density q. Within this approach, the dislocation an early work of Holt [160] in which patterning in a
kinetics equation governing the evolution of the total dislo- dislocation population was rst considered. While a sub-
cation density is represented in its simplest, yet rather gen- stantial body of evidence supports the validity of Eq. (2)
eral, way as: for steady-state deformation, extending it to the dynamic
case of evolving dislocation structure is a major assump- terms in the evolution equations represent possible disloca-
tion, which denitely needs further substantiation. tion reactions involved. Their physical origin was explained
The total dislocation density is considered to be given by in Refs. [153,154]. For example, the loss of cell interior dis-
the weighted sum of the dislocation densities in the cell locations to the walls where they get entrapped is repre-
walls (subscript w) and cell interiors (subscript c) sented by the rst term of Eq. (6) and the second term of
q f qw 1 f qc ; 3 Eq. (7). The last terms in both equations account for the
dynamic recovery. The quantity c_0 denotes a reference
where f denotes the volume fraction of the cell walls. Obvi- shear rate. In the low-temperature regime typical for SPD
ously, the latter quantity is linked to the cell size d and the processing, i.e. below half the melting temperature, the
wall thickness w through a relation that should account for exponent n in both equations can be taken to be inversely
cell morphology. As this relation is not very sensitive to the proportional to the absolute temperature T, while the coef-
particular shape of the cells, a simple expression cient ko can be considered constant. This corresponds to
d 3 d w3 dynamic recovery being governed by dislocation cross-slip.
f ; 4 In Zehetbauers model [146,155,156], it was assumed that
d3 dynamic recovery in cell walls is controlled by dislocation
corresponding to the idealized case of cube-shaped cells is a climba non-conservative process involving vacancy diu-
reasonably good one. In modelling SPD processes sion. This process is characterized by c_0 , which is given by
[161,162], it was assumed that the volume fraction de- an Arrhenius equation with the activation energy repre-
creases from an initial value fo to a saturation value f1 . senting that for self-diusion, the exponent n being a
This approach of saturation is governed by a phenomeno- constant.
logical equation: As vacancy formation is inuenced by hydrostatic pres-
f f1 fo f1 expc=~c; 5 sure, this approach introduces a direct eect of hydrostatic
pressure on the dislocation recovery kinetics [163]. An
which is supported by experiments on Cu. The parameter ~c appropriate modication of the dynamic recovery term in
represents the inverse of the rate of this variation with the Eq. (7) to include the hydrostatic pressure made it possible
plastic shear strain c. The growth of the total dislocation to account for the eect of back-pressure on the ECAP
density q and the concomitant decrease of the average cell processing of an Al alloy [164].
size d with strain suggests that a decrease of the cell volume The type of model described above proved to be a useful
fraction f, which is implied by Eq. (5) for f1 < fo, is only descriptive and predictive tool for computer simulations of
possible if the cell wall thickness decreases fast enough with ECAP processing of copper [157], aluminium [161], Al
strain. This assumption was implicit in the original model alloy 6016 [164], interstitial-free steel [165], CP titanium
[153,154]. Thinning of cell walls with the progress of [158] and HPT processing of copper [53,166]. The focus
straining is a reasonable notion, as geometrically unneces- of these simulations was the calculation of the strength
sary dislocations not contributing to misorientation be- characteristics of the ECAP-processed materials. However,
tween neighbouring cells will recover with strain. the model was also used for calculating the texture of cop-
However, the phenomenological ansatz made in Eq. (5) per developing as a result of ECAP processing, albeit in a
can be replaced by a more physical assumption of the var- very simplied way [167]. We shall return to the issue of
iation of the cell wall thickness. For instance, w can be de- texture below.
ned in terms of a characteristic length controlling the The model of grain fragmentation presented above is
decay of the stress eld of the cell wall dislocations, which based on the idea that ne granularity is attained through
p
should scale with 1= qw . In this way, both the average cell dislocation cell formation with (tacitly assumed) accumula-
size and the cell wall thickness would be expressed in terms tion of misorientations across the dislocation cell bound-
of the dislocation densities. aries. In other words, gradual transformation of
The evolution of the dislocation ensemble is captured in dislocation cell walls, or at least a large proportion of them,
a set of coupled dierential equations for the dislocation to high-angle grain boundaries is implied. Pantleon [168]
densities in the cell interior and cell walls under the Tay- and Estrin et al. [169] considered the increase of dislocation
lor-type assumption that the shear strain is the same in cell misorientations with progressing straining in terms of a
both phases: probabilistic approach. In both models, preferred storage
p p 1=n
dqw 6b 1 f
2=3
3b 1 f qw c_ of dislocations with a certain sign of the Burgers vector,
k0 qw ; which occurs locally within a cell wall, gives rise to misori-
dc bdf fb c_ 0
entation between the cells separated by the wall. This
6 occurs stochastically, leading to a continual increase in
p 1=n the misorientation angle, which eventually saturates. The
dqc 1 qw 6 c_
a p b 1=3
k 0 qc : 7 results are consistent with the observed levels of misorien-
dc 3 b bd1 f _
c 0
tation angles (several degrees) associated with the so-called
Here b is the magnitude of the Burgers vector and the coef- incidental dislocation boundaries (in the terminology of
cients a and b are numerical constants. The various the Hansen school [170172]), but cannot account for the
occurrence of a very signicant fraction of high-angle grain thesis [159] that the dislocation cell size and the misorienta-
boundaries usually found experimentally in SPD-processed tion angle tend to saturation with the same rate and that
materials, which are referred to as geometrically necessary their product is independent of strain.
boundaries [170,171]. Malygin, who also considered the It is pretty obvious that the mechanism of grain frag-
evolution kinetics of cell size and misorientation angle mentation considered cannot lead to an arbitrarily small
[173], associates the occurrence of the geometrically neces- grain size. Indeed, an estimate of the dislocation density
sary boundaries with elastic bending of the crystal caused in Eq. (2) in terms of the applied stress r Ms (where M
by non-uniformity of plastic deformation and the atten- is the Taylor factor, which accounts for texture) leads to
dant local distortions in the crystal bulk or the outer shape the following estimate for the smallest achievable grain size
of the specimen. Obviously, such boundaries are not ds :
accounted for by the models discussed. ds G
Although Eq. (2), which describes cell/grain size evolu- KMa : 8
b rm
tion with the accumulation of the dislocation density, was
introduced in a heuristic way, there are strong reasons to Here rm is the highest possible stress, G is the shear modu-
believe that it is a robust relation which can be used in cur- lus and a is a numerical constant, typically of the order of
rent and future models. This can be expected based on both 0.5. With K of the order of 10 and M around 3 it is easily
dimensional considerations and rudimentary modelling of seen that even for rm close to the theoretical strength the
dislocation pattern formation [171,174]. Nevertheless, nal grain size cannot be smaller than ds 100b. That is
developing a model which would provide an adequate to say, the average grain size cannot attain values in the
description of the evolution of dislocation cell size and mis- nano range, i.e. below 100 nm, if the assumed mecha-
orientation angle distributions is as much a challenge as is nism of grain subdivision via dislocation cell formation
the development of a full theory explaining the formation controls grain renement.
of a dislocation cell pattern in the rst place. There is also a further limitation on the smallest grain
Obviously, according to Eq. (2), the cell/grain size d has size achievable by this mechanism. As suggested in Ref.
to saturate, asymptotically reaching a steady-state value [177], below a certain critical value of the grain size, dc, dif-
prescribed by the steady-state values of the dislocation den- fusive accommodation of dislocations in the walls is pre-
sities governed by Eqs. (6) and (7). (We note that the vol- dominant and their storage is negligible. In this regime,
ume fraction of cell walls, f, also tends to saturation.) no strain hardening will occur. The critical grain size is
Observations tell us that even when d approaches satura- given by:
tion, e.g. with the number of ECAP passes or the rotation 1=3
DGB b
angle in HPT, the misorientation angle still evolves visibly dc ; 9
c_
(cf. [175]). Data for a Ni single crystal processed by HPT
(Fig. 4 [176]) show that the various characteristics of the where DGB is the grain boundary diusivity. The critical
microstructure, such as the mean length of small- and grain size dc estimated for room temperature SPD of cop-
high-angle boundaries, saturate at rates dierent from that per is about 250 nm. This is, indeed, consistent with the
for the average cell/grain size. This is at variance with the average grain size found in copper processed by ECAP at
Fig. 4. Tendency to saturation with equivalent strain for various characteristics of the microstructure of monocrystalline Ni fragmented into a dislocation
cell/grain structure. The data in the right-hand side gure represent the mean lengths of cell walls (misorientation angle below 15) and high-angle grain
boundaries (misorientation angle above 15), as well as the fraction of the high-angle grain boundaries. After Ref. [176] (reprinted with permission).
room temperature [161,178]. As seen from Eq. (9), dc is a are captured in the magnitude of the ZenerHollomon
decreasing function of the strain rate and, through the parameter Z [186]. For the case of copper, the authors
grain boundary diusivity, an increasing function of tem- demonstrated that deformation-induced grain renement
perature. Clearly, during SPD-induced grain fragmentation is favoured by large values of Z. Thus, the mean transverse
the grain size should saturate at the level of the larger of the grain size was shown to decrease from 320 to 66 nm when
two critical quantities, ds and dc. ln Z was raised from 22 to 66. The smallest grain size values
In deciding what mechanisms control the saturation of obtained are substantially smaller than dsthe lower
the microstructure evolution, one can be guided by the bound of the grain size for the case of gradual transforma-
above semi-intuitive arguments. However, a strict theory tion of the dislocation cell structure to a new, ultrane
based on a detailed analysis of the dislocationgrain grain structure. This implies that an entirely dierent mech-
boundary interactions that could shed light on these mechanism of grain renement operates at large Z-values. It was
anisms is still lacking. For instance, it is not quite under- concluded in Ref. [185] that this mechanism involves for-
stood at what grain size scale the grain boundaries lose mation of nanotwin bundles, which transform to nano-
their ability to eectively hinder dislocation motion and grains by fragmentation of twin/matrix lamellae due to
to act as storage sites where dislocation pile-ups forma interaction of twin boundaries with dislocations or shear
mechanism commonly accepted as the cause of the Hall banding. Nanotwinning was also shown to be a determin-
Petch eect. As dislocation-mediated plasticity is at play ing factor in the inner structure enabling a favourable com-
even in truly nanostructured materials [179], a systematic bination of strength and ductility of copper processed by
study of the relative roles of diusion- and dislocation- low-temperature ECAP followed by cryodrawing and cryo-
controlled processes using the entire available arsenal of rolling [187] and SUS316L austenitic stainless steel with
modelling techniques is the order of the day. low stacking fault energy [188,189].
A further, relatively new, modelling approach to grain Grain subdivision associated with nanotwinning, pro-
fragmentation was proposed in Ref. [180]. Grain subdivi- ducing a dynamic HallPetch eect under high Z-value
sion was treated there as a result of the development of lat- conditions possible for materials with a pronounced pro-
tice curvature within an individual grain due to constraints clivity for twinning, is not universal. However, it can be
imposed by the neighbouring grains. Specically, it was conjectured that quite generally more violent SPD defor-
assumed that the rotation of the crystallographic planes mation characterized by a large Z-value would promote
in a grain due to dislocation slip is impeded near the grain formation of a ner grain structure and a high strength
boundaries. Due to this retardation the lattice rotation at of the processed material. Indeed, suppression of dynamic
the periphery of a grain is smaller than in the middle part. recovery for increased Z-values [190] would promote the
The geometrically necessary dislocations associated with formation of ner granularity according to the scenario
the lattice curvature thus produced were considered as of a peaceful transformation of dislocation cell structure
the main cause of grain subdivision. Used in conjunction to the grain structure. In extreme cases, for most energetic
with the dislocation-density model [153,154], the grain sub- DPD conditions with very high Z-values, one probably
division rule dened in [180] enabled the prediction of the cannot rule out situations when severe local distortions
strain-hardening behaviour of copper, along with a simula- (or even amorphization) of the crystal lattice may induce
tion of the evolution of the grain size distribution and tex- nanocrystallization. The possibility of deformation-driven
ture. The model predictions were found to be in excellent amorphization was recently discussed in a stimulating
agreement with experiment. This consideration of grain and thought-provoking paper by Raabe et al. [191]. We
subdivision in texture simulations is a feature that was realize, of course, that at this stage the amorphization/
not implemented in earlier work, which was reviewed in nanocrystallization scenario of nanostructuring by high-Z
Ref. [181]. With the grain subdivision model [180], the SPD is somewhat speculative. It would take both model-
agreement between the calculated and the experimental ling and experimentation to verify or disprove its feasibil-
texture stemming from ECAP processing of copper was ityanother formidable task to work towards. It is
shown to be improved. The method was further advanced interesting to note that amorphization of the intermetallic
in a very recent work on SPD processing of Al [182]. compound Zr3Al by repeated cold rolling with subsequent
In this relatively short overview, we cannot address all nanocrystallization was reported recently [192].
possible mechanisms relevant for SPD and discuss all mod-
els proposed to account for them. Some complementary 4. Properties of UFG materials produced by SPD
material can be found in earlier reviews [183,184]. What
we would like to mention, however, is a radically dierent 4.1. Strength and ductility and their impact on other
pathway to grain renement, based on the work by the mechanical properties
group of Ke Lu at the Institute of Metal Research in
Shenyang, which was summarized in Ref. [185]. It is based Investigations of the behaviour of UFG materials have
on dynamic plastic deformation (DPD), which involves been greatly motivated by the expectations that they may
high strain rates, often in combination with low deforma- possess unique properties as well as by the desire to under-
tion temperature. Both strain-rate and temperature eects stand the fundamental mechanisms underlying the specic
Table 2
Mechanical properties of selected UFG metals and alloys produced by SPD.
Material Processing r0.2 rUTS d rfo
(MPa) (MPa) (MPa)
AZ31 [231] SC 50 170 10 40
HR 370 C 175 277 21 95
HR + ECAP 4Bc 200 C 115 251 27 95
[384] ST420 C 2 h + Q, ECAP4Bc 320200 C 180 286 9.4 40*
ZK60 [110] As-cast 222 264 7.4 55
[385] IE 300 C 310 351 17 150
AA1050 (99.5%, CP Al) [386] O 28 70 40 28
ECAP 8Bc N/A N/A N/ 52
A
1100 [387] ARB 8 210 275
Non-age-hardenable AA5052 (Al 2.6Mg [388] H38 255 290 7

0.22Cr, 0.26Fe)
ECAP 8, 150 C 394 421 9
[108] ECAP + A 200 C, 6 h 350 370 10.5
AA 5056 AlMg O 122 290 43 116
H18 407 434 10 152
ECAP 4C, 150 C 280 340 25 116
ECAP 8Bc, 110 C 392 442 7 116
AA5083 AlMg [389] O 145 290 22
H321 230 315 16
ST 350 C 1 h, ECAP 200 C, 8C 276 352 20
Age-hardenable AA6061 AlMg O 150 270 48 40**

T6 276 310 12 50**
[204] ST ECAP, 1, 125 C 310 375 20 80**
ST ECAP, 4Bc, 125 C 380 425 20 <60**
AA 2124 T851 455 492 7.2 125
[390] T851 + ECAE 8Bc, BP 330 602 7.2 290
AA 7075 O 105 230 17
T6 503 525 9
[391] ECAP 2Bc + NA 1 month 650 720 8.4
Al4Mg0.3Sc HD 315 415 17 160
Al5.2Mg0.32Mn HR 240 375 29 150
0.25Sc
Al1.5Mg0.2ScZr [200] ST + ECAP, 8Bc, 150 C 340 360 13 135
Al3.0Mg0.2ScZr ST + ECAP, 6Bc, 150 C 370 400 15 140
Al4.5Mg0.2ScZr ST + ECAP, 6Bc, 160 C 230 410 29 150
Al6.0Mg0.2ScZr ST460 C 24 h + ECAP, 4Bc, 320 C 240 260 8 100
Al5.7Mg0.32Sc0.4Mn [392] ST520 C 48 h + ECAP, 8C, 325 C 280 300 8 190
AA6106 + 0.1Zr [205] ST, AG190 C 4 h 250 350 23 175
AA6106d + 0.1Zr + 0.5Sc ST + ECAP 4 + Ag190 C 4 h 570 590 9 225
ST, AG190 C2 h 375 425 16 210
ST + ECAP 4 + AG190 C2 h 625 650 8 275
Ti (grade 2) CR 380 460 26 240

[205] ECAP 8Bc 400 C 640 810 15 380
[393] ECAP 8Bc 400 C, CR 87% ECAP 970 1050 8 420
[394] ECAP 6Bc 420 C 630 670 32 350
Ti (grade 4) [265] CR 530 700 25 350***

ECAP 4Bc450400 C, FD300 C 1150 1240 11 590***
ECAP 4Bc450400 C, F400300 C, D, 1100 1250 13 610***
A350 C 6 h
(continued on next page)
Table 2 (continued)
(MPa) (MPa) (MPa)
Ti6Al4V (grade 5) STA, ST 950 C, AG 540 C 1100 1170 10 700
[395] MF 1180 1300 7 700***
[396397] ECAP 600 C, A 500 C 2 h 1270 1370 11 740***
A960 C 1 h, Q, AG 650 C 4 h, ECAP 1340 1370 14 620
4Bc650 C,E30020 C
Au (K24) [47] O 133 80

Drawn 185 1
ECAP, 4Bc 245 34
Au25Ag (K18) O 185 82
ECAP, 4Bc 430 25
Au12.5 wt.% Ag12.5 wt.% Cu (K18) Q 505 64
CR 75% 685 21
CR 75%, AG 300 C, 1 h 835 13
ECAP, 4Bc 880 6
ECAP, 4Bc, AG 300 C, 1 h 1070 3
Cu 99.96% A 140 240 46 65
Cu 99.96% [246] ECAP, 8B 390 440 22 80
Cu 99.96% [248] ECAP, 12Bc 480 520 18 80
Cu 99.95% [176] A 68 332 45.5
ECAP 1 342 358 8.9
ECAP 2Bc 407 424 8.6
ECAP 4Bc 415 455 8.2
ECAP 8Bc 385 449 8.5
ECAP12Bc 358 423 8.5
ECAP 16Bc 348 407 10.0
Cu 99.98% [245] ECAP 20Bc 375 440 15
Cu 99.9% CR 100
Cu (99.99%) [398] ECAP 8Bc 375 387 170
[210] ECAP + CrioD95% + CrioR96% 500 600 11
Cu0.8Cr0.07Zr Q, D, AG 500 C, 1 h 100 100
Cu0.8Cr0.05Zr [399] ECAP 8Bc, AG 450 C, 1 h 490 630 14 240
Cu0.44Cr0.21Zr [37] [222] ECAP 8Bc, AG 500 C, 1 h 650 720 12 285
Cu0.36Cr [221] ECAP 8A, AG 500 C, 1 h 409 427 24 170
Cu0.36Cr ECAP 8Bc, AG 500 C, 1 h 456 467 20 160
Cu0.36Cr ECAP 8CA, AG 500 C, 1 h 438 454 23 180
Fe (99.95%) A 90 260 54
[400] ECAP 4Bc 696 723 7
[37] ECAP 8B 850 980 1
Fe36Ni Invar [206] A 275 490 40 137
ECAP 2Bc 570 732 47 280
ECAP 8Bc 690 790 35 290
ECAP 12Bc 835 912 52 330
LC steel [401] CR 70% 500 700 20
Fe0.08C0.18Si0.42Mn0.024P0.018S ECAP 3Bc 420 820 40
LC steel [402] ECAP 350 C 310 480 30
Fe0.15C0.25Si1.1Mn ECAP, A 480 C 1 h 937 943 11
ECAP, A 480 C 24 h 805 823 12
ECAP, A 480 C 72 h 713 733 19
683 720 20
LC steel [65] HR 110 70
Fe0.15C0.9Si9Mn0.5P0.4S0.4Al RSE 1 580 24
0.27Ti RSE 2 650 21
RSE 10 1050 10
SUS 316L stainless steel [187] Q 1050 C 220 560 80 210
ECAP 1 150 C 850 900 30 360
ECAP 2Bc 150 C 1040 1120 20 420
ECAP 3Bc 150 C 1300 1340 18 570
ECAP 4Bc 150 C 1480 1560 17
Table 2 (continued)
(MPa) (MPa) (MPa)
08Kh18N10T stainless steel [403] HR, Q 1050 C 319 623 62

Fe0.07C17.3Cr9.2Ni0.2Cu0.7Ti ECAP 2Bc 990 1080 13
0.6Si1.4Mn 0.003S0.003P ECAP 3Bc 1120 1180 13.5
ECAP 4Bc 1315 1140 11
AISI 304L stainless steel [404] A1150 C 2 h 168 176 61
ECAP 700 C 710 556 34
1121 1136 12
d, Grain size; r0.2, conventional yield stress; rUTS, ultimate tensile strength; d, elongation at break; rfo, endurance limit (on the basis of 107 symmetric
pushpull cycles, and stress ratio R = 1, if not otherwise specied); processing temperature is shown where it diers from ambient; O, as received
condition, no SPD processing; CR, cold rolling; HR, hot rolling; F, forging; D, drawing; MF, multistep forging; S, solution treatment; Q, quenching; A,
annealing; AG, ageing; NA, natural ageing; BP, back pressure.
Data obtained from the total strain amplitude control test at about 106 cycles to failure.
*
R = 0.05.
**
R = 0.
***
Rotation-bending test.
Based on 5 108 cycles to failure.
Data obtained from the total strain control test at about 2 105 cycles to failure.
properties associated with extreme grain renement. In the tive of dierent groups of pure metals, as well as of some
present section we review the state-of-the-art of both model and commercial alloys.
aspects of research. Despite the broad diversity of structural states and pro-
Strength and ductility are primary grain-size-dependent cessing schedules used in SPD, cf. Table 1, the common
characteristics of a material, which determine virtually all trends seem to be clear: a spectacular enhancement of
facets of its mechanical response. We shall, therefore, rst strength upon SPD processing concurs with a loss of duc-
address these properties, especially as they have been tility. This is vividly illustrated in Fig. 5, where the
repeatedly claimed in literature as the ones that benet improvement in strength with the number of ECAP passes
most from grain renement. Fatigue resistance and the is shown. The main reason for this loss of ductility is a
toughness are the most important secondary properties, combination of high ow stress and low strain-hardening
which are directly governed by strength and ductility. The capability of SPD-processed materials. The Considere cri-
ideal structural material should combine high strength with terion signifying the onset of necking at the point where
sucient ductility, along with high fracture toughness. the strain-hardening coecient drops below the value of
However, high strength and good ductility are often mutu- the ow stress (see Eq. (11) below) is therefore more readily
ally exclusive, and improving both at the same time is a fullled in materials modied by SPD. Nevertheless, we
very challenging task. A strategy for strength improvement note that the tensile ductility of materials processed by
follows straightforwardly from the HallPetch relation SPD is actually higher than that of the nanostructured
between the yield stress ry and the grain size d: materials produced, for example, by cryomilling [197]. In
some cases the ductility of the SPD-processed materials
ry r0 K HP d 1=2 : 10
may even exceed that of their conventionally strain-hard-
Here r0 is the so-called friction stress and KHP is a constant ened analogues. Thus, enhancement of ductility was dem-
for a given material. Grain renement has long been used onstrated for ECAP-processed CP Al, as well as for
as an ecient tool to improve both strength and toughness ARB-processed UFG Al and AA6016 [198,199]. In review-
of steels simultaneously. (This was the basis of the ancient ing the data available for Al alloys, Markushev and Vinog-
art of swordmaking mentioned in Section 1.) It should be radov [200] came to the conclusion that no improvement in
noted that due to the additive nature by which the various ductility was found in non-age-hardenable AlMg alloys,
mechanisms contribute to strength, pure materials and di- such as AA5056 [201]. The situation is quite dierent with
lute solutions, which are most responsive to grain rene- the age-hardenable Al alloys, which were found to be most
ment, have a great potential for replacing some responsive to SPD in terms of structure renement,
conventional alloys. Replacing titanium alloys with leaner strength enhancement and fatigue life and ductility
CP Ti is one example that will be discussed below. Starting improvement [27,201205]. For example, Roven et al.
from the early studies in SPD [21,37,193196], a substantial [206] reported a considerable (2535%) increase in the ulti-
increase in strength (say, by a factor of 38) over that of the mate tensile strength, rUTS, in various Al alloys of the 6xxx
well-annealed or conventionally manufactured samples was series as compared with their conventional T6-heat treated
reported repeatedly. This is seen in Table 2, which displays analogues. Not only was this strength increase achieved
a list of currently available experimental data representa- without compromising ductility, but, in fact, tensile
It is evident that the uniform elongation does not com-

monly improve as a result of SPD processing; however, the
materials resistance to localized plastic ow in the post-
necking regime can increase remarkably. This is exempli-
ed by numerous observations, e.g. on Al alloy 6061
[207], Ti [208] and Fe36Ni Invar [209], cf. also Figs. 5
and 6 for SUS 316L steel and copper, respectively.
Enhancement of both strength and ductility is, however,
tricky and is not common. Some successful examples,
which are exceptions rather than the rule, have, however,
been reported. These include the results on Ti [210], Cu
and CuAl alloy [187,211,212], CuZn [213], AlMgSc
[214] and AlMgSi [215]. In all these examples, success
was based on a savvy choice of chemical composition
and the specic processing schedules combining the above
principles. For instance, Zhao et al. [213] developed a mul-
tistep processing schedule involving ECAP followed by
cryodrawing and cryorolling. They demonstrated a tremen-
dous improvement of strength coupled with enhanced duc-
tility (with uniform tensile elongation for Cu amounting to
910%, Table 2). However, the authors of this impressive
report used sub-size specimens of 0.1 mm thickness. They
suggested that thicker samples would exhibit even higher
ductility, but we are not aware of any published result con-
rming the ductility being the same or higher for conven-
tional size specimens. The problem of small-size
specimens, which are commonly prepared after HPT or
other kinds of SPD processing, has been addressed to some
extent by Zhao et al. [216,217], who demonstrated that
tests without appropriate strain measurements across the
gauge length conducted on sub-size specimens return con-
Fig. 5. Tensile stressstrain curves (a) and SN fatigue plot (b) for the
SUS 316L austenitic stainless steel after ECAP (14 passes at 150 C, route siderably overestimated elongations to failure.
Bc). The bright-eld TEM images in the inset illustrate the nanostructure Another strategy for achieving a simultaneous increase
which formed uniformly across the specimen due to mechanical twinning. in ductility and strength can be borrowed from the classical
Adapted from Ref. [189] (reprinted with permission). coarse-grain world: it has been recognized in conven-
tional metallurgy that improved ductility can be associated
elongation to rupture increased by a factor of 1.52. Simi- with delayed necking. This can be achieved by activating
larly, it was reported that the inuence of SPD on the room mechanisms of deformation other than dislocation-based
temperature ductility of Al alloys may be ambivalent [200]. ones, such as phase transformations or twinning, when
500 500
2A passes 2A passes 4A passes
4A passes
400 400
Stress, / MPa
300 300 rolling

1 pass
200 rolling 200

1 pass
100 100
(a) (b) c
0 0
0.00 0.05 0.10 0.15 0.20 0.00 0.01 0.02 0.03 0.04 0.05
Plastic strain pl Plastic strain pl
Fig. 6. (a) Tensile stressstrain curves for SPD-manufactured copper (rolled to 75% equivalent strain or ECAP-processed by 1, 2 or 4 passes via route A):
full curves; (b) enlarged parts of the curves representing the initial hardening behaviour, which can be accurately tted by the single dislocation density
model (Eq. (13)).
dislocations are blocked and cannot accommodate dilute CuCrZr alloys [224225]. Potentially it is applica-
imposed plastic strains eectively. These well-known mech- ble to many UFG and nanostructured systems, opening the
anisms, widely utilized in steels, are referred to as transfor- door for large-scale industrial applications.
mation-induced plasticity (TRIP) [218] and twinning An impressive ductility enhancement was observed for
induced plasticity (TWIP) [219]. The formation of a tensile Mg alloys processed by ECAP [226228], which is believed
neck is accompanied by a concentration of stress and an to be due to the specic texture that develops under simple
increase in stress triaxiality at the neck [220]. As a result shear in hexagonal close-packed (hcp) materials. Record
of the increased triaxiality and raised stress, the probability tensile elongations were reached in ECAP-processed Mg
of martensite nucleation increases in austenitic TRIP steels alloys ZK60 [229232] in the superplastic deformation
[221]. A local phase transformation at sites with high stress regime. An exceptionally good combination of tensile
concentrations leads to intensive local hardening and strength and ductility was also achieved with titanium pro-
blunting of the crack tip. Therefore enhanced uniform cessed by ECAP [233].
elongation is achieved because of retardation of local neck- Of course, grain renement alone is not sucient for
ing. So far the ecacy of the TRIP eect in metastable achieving enhanced strength and improved fatigue perfor-
UFG steels is largely unexplored, but the rst results are mance, particularly for hcp-Mg-based alloys where the tex-
encouraging. Tao et al. [222] showed that the martensitic ture produced by ECAP, or a derivative thereof, is not
phase transformation provides a source of strain hardening favourable for strength [226,227]. Indeed, under ECAP
through replacement of the austenite with the much harder with the commonly used 90 angle between the entrance
martensite. This contributes to local strain hardening, thus and the exit channels the texture is such that the basal
delaying strain localization. Successful implementation of planes in the majority of the grains are predominantly ori-
the twinning-based deformation strategy using the major ented at 45 to the pressing direction [226]. In subsequent
advantages of TWIP alloys with low stacking fault energy tensile tests with the tensile direction aligned with or close
(SFE) was demonstrated by Zhao et al. [213]. The SFE, a to the pressing direction, basal slip is activated relatively
key parameter controlling the ability of dislocations to easily. The associated texture-related reduction in the yield
cross-slip, is sensitive to the chemical composition and strength acts against the HallPetch-type strength enhance-
therefore can be tuned by alloying. Specically, UFG brass ment due to grain renement, while ductility is improved,
Cu10 wt.% Zn with a SFE of 35 mJ m2 was found to as was demonstrated for Mg alloy AZ31 [234].
have a much higher strength than UFG copper with a Orlov et al. [111] recently proposed a new integrated
SFE of 78 mJ m2 [213]. This is, of course, not surprising SPD processing route (Table 1l). The combination of a
in view of the solid-solution strengthening and planarity large reduction in the cross-sectional area of a billet by
of slip in brass, but what is remarkable is that the ductility extrusion with severe deformation by ECAP in an inte-
of this material was also considerably improved. This was grated process allowed the production of magnesium
attributed to accumulation of both twins and dislocations ZK60 bars 16 mm in diameter and up to 4 m in length in
during tensile deformation. The success of this strategy is a single pass. The produced bars exhibit a remarkably good
also illustrated in Fig. 5 for a stable SUS 316L austenitic balance of strength and ductility (Table 2). The analysis of
stainless steel. Due to its low SFE, this steel has a propen- the microstructure and texture of the processed bars
sity for twinning, and, indeed, deformation twinning was showed that this excellent combination of properties is
activated during ECAP processing at 150 C, as shown in attributable to the synergy of the ne-grained microstruc-
the inset of Fig. 5a. After just three ECAP passes by route ture and the favourable texture promoting basal slip (in
Bc, a truly nanoscale grain structure with grain dimensions concert with non-basal slip), yet not to an extent that
far below 100 nm on average was formed due to nely strength is sacriced. This semi-continuous process can
spaced, intersecting twin lamellae. This nanostructured deliver long magnesium products with very good strength
steel exhibited an excellent fatigue performance and and ductility and, as will be seen below, improved corro-
impressive thermal stability, as will be shown in the next sion resistance. It is believed to oer a promising possibility
section. Furthermore, Zhao et al. [223] showed that by for transfer of SPD processing to industrial manufacturing.
engineering very small second-phase particles into a nano- With regard to a possible explanation of the generally
structured Al alloy 7075 matrix, it was possible to double low ductility of SPD-processed materials, two concepts
its uniform elongation, while further gaining yield strength. appear to be favoured in the literature. The rst is micro-
The alloy was solution treated, cryorolled to produce nano- structurally based and builds explicitly or implicitly on
structures with an average grain size of 100 nm and then the role of dynamic recovery acting as a primary softening
aged at low temperature to introduce very small second- mechanism that reduces the strain-hardening rate. The
phase particles. The simultaneous enhancement of strength reasoning goes as follows [235]. During deformation the
and ductility was interpreted in terms of increased resis- dislocations are non-uniformly distributed among disloca-
tance to dislocation slip from second-phase particles and tion-rich areas (cell or grain boundaries, or grain
increased dislocation accumulation. A similar strategy boundary-aected zones) and areas less populated with
based on stabilization of the microstructure by uniformly dislocationsthe cell or grain interiors. Both sub-systems
distributed nanoscale precipitates was utilized earlier for tend to recover, albeit at dierent rates. The authors
estimated the recovery times for the grain interior and the can be simplied further. Routine manipulation of Eqs.
grain boundaries, which are substantially dierent. They (13) and (14) leads to a simple functional relation between
concluded that in UFG steel, unlike in coarse-grained the proof stress r0.2 (for e = 0.002) and
the uniform elonga-
one, the grain interior dislocations reach the grain bound- tion ec in the form of r0:2 / ebL
c k2
exp e2c k2 , which is in gen-
aries where they recover much faster than within the grains. eral agreement with the results presented in Ref. [239]. It is
The ensuing reduction of the dislocation density inside the also in accord with Fig. 7, showing an exponential decrease
grains in the UFG material reduces strain hardening in of r0.2 with ec for Cu specimens manufactured in dierent
comparison with the case of large grain size. ways. The above derivation was based on the assumption
The second concept exploits the mechanistic approach that dislocation-mediated mechanisms of plasticity remain
on the basis of the Considere criterion: predominant in the UFG range. Thus, most of the salient
drT features of strength and plasticity of UFG materials,
6 rT ; 11 including their response to cyclic loading, see below, are
deT
captured well by the dislocation-based model.
for the onset of macroscopic instability associated with Indeed, one can see that specimens deformed by one
necking in terms of the true stress rT and true strain eT. ECAP pass or rolled to the same equivalent strain exhibit
As the reduction of the grain size down to the sub-micron similar hardening behaviour and nearly the same critical
or nanoscale range leads to a pronounced increase in the strain for necking, ec, with just slightly dierent k2 values,
ow stress with a simultaneous drop in the capacity of close to 90 6. The second path by route A gives rise to
the material to strain-harden, the necking criterion given extension and thinning of grains, leading to a reduction
by Eq. (11) is met at small tensile strains, which means in the dislocation mean free path. The ensuing rapid hard-
low uniform elongation. It is easy to recognize through a ening raises the k2 value to 280 20. A drop in uniform
simple exercise that both concepts are essentially the same. elongation is recorded. When further straining to four
Eq. (1) is integrated analytically with the initial condition passes reduces the k2 value eectively to about 120, the uni-
q(0) = q0 and yields the dislocation density q(e) as a func- form elongation rises again, as predicted by Eq. (14).
tion of strain. The ow stress r is linear in the square root Based on the outcomes of the Considere analysis dis-
of q, as prescribed by the Taylor relation, which holds al- cussed above, Hoppel et al. [240,241], and then Wang
most regardless of the particular arrangement of disloca- et al. [239] suggested that a bimodal grain size distribution,
tions for a wide range of dislocation mechanisms: with micrometer-sized grains embedded in a sea of nano-
p crystalline and ultrane (<300 nm) grains, is conducive
re r0 MaGb qe: 12
for good ductility. In a somewhat simplistic fashion it
Solving Eq. (1) (for simplicity, for a constant L) one gets: was claimed that the nanoscale fraction of the grain popu-
r lation was responsible for high strength, while the coarse
k0
re r0 MaGb 1 ek2 e q0 ek2 e : 13 grains contributed to ductility by promoting the strain
k 2 bL
hardening necessary to stabilize the tensile deformation
Using the necking criterion expressed by Eq. (11), the crit- against strain localizations. Improved tensile ductility (up
ical strain ec at which the strain hardening rate has dropped
to the level of the applied stress is obtained as:

1 k0 2
ec ln k 2 bL k 2 q0 1 2k 0 : 14
k2 bL k0
It is obvious from this equation that ec is reduced when the
dynamic recovery rate controlled by the coecient k2 in-
creases. The parameter k2 is strain rate and temperature
dependent. In the formulation by Essmann and Mughrabi
[149,236] this phenomenological coecient is associated
with the dislocation annihilation length. In the Kocks
Mecking model it is related to dislocation cross-slip or
climb probability [144,145]. This very simple reasoning
can be extended in various ways, particularly by replacing
the Considere criterion (11) with Harts criterion, which in-
cludes the eect of the strain-rate sensitivity of the ow
stress [237,238]. In essence, however, Eq. (14) provides a
formal footing for the popular speculative argument about
the vital role of recovery and dislocation annihilation in re- Fig. 7. Experimental data illustrating the relation between the yield
strength and the uniform elongation in coarse grained (CG) and ultrane-
duced ductility of UFG metals and alloys. Besides, in the
grained (UFG) copper including the results for the samples with a bimodal
low strain limit k2e
1 when steep hardening is observed, structure produced by annealing for 1, 3 and 10 min at 200 C after ECAP
cf. Fig. 5a (stainless steel) and Fig. 6b (copper), Eq. (13) (four Bc passes). Data are compiled from Refs. [178,239,248251].
to 65% elongation to failure, and 30% uniform elongation) 4.2. Fatigue

in copper produced by cold rolling at liquid nitrogen tem-
perature, followed by an annealing treatment at a moderate For prospective engineering applications of UFG mate-
temperature, which again led to a bimodal grain size distri- rials, their cyclic properties need to be considered along
bution, was reported [239], cf. Fig. 7. A positive eect of with the strength and ductility under monotonic loading.
the bimodal structure on tensile ductility was found in sev- Improvement of fatigue properties is both very important
eral investigations, although in most cases the high strength and challenging. Whereas strength under monotonic load-
was sacriced to a degree. It is also backed by results of ing obeys the HallPetch relation extended to sub-micron
numerical simulations of the deformation behaviour of grain sizes, the 150-year history of fatigue studies has
elasticviscoplastic materials [242] (see also Ref. [243]). taught us that the cyclic stressstrain behaviour of face-
The numerical results show the impact the variance of centred cubic and body-centred cubic metals with conven-
the grain size distribution has on the mechanical response tional grain size does not exhibit a strong grain-size depen-
of a material with a bimodal grain size distribution. Not dence (see a review by Mughrabi [256]).These properties
surprisingly, the importance of the coarsest grains within were extensively studied in relation to UFG metals and sev-
the microstructure due to their lowest yield strength is eral comprehensive reviews cover this topic specically
clearly seen. This provides general guidelines for develop- [257259]. So far, most of the experimental results related
ing ne-grained materials with bimodal grain size distribu- to fatigue of UFG metals were obtained on specimens pro-
tions, suggesting that the two modes should be relatively duced by ECAP in combination with other thermomechan-
close to each other. This result is in line with the recom- ical treatments. Analysis of the currently available body of
mendations of Wang et al. [239]. After their publication, experimental data shows that the fatigue behaviour of
many researchers advocated the advantages of using UFG metals follows common trends determined by the
UFG materials with a bimodal grain size distribution for fatigue life approach based on the interplay between the
obtaining good strength and ductility. Although some strength and ductility. It can be conjectured that without
improvement of ductility cannot be denied [244], we believe loss of generality similar principles can be expected to
that the magnitude of the eect does not meet the high apply for other processing schedules. The results depend
expectations raised, and controversy still exists. For exam- on how they manage strength and ductility, as well as the
ple, Mughrabi et al. [107,245] showed that only a marginal key microstructural factor, uniformity of strain, they
improvement of the low-cycle fatigue (LCF) performance produce.
was achieved in UFG a-brass with a bimodal grain size dis- The LCF and HCF regimes are conventionally distin-
tribution, despite the systematic way in which the parame- guished on the basis of the applied strain amplitude
ters of the annealing treatment were varied. The original [257,260,261]. HCF testing corresponds to probing a mate-
data reported in Ref. [239], as well as a compilation of rials resistance to crack initiation, whereas LCF testing
new data, are presented in Fig. 7. This indicates that, con- corresponds to assessing the materials tolerance to defects
trary to the results of Wang et al. [236], the samples with in a regime when fatigue life is controlled by crack propa-
bimodal structures still follow the common trend and this gation. Combining these two regimes, the total strain range
kind of structure does not necessarily result in a substantial Det is considered as a sum of two additive components: the
increase in ductility. While bimodal structures were found elastic, Deel, and the plastic, Depl,: Det = Deel + Depl. An
in Mg alloys whose superplastic properties were boosted empirical formula relates the total fatigue life represented
by ECAP [229,232], the role of bimodality in superplastic- by the number of cycles to failure, Nf, to the strain ampli-
ity was questioned in Refs. [230,246]. The idea of structural tude, Det, as follows:
bimodality may even be counterproductive for high-cycle
Det r0f b0 c0
fatigue (HCF) properties, which are known to benet 2N f e0f 2N f : 15
strongly from a uniform grain size distribution [247]. It 2 E
can be concluded that the bimodality recipe cannot gener- Here the rst and the second terms on the right-hand side
ally be regarded as a panacea for the low-ductility malaise correspond to the elastic and the plastic components of the
of SPD-processed materials total strain, respectively; E is Youngs modulus, r0f is the
In some investigations the high ductility was attributed fatigue strength (which is believed to be related to the yield
to pre-existing growth twins in the nanostructured Cu stress or the ultimate tensile strength of the material), b0 is
[252]. The positive eect of twinned structure on ductility the Basquin exponent, e0f is the fatigue ductility coecient
and toughness is well documented [253255]. It may be and c0 is the fatigue ductility exponent, also known as the
associated with the shorter mean free path of dislocations ConManson exponent. Hence, the fatigue life under a
in such structures, giving rise to a higher strain-hardening given total strain amplitude is expressed in terms of four
capacity of the material. If twinning occurs in situ, during material parameters: e0f , r0f , c0 and b0 . Although direct
the deformation, a dynamic HallPetch eect, as men- equivalence of the parameters e0f and r0f to the tensile duc-
tioned above, can lead to a continual decrease in the dis- tility and the ultimate tensile strength, rUTS, respectively, is
location mean free path and the attendant delay of rarely observed in experiment, a correlation between these
necking. pairs of quantities does often exist. At large strain
Cu-0.75Cr, from Gadalla and Gerold (1998)

CuCrZr, Leedy et al. (1996)
600 OFHC Cu, Leedy et al. (1996)
CuNiBe BW, Leedy et al. (1996)
ECAP+aged Cu0.44Cr0.022Zr, Vinogradov et al. (2002)
ECAP Cu0.44Cr0.22Zr, Vinogradov et al. (2004)
500
Cu0.36Cr ECAP+aged
Stress Amplitude, a / MPa

Cu0.69Cr, Xu et al. (2008)
400
300
ageing effect
200
100
pure Cu
0
102 103 104 105 106 107 108
Number of Cycles to Failure, Nf
Fig. 8. The Wohler plot comparing fatigue lives and endurance limits for conventional and SPD-manufactured Cu-based alloys (CuCr and CuCrZr).
amplitudes corresponding to short fatigue lives, the plastic More troublesome are the results for LCF: regardless of
strain component is prevalent in the total applied strain the SPD technique used to produce UFG and nanostruc-
and the fatigue life is determined primarily by ductility. tured metals, they are consistently inferior in their ability
At long fatigue lives, the elastic strain amplitude is more to sustain cyclic loads at fairly large imposed plastic
signicant than the plastic one, and fatigue life is dictated strains. In line with the fatigue life approach based on
by the fracture strength, so that the endurance limit in- Eq. (15), this is rationalized in terms of lower ductility, sus-
creases with tensile strength [209,247,262]. This trend is ceptibility to strain localization in shear bands and greater
clearly seen in Fig. 7. As already discussed, in most cases availability of grain boundaries in orientations favourable
the highest strength levels are achieved at the expense of for intergranular crack propagation in a material with a
ductility (cf. Table 2). Process design aimed at enhancing ner grain structure.
fatigue properties is hindered by the fact that no commonly In some cases, however, it turns out to be possible to
accepted physically based models capable of explaining the improve both HCF and LCF performance. For example,
physical origin and predicting the values of the four param- it was demonstrated [224,225] that by combining ECAP
eters, e0f , r0f , c0 and b0 , in Eq. (15) are available to date even of several dilute CuCrZr alloys with subsequent opti-
for structurally simple pure polycrystals. mized ageing it is possible to fabricate UFG materials with
Based on the foregoing consideration, a traditional fati- superior multifunctional properties, including excellent
gue improvement strategy relies on the following correla- strength and very high endurance limit exceeding by far
tion: the higher the strength under monotonic loading, those for pure copper. Even more strikingly, the endurance
the higher is the endurance (fatigue) limit. This is certainly limit was higher than that of a representative group of
not a rm law, and the eectiveness of the strategy for highly alloyed Cu (Fig. 8). The signicant improvement
improving fatigue properties by raising the ultimate tensile of tensile strength and HCF strength observed was
strength depends on the material and the grain renement achieved without sacricing ductility and LCF properties.
process used. The most successful example of the use of this Similarly, an improvement of monotonic and fatigue
strategy in combination with SPD techniques was demon- strength was reported by Xu et al. [268] for Cu0.69Cr
strated by the group of R.Z. Valiev for Ti [208,210,263 0.05Fe0.02Ni, albeit with a markedly lower fatigue limit.
267]. Starting o from ordinary ECAP processing of CP Since the LCF performance relies on the resistance to
Ti, this group designed increasingly sophisticated strain- aws either induced during processing or created during
hardening schedules involving cold rolling, forging and/ testing, the crack growth resistance was found to follow
or drawing to convert the residual ductility after ECAP the common trends for materials exhibiting increased
into strength via further grain renement and/or disloca- strength and reduced ductility. The fatigue threshold is
tion hardening. While a materials performance under usually lower and the fatigue crack growth rate is consider-
monotonic loading is improved considerably with the grain ably higher in UFG materials as compared to their coarse-
size reduction by SPD, for many metals and alloys the grained counterparts (Fig. 9) [201,204,257,262,269271].
HCF properties, particularly the endurance limit, are not Many discussions in the literature are concerned with
enhanced to the same extent [109,201203] (cf. Table 2). the particular role of grain boundaries in the properties
of UFG materials [21]. Obviously, the interfacial energy

and higher diusivity of grain boundaries (see the next sec-
tion) cannot be disregarded for many phenomena. In fati-
gue of SPD metals, for instance, grain boundaries play a
signicant role [251,272]. On one hand, the ne-grained
structure usually gives rise to longer fatigue lifeat least
under stress-controlled cyclingthan the coarse-grained
one. On the other hand, the grain boundaries appear to
contribute to the relatively low stability of the UFG
structure and the tendency toward recovery and grain
coarsening during cycling [241] and fatigue crack growth
(cf. Fig. 9) [269]. Furthermore, grain boundaries are
believed to play a role in the frequently observed shear
banding as well as crack initiation and propagation
[251,257,262,269,273276]. Therefore grain boundaries
arguably represent the most critical structural element.
Despite the complexity of the nanocrystalline structures,
the fatigue behaviour of UFG metals can be more easily Fig. 9. Fatigue crack growth rate in UFG Cu (99.96%) and the EBSD and
described than that of ordinary polycrystals and single ECCI (Electron Channeling Contrast Imaging) map illustrating structural
instability and grain coarsening along the crack path in UFG Cu produced
crystals. The main reason for this simplication is the lack by eight ECAP passes via route Bc; fatigue thresholds are approximately
of dislocation patterning within the UFG structures since indicated by arrows. The arrow in the inset indicates the crack growth
the characteristic dimensions of the major structural ele- direction. After Ref. [269].
mentsgrains or cellsare smaller than the characteristic
length scale of dislocation structures that self-organization
during cyclic loading would induce. Vinogradov et al. pull cyclic loading. It was demonstrated that no high-angle
[109,208] suggested that in light of this argument it is sen- grain boundaries formed during a single ECAP pass;
sible to describe the shape of a stable hysteresis loop and rather, a well-developed cell structure was observed
the cyclic stressstrain curve in terms of the one-internal [279,280] in line with ideas of microstructure formation dis-
variable approach and apply Eq. (1). It was assumed that cussed in Section 3.2 and with early experimental observa-
the mobile dislocations generated at a grain boundary pass tions of fragmented structures formed during plastic
through the grain and disappear at the opposite grain deformation [136,137]. A very large strengthening eect
boundary, i.e. the grain boundaries act as eective sources comparable with that in polycrystals of the same purity
and sinks for dislocations and the grain (cell) size deter- deformed under the same conditions was achieved entirely
mines the dislocation mean free path scale. Because TEM due to dislocation storage in cell walls that gave rise to low
observations do not reveal any substantial dierences misorientation angles (incidental boundaries). Although
between the initial and the post-fatigue structures, at least old grain boundaries had no eect on the monotonic
in some UFG metals, it is plausible that in these cases dis- and cyclic strength and ductility, the r0.2, rUTS and rf val-
locations are not accumulated inside the ne grains during ues were quite high: 260, 275 and 105 MPa, respectively.
cycling. The model was tested on UFG AlMg alloy Such dislocation ensembles are not stable thermally or
AA5056 [109,208] and CP grade 2 titanium [109,208] after mechanically and tend to recover during cyclic loading.
ECAP, and it showed a surprisingly good agreement with This recovery is a root cause of a well-known cyclic soften-
experiment. Later the same model was successfully applied ing, i.e. the reduction of the cyclic stress amplitude with the
by Klemm [277] for UFG nickel after dierent processing number of cycles (Fig. 10b). The model [109,208] correctly
schedules (see also Ref. [258]). Both groups of researchers captures this feature as well.
arrived at essentially the same conclusions and obtained
very reasonable values of the slip distance L (of the order 4.3. Creep behaviour
of the grain size) entering Eq. (1) explicitly, and the annihi-
lation distance y which is implicitly hidden in k2. As an Reports on the creep behaviour of UFG materials man-
example, a typical ascending part of the stable hysteresis ufactured by SPD are still relatively scarce. Sklenicka et al.
loop of CP (grade 4) titanium in three dierent structural [282284] evaluated the roles of dierent factors aecting
states created under dierent SPD processing schedules is the creep performance of pure aluminium, pure copper
plotted in Fig. 10a. A good agreement between the model and the binary Al0.2 wt.% Sc alloy processed by ECAP.
t and the experimental data is seen (cf. [109,208]). It was found that the creep behaviour of ECAP materials
Furthermore, the model applies reasonably well to depends strongly on the number of passes, a decrease in
severely deformed copper single crystal of {1 1 0} initial the creep resistance being associated with each successive
crystallographic orientation which was pressed through a pass. This may be attributed to a number of factors,
90 ECAP die [48] (cf. [278]) and then subjected to push including microstructural changes, homogenization of the
scopic shear bands along the shear plane of the last ECAP
pass, similar to those observed during fatigue, can have an
unfavourable eect on the creep resistance. As was demon-
strated in Ref. [106], the detrimental eect of the last ECAP
step can be alleviated by manipulating the specic shear
texture induced by ECAP. This can be achieved by post-
ECAP drawing or rolling. The examples considered show
that the outcomes of SPD in terms of creep behaviour
can be very diverse, and no conclusive picture has emerged
so far. What is obvious, though, is that in many cases the
creep resistance is intimately related to thermal stability
of the microstructure.
4.4. Properties other than mechanical
4.4.1. Thermal stability

Improving several properties of a material at the same
time to provide it with the often-desired multifunctionality
is a very challenging task materials science is facing quite
generally. Strengthening often involves considerable
trade-os, as other material properties may be compro-
mised. Since strengthening is commonly a main goal and
the usual outcome of SPD-induced grain renement, it
can be expected that this occurs at the expense of some
other properties. For instance, beside tensile ductility and
fatigue behaviour discussed above, thermal stability, elec-
trical conductivity and corrosion resistance are among
the most important properties that may be at risk of being
sacriced. Depending on the material and the targeted
application, a full portrait of the properties after SPD pro-
Fig. 10. Typical ascending part of the stable hysteresis loop of (a) grade 4 cessing needs to be obtained. Unfortunately, this has rarely
titanium in two dierent structural states: ECAP followed by hot rolling been done [286].
(ECAP + HR), and ECAP followed by hot rolling and annealing for As is typical for cold-worked materials in general, ther-
30 min at 500 C (ECAP + HT + A500 C 30 min) [281]; and (b) copper
single crystal after one ECAP passthe three curves correspond to the
mal stability is an Achilles heel of many SPD-treated mate-
cycle numbers 40, 70 and 100, showing reduction in the stress amplitude rials. For example, SPD-manufactured pure oxygen-free
due to continual cyclic softening; curve ts by Eq. (13) are shown by thin copper shows relatively poor thermal stability [287,288]
lines. (even compared to copper cold-rolled to the same strain
[289]). It tends to recover during storage even at room tem-
microstructure and the microtexture and nanoporosity perature due to annihilation of excess dislocations accumu-
induced by ECAP. lated during severe straining [250] (Fig. 11a). It is seen that
High-purity aluminium processed by ECAP was tested the greater the number of ECAP passes, the faster is the
under creep conditions at 200 C in Ref. [285]. The results rate of recovery. No signicant change of microstructure
showed conventional power-law creep with a stress expo- is typically observed in SPD-manufactured copper up to
nent of n = 5, which is consistent with intragranular dislo- 120150 C, while in the temperature range between 150
cation processes involving glide and climb of dislocations. and 250 C recovery followed by recrystallization and
The results suggested that diusion creep was not impor- abnormal grain growth takes place, as seen in the micro-
tant in these tests because the ultrane grains produced graphs in the insets in Fig. 11b. One can follow the trans-
by ECAP were not stable at the test temperature. (In the formation of UFG structure into a bimodal one after
opposite case of a material whose extremely ne grain annealing at 200 C for 10 min, which then evolves to a
structure persists under service conditions and creep is con- fully recrystallized coarse-grained structure at higher tem-
trolled by diusion, e.g. by the NabarroHerring or Coble peratures. Of course, the temperature signifying loss of sta-
mechanism, its use is obviously contraindicated.) There are bility depends on the purity of copper and the amount of
reported cases when SPD processing leads to improved the imposed strain.
creep resistance. Thus, binary Cu0.02Zr alloy after ECAP Strategies towards microstructure stabilization and
exhibited a signicantly better creep resistance than its enhancement of multifunctional properties of SPD materi-
coarse-grained counterpart in the homogenized or the als align well with the general philosophy of materials
cold-rolled condition. By contrast, the formation of meso- design based on a balance between the basic strengthening
(a) Post-process annealing below recrystallization tem-

perature to relieve internal stresses increases the
work-hardening capacity, thereby improving the
overall ductility of cold-worked materials
[107,109,235].
(b) Avoiding materials that exhibit wavy slip. Thus, tita-
nium with its hcp crystal lattice shows reasonably
high thermal and microstructural stability under cyc-
lic loading, retaining its UFG microstructure up to
annealing temperatures of 450 C [290] and exhibiting
no cyclic softening during LCF [208]; see also Ref.
[291] for ECAP-processed iron.
(c) Stabilization by solutes preventing grain coarsening
by pinning of grain boundaries [47,292].
(d) Particle-induced stabilization [47,203,213].
(e) Grain boundary engineeringa concept proposed by
Watanabe [293] as a means of designing high-temper-
ature materials, which exploits the idea of higher sta-
bility of special grain boundaries with low energy.
Specically, R3 (twin) boundaries should be particu-
larly benecial for enhanced thermal stability (see
also Section 4.3.4 for further discussion). This is
clearly illustrated in Fig. 10c [294] for the SUS
316L austenitic steel nanostructured by mechanical
twinning (cf. Fig. 5), which remains stable at temper-
atures up to 500 C.
A judicious choice of materials in conjunction with opti-

mized thermomechanical treatment helps to overcome
microstructural instability, which was identied as a most
serious drawback of SPD processing. For instance, alloy-
ing of pure copper with Zr in small concentrations helps
to stabilize the UFG microstructure against thermal [244]
or mechanical (both monotonic and cyclic) inuences
[48]. Similarly, alloying with Sc provides aluminium with
stability of its SPD-induced UFG microstructure
[203,295300]. The excellent fatigue properties of the
ECAP-processed CuCrZr alloys [224225] mentioned
in the previous section may be related to their remarkable
thermal stability. Transmission electron microscopy obser-
vations showed that their ECAP-induced structure
remained ne, the grain size not exceeding 250 nm even
after heating to temperatures up to 600 C. Grain growth
was obviously suppressed due to nanoscale CuZr precipi-
tates at the grain boundaries [224,225]. Grain coarsening
set in only at temperatures as high as 650700 C. A similar
Fig. 11. Thermal stability of ECAPed (eight Bc passes) copper (99.96%) (a result was reported for a CuZr alloy in Ref. [301].
and b) and SUS 316L stainless steel (c). (a) Reduction of Vickers
microhardness during natural ageing of UFG Cu sample at room
4.4.2. Diusion properties
temperature for 1 year; (b) the eect of annealing on the grain size; (c)
Vickers hardness of the SUS316L steel after one ECAP pass and annealing It is intuitively obvious that grain renement by SPD
for 1 h. should lead to enhanced atomic transport. Indeed, SPD
promotes fast short-circuit diusion through an increased
mechanismsgrain renement, strain hardening, solid- volume fraction of grain boundaries and a higher disloca-
solution hardening and precipitation hardeningand tion density in the processed material. It is not obvious a
stress relief or recovery. As applied to UFG metals, the fol- priori, however, whether the eect of grain renement is
lowing measures have proven to be eective for this restricted just to this increased availability of fast diusion
purpose. pathways, or the diusivity for the short-circuit paths itself
changes upon SPD processing. There is some controversy boundaries occurs, which retards their diusion. By con-
in literature about this issue, as both nearly unaltered trast, for Ag atoms, which migrate by substitutional diu-
[302] and enhanced [303,304] grain boundary diusivities sion, SPD-induced grain boundary defects boost the
were found in SPD-processed materials. The complexity diusion along non-equilibrium grain boundaries.
of singling out the contribution of grain boundaries from The studies by the same group revealed furthermore
the overall diusivity is compounded by the fact that old, that, in addition to the more conventional, grain-bound-
equilibrium grain boundaries coexist with non-equilib- ary related, fast diusion paths, some new, ultra-fast
rium ones [305307], freshly produced by SPD. Such short-circuit paths specic for UFG materials produced
non-equilibrium grain boundaries possess a higher energy by SPD may also exist. It was initially assumed that the
and a larger excess free volume, which is believed to lead ultra-fast diusion channels were associated exclusively
to higher diusivities than those of equilibrium grain with the non-equilibrium grain boundaries [308,312]. This
boundaries in well-annealed coarse-grained materials. idea was later disproved [311,312,314], as evidence had
The research group of Wilde and Divinski in Munster emerged that a long-range network of interconnected
did a lot to shed light on the specics of diusion in nano- and micropores created by SPD and residing pre-
SPD-processed materials. Based on their thorough radio- dominantly at non-equilibrium grain boundaries and tri-
tracer measurements [308312], a hierarchy of short-circuit ple junctions gives rise to ultra-fast diusion [310,311].
diusion paths in UFG materials produced by SPD was An example of such pore structure in ECAP-deformed
experimentally established. It was suggested that alongside Cu is shown in Fig. 12. It should be noted that no such
relaxed (equilibrium) high-angle grain boundaries, there percolating porosity was found in Ni deformed by
exist interfaces with signicantly higher diusivities. The room-temperature ECAP and the ultra-fast diusion
enhanced diusion rates for solute and self-diusion in observed is believed to be governed by a specic non-
UFG materials prepared by SPD were attributed to the equilibrium state of the SPD-induced grain boundaries
non-equilibrium state of the grain boundaries [267]. [315].
However, the most recent study [313] showed that this is The occurrence of nano- and micropores as a conse-
not universally true. Rather, the eect of SPD processing quence of SPD processing may appear worrisome, but
was shown to be selective: grain boundary diusivity of the levels of porosity in question are extremely low, about
Co in ECAP-modied Ti was slower than in coarse-grained 2 ppm [312]. The mechanical properties of SPD-treated
Ti, in contrast to accelerated grain boundary diusivity of materials do not seem to suer from it anyway. It should
Ag atoms in Ti. This is an indication that for interstitially be mentioned that nanopores dispersed in the bulk are very
diusing Co atoms trapping or scattering due to high con- ecient obstacles to dislocation motion, so that their pres-
centration of lattice defects within non-equilibrium grain ence may be adding to strength.
Fig. 12. SEM micrographs of ECAP-processed copper obtained by eld ion beam milling at dierent locations around a triple junction. The locations are
indicated by the coloured lines; the corresponding micrographs are provided within a frame of the same colour. The grain boundaries (assumed to be SPD-
induced, non-equilibrium ones) are visible through thermal grooves formed on them. Also seen are micro- and nanopores at grain boundaries. Note that
the 1 lm scale bars have dierent lengths in the micrographs (a), (b) and (c). (Adapted from Ref. [309].) (For interpretation of the references to colour in
this gure legend, the reader is referred to the web version of this article.)
With the mentioned exception of interstitial diusion ing may appear surprising in view of the general concern
being slowed down, SPD can be generally considered to that grain boundaries are regions with high excess energy
enhance diusion of solutes as well as self-diusion. It that act as preferred sites for corrosion attack.
can thus be expected that kinetic properties of metals and The abundance of grain boundaries as preferential sites
alloys that involve diusion will be accelerated as a result of attack by corrosive media increases the propensity of an
of SPD. Conrmations of this general expectation can be UFG material to undergo intergranular cracking in the
seen in the acceleration of such processes as plasma nitrid- low-strain-rate SCC tests. This is compounded by a higher
ing of steels [316] and hydrogen sorption in magnesium dislocation density in SPD-processed materials. Despite
alloys [317]. The latter eect will be presented below. these negative factors, the corrosion damage on the surface
of UFG copper turns out to be rather uniform at the mac-
4.4.3. Corrosion resistance roscale, whereas obvious attack at grain boundaries and
Another property of great interest for prospective engi- selective corrosion of some grain interiors were observed
neering applications is corrosion resistance. Corrosion in in coarse-grained copper.
single-phase polycrystalline aggregates is greatly inuenced These rst observations were later conrmed by dier-
by grain boundaries and their area, which is determined by ent researchers who found enhanced (or at least not
the grain size. Normally one would expect that any reduced) corrosion resistance of UFG Cu [324325], Al
strengthening mechanism involved in SPD processing and a variety of Al-alloys [318,326328], titanium [329],
should deteriorate the corrosion behaviour of a defect-free interstitial-free steel [330], austenitic stainless steels 316L
single-phase metal. Indeed, at rst glance both the SPD- [331] and 304 [332], FeCr [333], Mg [334] and Mg-based
induced structural inhomogeneities leading to local dier- alloy ZK60 [335]. The improvement in corrosion resis-
ences in the surface potential [318] and the higher reactivity tance of ZK60 by the integrated extrusion + ECAP pro-
of grain boundaries intersecting the surface of an UFG cess (Table 1l), was interpreted in terms of two factors:
material could promote its degradation in a corrosive grain renement and the redistribution of Zn and Zr sol-
medium. utes within the microstructure. These microstructural
The nature of environmental degradation of metals and changes impacted on the anodic and cathodic reaction
alloys is a multidisciplinary subject, which should be stud- kinetics of corrosion in a favourable manner, through
ied with respect to many aspects, including the three major both structural and chemical variations. A detailed under-
ones: corrosion (chemical, electrochemical, pitting, etc.), standing of the enhanced corrosion resistance observed
stress corrosion cracking (SCC) and corrosion fatigue. To for several SPD processed materials is, however, lacking,
the best of our knowledge, the only material which has and this area denitely requires the attention of corrosion
been investigated with regard to all these aspects is scientists.
ECAP-processed copper [319323]. A general encouraging In contrast to coarse-grained copper specimens showing
conclusion obtained in these rst investigations is that a transgranular fracture when immersed in an aggressive
SPD, while enhancing mechanical characteristics, does liquid during SCC or fatigue deformation, the fracture of
not compromise the overall corrosion resistance and UFG specimens occurred intergranularly under the same
improves the SCC and corrosion fatigue resistance. More- conditions. This shows the dominant role grain boundaries
over, the homogeneity of corrosion damage of UFG Cu, played in the latter case. While it is true also for this case
which contrasts the localized intergranular corrosion in that increasing aggressiveness of a corrosive environment
coarse-grained Cu polycrystals (cf. Fig. 13a and b), is seen reduces the fatigue resistance, the observations in Ref.
as an advantageous property of ECAPed copper that [321] demonstrated that the bulk microstructure, which is
makes it attractive for engineering applications. This nd- reected in the surface properties, is a major factor
Fig. 13. SEM micrographs showing the surface morphology of ECAP copper after potentiostatic tests in a modied Livingston etchant: (a) UFG state
after ECAP and (b) a coarse-grained state after annealing at 823 K for 30 min. (After Ref. [319]).
governing the damaging eect of the environment and the e.g. for bone or tooth replacement, obviously need to be
degree of degradation under load. as inert in bodily uids as possible, those for temporary
As mentioned above, the grain boundaries act as sites of implants must degrade at a rate suitable for the targeted
preferential corrosion attack because of their imperfect application. Two archetypal alloy systemsthose based
atomic arrangement giving rise to increased local energy, on titanium and magnesiumare the favourites in these
higher excess volume, and stresses. Furthermore, the corro- two respective categories.
sion resistance is very sensitive to the grain boundary type. In the case of permanent implants, titanium alloys, par-
Thus, grain boundaries having low energy, such as special ticularly Ti6Al4V, have dominated the market for dec-
boundaries with low reciprocal coincident site lattice ratio ades. Titanium-based implants owe their great popularity
R (R3, R7, etc.), are particularly resistant to corrosion to a very favourable combination of properties. These
[336]. Following the above-mentioned concept of grain include a high corrosion resistance due to the protective
boundary engineering [286], micro- and nanostructures surface layer of titania they form, reasonable bioinertness,
with the majority of energetically stable R3 boundaries high strength-to-weight ratio and very good fatigue resis-
were articially produced by mechanical twinning during tance. An obvious choice for bioresorbable metallic
smooth [189] or violent [337] processing, and these implant material is magnesium, which is highly biodegrad-
structures are considered to be benecial for sustained able. There is a huge literature on the medical implant
resistance against corrosion. applications of these materials, which we are not going
to review here. Our goal is much narrower: a discourse
4.4.4. Biocorrosion properties on the suitability of SPD processing for improving the
As one of the prospective uses of SPD-processed UFG properties of Ti and Mg relevant to medical implant
materials is in biomedical implants (see below), their corro- applications.
sion behaviour in bodily uids has become a vigorously Current research focuses on improving the biocompati-
growing research area. For brevity, we can only oer some bility and the mechanical performance of these systems
sketchy glimpses of this research. through variations in alloy composition, microstructure
The biocorrosion properties of severely deformed CP and surface treatment. In the case of titanium, a target is
titanium was shown to be similar to [338] or better than to improve the strength characteristics of CP grades, which
[339,340] those of its coarse-grained counterpart. Of could replace currently used alloys, thus avoiding potential
course, it should not be forgotten that this occurs against biotoxicity of the alloying elements. If CP titanium is ever
the background of the hugely enhanced mechanical to replace Ti alloys, the decit of strength in the unalloyed
strength of the material. material will have to be compensated for. As discussed
Whereas improved corrosion resistance of ECAP-modi- above, this can be readily achieved by SPD. ECAP [346],
ed copper was reported by several authors for salty or twist extrusion [63], helical rolling [101] and other SPD
acidic media [323,341], Xu et al. observed an increase in techniques are well suited for this purpose. Microstructure
corrosion current in a simulated body uid [342]. They sug- modication of CP titanium by ECAP was shown to be
gested that this property of ECAP-modied copper could very ecient [347349], with average grain sizes of 250
be used in intrauterine contraceptive devices. 300 nm being achieved, and tensile strengths and HCF
Making a virtue of necessity and putting the high reac- endurance limits (depending on the Ti grade used)
tivity of magnesium to service, numerous researchers are approaching the levels for conventional Ti6Al4V. A sur-
working on the development of biodegradable Mg alloys prising by-product of ECAP is that the response of the
[343]. A critical review of current methodologies and their living cells to the surface of CP titanium after extreme grain
limitations can be found in Ref. [344]. Low corrosion resis- renement in the bulk is aected positively, resulting in
tance is, of course, essential in bioresorbable Mg-based increased adhesion and growth. This was found by
implants (e.g. bone implants or vascular stents), but the in vitro assays with broblast cells [347,348], pre-osteoblast
excessively high rate of degradation, which is accompanied cells [349,350] and human bone marrow-derived mesenchy-
by hydrogen evolution, is a hindrance to the use of mal stem cells [351]. On the negative side, it was found that
uncoated Mg implants. Fortunately, SPD dampens the bacterial growth on the surfaces of ECAP-modied CP Ti
degradation rate of Mg and its alloys, especially in the early is also enhanced [352,353]. Evidence that the surface mor-
stages of exposure to body uids, while improving their phology, including nanoroughness, may be a major gov-
mechanical performance [345]. erning factor in cell attachment and proliferation is
rming up [351,354]. However, many other factors may
4.4.5. Biocompatibility of SPD-processed materials also be responsible for these phenomena, including hydro-
Contemporary development of metallic implant materi- philicity, surface chemistry, texture [355], etc., and the
als is driven by the need for improved mechanical perfor- mechanisms of enhanced bioactivity of the ECAPed CP
mance of biomedical implants, while fullling demanding Ti have yet to be unravelled. In addition, machining and
biocompatibility requirements. Dierent paradigms govern subsequent surface treatment involved in implant manufac-
this development for permanent and temporary (bioresorb- turing may change these factors dramatically, and it is not
able) implants. While materials for permanent implants, known whether the benets of bulk grain renement for
cellular response will survive such surface-modifying as sinks for radiation-induced point defects, is signi-
processes. cantly increased by grain renement. Interplay between
The potential for using Mg alloys in bioresorbable vas- rapid healing of radiation eects due to an abundance
cular stents or bone implants is currently attracting huge of closely spaced sinks for point defects and segregation
interest [356,357]. A major challenge is the excessively high of solutes to grain boundaries is quite complex, however.
rate of degradation of these materials, which is problematic Atom probe evidence for grain boundary segregation of
both in terms of the durability of the implant and the high Si and Ni induced by ion irradiation of 316L austenitic
rate of hydrogen evolution during corrosion, e.g. in vascu- stainless steel nanostructured by HPT was reported by
lar stent applications. As discussed above, the biodegrada- Pareige et al. [356] and Etienne et al. [359,360]. The pos-
tion of Mg and Mg alloys can be manipulated by SPD. sibility to manipulate the kinetics of irradiation damage
What can be stated safely at this stage is that enhancement and potentially suppress such unwanted phenomena as
of mechanical performance (particularly, the fatigue char- swelling, radiation creep, etc., in nuclear materials by
acteristics) can be achieved with Mg alloys by such pro- controlled grain renement by SPD opens up exciting
cesses as ECAP without a loss (or even with some new opportunities in nuclear power plant development.
increase) in their resistance to biocorrosion [358]. However, Compelling evidence that radiation tolerance of UFG
bulk grain renement does not seem to be sucient to materials is higher than that of the coarse-grained ones
reduce the biocorrosion rate to the levels required by clin- has begun to crop up [361363]. More work in this area
ical needs. A tractable way to contain corrosion of Mg and is required in order to develop ecient SPD processing
achieve controllable corrosion rates will most probably be routes leading to controlled improvement of radiation
by surface modication, particularly through smart coating damage tolerance of structural materials.
design. Possible interactions between the surface treatment
and the ne granularity of the SPD-processed Mg alloys 4.4.7. Hydrogen sorption kinetics
should be an interesting subject for research. Magnesium and its alloys are attractive materials for
Development of metallic materials for bioimplants and hydrogen storage due to their high storage capacity and
medical devices is currently a buoyant area of research with the reversibility of hydrogen absorption/desorption.
the promise of technological, commercial and societal ben- Unfortunately, the kinetics of hydrogen absorption and
ets. Bulk and surface modication by SPD is a scienti- desorption are too slow, which hinders practical applica-
cally challenging and potentially rewarding avenue to tion. A way to change both the kinetics and the thermody-
achieving better manufacturability and improved proper- namics of hydrogen storage by SPD was rst proposed by
ties of the targeted products. Skripnyuk et al. [317] who observed a pronounced
enhancement of hydrogen desorption rate in Mg alloy
4.4.6. Radiation tolerance ZK60 upon ECAP (Fig. 14). A recent publication reported
A further benet of SPD-processed UFG materials is an even greater acceleration of hydrogen desorption in
the greater radiation tolerance they may oer. This can ZK60 after ECAP [115]. The success of this approach
be expected, as the area of grain boundaries, which act prompted further studies [129,131,352,364].
The group of Horita investigated the eect of HPT on
hydrogen storage in pure Mg and also found that the
hydrogenation rate can be increased substantially
[365,366]. Further studies employing HPT [367370] con-
rmed the benecial eects of grain renement by SPD
on hydrogen storage capacity or the sorption kinetics, or
both. HPT processing also proved to be eective in enhanc-
ing the sorption of MgH2 powders [368].
With more and more experimental data on the eect of
SPD processing on the thermodynamics and kinetics of
hydrogen sorption in Mg and Mg alloys becoming avail-
able, the time has come to develop a better understanding
of the physical mechanisms underlying these eects.
4.4.8. Further functional properties

There is hardly a physical property of a solid that is not
aected by extreme grain renement down to the submi-
Fig. 14. Accelerated hydrogen desorption kinetics in Mg alloy ZK60 after cron range. Despite the long history of SPD processing,
ECAP. Filled circles represent the data points for ZK60 after ECAP or
the many possible eects are still largely unexplored, and
combined high-energy ball milling (HEBM) and ECAP [317]; open
triangles correspond to coarse-grained ZK60. The solid line represents the there may be some hidden treasures to be uncovered out
hydrogen desorption kinetics for ZK60 after ECAP using the processing there. We briey mention some eects that have recently
schedule reported in Ref. [115]. been discovered.
There is evidence that magnetic properties are aected inversely proportional to the electrical resistivity and
by SPD. Examples of coercivity measurements in thermal conductivity. Potentially, HPT can increase the
HPT-processed Fe, Ni, Fe17Co, Fe3Si and Fe6.5Si thermopower and reduce the thermal conductivity. This
[113] show that the decrease in coercivity with decreas- needs to be done in such a smart way that these benecial
ing grain size in the nanorange, which should follow eects are not outstripped by a simultaneous increase in
the d6-law, is actually much slowermost probably as the electrical resistivity. The case of HPT-deformed
a result of the severe deformation the materials have thermoelectric compounds with skutterudite structure
undergone. studied by the Vienna group [376] is a demonstration
A marked inuence of SPD processing on the properties that this strategy may work. In this rst exercise the
of shape memory alloys was observed by a number of increased electrical resistivity due to microcrack forma-
researchers (e.g. [114,233,371,372]). A summary of these tion did not, however, produce an overall increase in
eects is given in Ref. [113]. As was found in a recent the gure of merit. The most recent publication of the
study [373], ECAP of NiTi shape memory alloy can same group [377] reports further improvements in the g-
improve its strength without aecting the transforma- ure of merit for skutterudite Sr0.07Ba0.07Yb0.07Co4Sb12,
tion temperature. A big increase (by 80%) in the actu- mainly due to substantially reduced thermal conductiv-
ation stress was demonstrated, which is of signicance ity. The problem with HPT-induced microcracks,
for applications in miniaturized devices where high actu- however, still remains. The challenge now is to nd
ation stresses are at a premium. suitable processing conditions that would suppress the
An ultrane grain structure and a high density of dislo- occurrence of microcracks.
cations and point defects generated by SPD inevitably
diminish the thermal conductivity [374] as well as the
electrical conductivity [375]. This is bad news for Cu, 5. Discussion and outlook
Cu alloys and other conductors, as the intention behind
SPD processing is to raise their mechanical strength with In the foregoing sections we presented a brief history of
only moderate loss of conductivity. Post-processing, SPD techniques as a means of producing UFG materials,
including annealing, helped to restore a large part of gave a summary of the existing methods and looked into
the lost conductivity up to acceptable values (>75% of the mechanism-based models that describe the material
International Copper Annealed Standard IACS) behaviour during SPD. The intention was to give the
[225,375], but this was based on a rather empirical reader an overview of the subject and to oer insights in
approach. A lot more needs to be done to provide guid- the mechanisms underlying SPD as well as the unusual
ance for rational process optimization. As an aid in eval- material properties that can be achieved by SPD process-
uating the magnitude of the possible eect of the SPD ing. We hope that this expose will serve as an introduction
on thermal conductivity, we refer to a simple model and a reference for the uninitiated, while also presenting
[374], which relates the thermal conductivity j of the our views on this area to those specializing in nanoSPD.
processed UFG material to that of the unperturbed bulk We also hope that through this exercise we were able to
material, jbulk: show that the microcosm of the specic scientic challenges
this area is facing reects the fundamental problems of the
1 physical theory of strength and plasticity at large. We tried
4k
j jbulk 1 : 16 to highlight these challenges throughout the manuscript,
3xd1 r
within the context of the particular subjects discussed,
Here k is the electron mean free path and r is the elec- and are not going to list them here again. However, the
tron reectivity, which accounts for the fact that the most salient ones will be recapitulated below. An attempt
electrons reected from a grain boundary do not con- at predicting where the nanoSPD research may be heading
tribute to heat transfer. Finally, x (which is smaller than in the future will also be made.
unity) is a shape factor accounting for the grain topol- First and foremost, in our view the question of how dis-
ogy. This formula was shown to describe the grain size locations organize themselves in characteristic patterns,
dependence of the thermal conductivity of ECAPed cop- such as dislocation cell structures, and how these structures
per very well. evolve in the process of straining, is largely unresolved. In
particular, a comprehensive theory of the transformation
SPD processing of thermoelectric materials gives prom- of the dislocation cell structure into a new grain structure
ise as a potentially viable strategy for raising the gure with a large proportion of high-angle grain boundaries
of merit that characterizes the eciency of a thermo- needs to be developed. Such a theory should provide
electric material and its suitability for applications in insights in the mechanisms and governing factors that
thermoelectric generators. As these materials are com- determine the smallest achievable grain size. Ideally, this
monly very brittle, HPT appears to be the only SPD tech- will be a probabilistic theory able to predict grain size
nique suitable for processing them. The gure of merit is and misorientation angle distributions and their variation
proportional to the square of the thermopower and with strain for dierent deformation paths. The models
to be developed will have to possess the predictive power to Understanding the mechanisms through which functional
adequately represent the strain hardening and texture evo- properties can be aected by SPD processing and identify-
lution during SPD processing, while also providing a reli- ing promising applications in this space pose interesting sci-
able basis for simulations of the post-SPD performance entic problems and challenges.
of the processed material under service conditions. Under- The greatest expectations are being placed in achieving
standing the nature of dislocationgrain boundary interac- superior mechanical properties of structural materials.
tions for small grain size systems and the role of grain Despite a steady growth of the SPD research area and
boundaries as sinks and sources of dislocations is a partic- the promise it oers, an overly cautious attitude towards
ularly interesting goal of research. this group of processing techniques has until recently pre-
It would be nave, of course, to believe that an all- vailed in the metal-forming industry. There are various rea-
embracing model of SPD based on dislocation dynamics sons for this, one of them being the degree of overpromise
is feasible. As indicated above, a distinction needs to be of the benets of SPD processing in the past two decades.
made between the case when a dislocation cell structure Now that this research has matured, the situation is chang-
formed early on transforms smoothly to the nal, smal- ing, and there are real and tangible applications of SPD
ler-scale grain structure and the situations when a violent processing ready to be picked up by industry. Manufactur-
(high-Z) deformation process breaks down the grain struc- ing of biomedical implants, where commercial products
ture to a ner one. It is yet to be explored whether amor- have emerged recently, is a market-ready area par excel-
phization of the material on the way to a nal structure lence [378]. Nevertheless, the challenge of providing com-
is a necessary prerequisite for the formation of nanostruc- pelling and persuasive arguments to promote SPD
ture. Experimentation with such demanding deformation technologies still remains.
paths supported by modelling and atomistic simulations In addition to such psychological barriers to taking SPD
may reveal interesting possibilities for nanostructuring. processing from the laboratory to the shop oor, there are,
There are a number of concepts which have established of course, real technological challenges, such as the need
a rm place in the literature on nanoSPD materials, but for for upscaling the processes and making them continuous
which a thorough justication is missing. This refers, in or semicontinuous. Some examples of processing routes
particular, to the widespread belief that grain boundary of this kind, which promise successful transfer to indus-
sliding may become a predominant mechanism of deforma- trial-scale manufacturing [111,121,128,129,379], were given
tion of SPD materials. Indeed, the increased strain-rate in this review.
sensitivity of ow stress often found in severely deformed SPD methods that were initially developed for process-
materials suggests that grain boundary sliding or other dif- ing of bulk materials as an extension of conventional met-
fusion-controlled mechanisms may contribute to their plas- alworking techniques can also be used for other purposes,
ticity. However, there is no solid evidence that such such as ecient compaction of powders [380], particularly
deformation mechanisms are prevalent. Another concept for producing alloys from blended elemental powders [381],
that warrants scrutiny is that of bimodality of the grain and swarf [112,382]. We also expect that SPD techniques
structure being responsible for a good balance between targeting improvement of surface, rather than bulk, prop-
strength and ductility. There are indications that this may erties will experience a period of growth. In particular, in
be so, but a strict relationship between improved the spirit of an eighteenth-century aphorism by George
strengthductility balance and the occurrence of a bimodal Christoph Lichtenberg that the most important things
grain structure cannot be considered as proven. are done through tubes, we see great opportunities in
An exciting area of research is the possible link between nanostructuring of tubes by SPD methods [96,114,115].
surface and bulk properties of SPD-treated materials. The An attractive new application of SPD processing, which
enhancement of corrosion resistance and cell attachment should give new life to mature SPD methods, was sug-
and proliferation discussed in the previous section are in gested in Ref. [383]. It was proposed to produce simulta-
the category of surface phenomena aected by this link. neous architecturing and nanostructuring of hybrid
It is fair to say that the mechanisms for these phenomena materials by using established SPD techniques. In particu-
are not understood, which calls for more research on the lar, twist extrusion, HPT and some newer methods appear
subject. Of particular interest is the interaction of bulk suitable for producing a range of spiral architectures bene-
nanostructured metals with the living matteran area that cial for strength and ductility. This eld is an excellent
may be full of surprises and exciting opportunities. playground for creative materials and process design, and
Further unusual eects may be expected from the appli- we predict an exciting future for it.
cation of SPD techniques to modify various physical or
physicochemical properties of functional materials. The Acknowledgements
exemplary studies mentioned in this article (including the
eects of SPD treatment on shape memory eect, hydrogen Useful comments by Sergey Divinski on the eect of
sorption, magnetic and thermoelectric properties, etc.) SPD processing on diusion are gratefully acknowledged.
have possibly just scratched the surface of a hidden gold- One of the authors (A.V.) wishes to thank the Russian
mine of opportunities in terms of improving properties. Ministry of Education and Science and MEXT, Japan,
for partial support of research in this eld through grants- [38] Segal VM. Mater Sci Eng A 1999;271:322.
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Acta Materialia 61 (2013) 782817

Extreme grain renement by severe plastic deformation: A wealth

Keywords: Severe plastic deformation; Ultrane-grained materials; Modelling; Properties

(b)High-pressure torsion (HPT) eeff N p23 prt [34]

(c) Accumulative roll bonding (ARB) eeff N p23 lntt0 [54]

(d) Multi-axial forging eeff N p23 lnab [57]

(continued on next page)

(h) Cyclic extrusioncompression eeff N 4 lnDd [75]

(i) Cyclic close-die forging (CCDF) eeff N p23 lnWH [76]

(k) Repetitive corrugation and eeff N p43 lnr0:5t

(m) Parallel channel ECAP (PC- ECAP equivalent [67]

(p) Continuous conned strip [122]

(q) Continuous repetitive corrugating [73]

(r) Incremental ECAP (I-ECAP) [126]

(s) Continuous high-pressure torsion [127]

(t) Continuous manufacturing [129]

AlMg alloy AA5083 and interstitial-free steel, and was

modication of the CONFORM method for processing of

the demand for advanced high-performance structural dq k 0

Non-age-hardenable AA5052 (Al 2.6Mg [388] H38 255 290 7

Age-hardenable AA6061 AlMg O 150 270 48 40**

Ti (grade 2) CR 380 460 26 240

Ti (grade 4) [265] CR 530 700 25 350***

Au (K24) [47] O 133 80

08Kh18N10T stainless steel [403] HR, Q 1050 C 319 623 62

Based on 5 108 cycles to failure.

It is evident that the uniform elongation does not com-

300 300 rolling

200 rolling 200

to 65% elongation to failure, and 30% uniform elongation) 4.2. Fatigue

Cu-0.75Cr, from Gadalla and Gerold (1998)

Stress Amplitude, a / MPa

of UFG materials [21]. Obviously, the interfacial energy

4.4. Properties other than mechanical

4.4.1. Thermal stability

(a) Post-process annealing below recrystallization tem-

A judicious choice of materials in conjunction with opti-

4.4.8. Further functional properties

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