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Severe plastic deformation (SPD) process for


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Article in CIRP Annals - Manufacturing Technology · December 2008


DOI: 10.1016/j.cirp.2008.09.005

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CIRP Annals - Manufacturing Technology 57 (2008) 716–735

Contents lists available at ScienceDirect

CIRP Annals - Manufacturing Technology


journal homepage: http://ees.elsevier.com/cirp/default.asp

Severe plastic deformation (SPD) processes for metals


A. Azushima (1)a,*, R. Kopp (1)b, A. Korhonen (1)c, D.Y. Yang (1)d, F. Micari (1)e, G.D. Lahoti (1)f,
P. Groche (2)g, J. Yanagimoto (2)h, N. Tsuji i, A. Rosochowski j, A. Yanagida a
a
Department of Mechanical Engineering, Graduate School of Engineering, Yokohama National University, Yokohama, Japan
b
Institute of Metal Forming, RWTH Aachen University, Aachen, Germany
c
Department of Materials Science and Engineering, Helsinki University of Technology, Espoo, Finland
d
Department of Mechanical Engineering, KAIST, Deajeon, Republic of Korea
e
Department of Manufacturing and Management Engineering, University of Palermo, Palermo, Italy
f
Timken Research, The Timken Company, Canton, OH, USA
g
Institute for Production Engineering and Forming Machines, University of Technology, Darmstadt, Germany
h
Institute of industrial Science, The University of Tokyo, Tokyo, Japan
i
Department of Adaptive Machine Systems, Graduate School of Engineering, Osaka University, Osaka, Japan
j
Department of Design, Manufacture and Engineering Management, University of Strathclyde, Glasgow, United Kingdom

A R T I C L E I N F O A B S T R A C T

Keywords: Processes of severe plastic deformation (SPD) are defined as metal forming processes in which a very
Forming large plastic strain is imposed on a bulk process in order to make an ultra-fine grained metal. The
Metal objective of the SPD processes for creating ultra-fine grained metal is to produce lightweight parts by
Strain
using high strength metal for the safety and reliability of micro-parts and for environmental harmony. In
this keynote paper, the fabrication process of equal channel angular pressing (ECAP), accumulative roll-
bonding (ARB), high pressure torsion (HPT), and others are introduced, and the properties of metals
processed by the SPD processes are shown. Moreover, the combined processes developed recently are
also explained. Finally, the applications of the ultra-fine grained (UFG) metals are discussed.
ß 2008 CIRP.

1. Introduction fine grained metals. It is known that the metals produced by these
processes have very small average grain sizes of less than 1 mm,
Processes with severe plastic deformation (SPD) may be defined with grain boundaries of mostly high angle mis-orientation.
as metal forming processes in which an ultra-large plastic strain is The ultra-fine grained metals created by the SPD processes
introduced into a bulk metal in order to create ultra-fine grained exhibit high strength [23–25], and thus they may be used as ultra-
metals [1–7]. The main objective of a SPD process is to produce high strength metals with environmental harmony. The yield
high strength and lightweight parts with environmental harmony. stress of polycrystalline metals is related to the grain diameter d by
In the conventional metal forming processes such as rolling, the following Hall–Petch equation:
forging and extrusion, the imposed plastic strain is generally less
than about 2.0. When multi-pass rolling, drawing and extrusion s Y ¼ s 0 þ Ad1=2 (1)
are carried out up to a plastic strain of greater than 2.0, the
thickness and the diameter become very thin and are not suitable where s0 is the friction stress and A is a constant.
to be used for structural parts. In order to impose an extremely Eq. (1) means that the yield stress increases with decreasing
large strain on the bulk metal without changing the shape, many square root of the grain size. The decrease of grain size leads to a
SPD processes have been developed. higher tensile strength without reducing the toughness, which
Various SPD processes such as equal channel angular pressing differs from other strengthening methods such as heat treatment.
(ECAP) [8–11], accumulative roll-bonding (ARB) [12–14], high The relationship between proof stress and grain size of pure
pressure torsion (HPT) [15,16], repetitive corrugation and straigh- iron is shown in Fig. 1 [6]. The proof stress changes inversely with
tening (RCS) [17], cyclic extrusion compression (CEC) [18], torsion the square root of the grain size, following the Hall–Petch
extrusion [19], severe torsion straining (STS) [20], cyclic closed-die relationship. It is seen that the proof stress of the ultra-fine
forging (CCDF) [21], super short multi-pass rolling (SSMR) [22] grained irons, with sub-micrometer grains, is five times greater
have been developed. than commercially pure iron. Thus, the conventional structural
The major SPD processes are summarized in Table 1 with metals with ultra-fine grains are lighter due to their high strength.
schematic configurations and the attainable plastic strain. ECAP, Since pure iron does not contain harmful elements, it is in harmony
ARB and HPT processes are well-investigated for producing ultra- with a clean environment. Moreover, the improvements of the
superplasticity, corrosion and fatigue properties of metals
processed by SPD are expected. On the other hand, the ultra-fine
* Corresponding author. grained metals are available only for micro-parts [26,27].

0007-8506/$ – see front matter ß 2008 CIRP.


doi:10.1016/j.cirp.2008.09.005
A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735 717

Table 1
Summary of major SPD processes

Process name Schematic representation Equivalent plastic strain

Equal channel angular extrusion (ECAE) (Segal, 1977) e ¼ n p2ffiffi3 cotð’Þ

High-pressure torsion (HPT) (Valiev et al., 1989) e ¼ gpðrÞffiffi3 , g ðrÞ ¼ n 2pt r

 
t0
Accumulative roll-bonding (ARB) (Saito, Tsuji, Utsunomiya, Sakai, 1998) e ¼ n p2ffiffi3 ln t

In Fig. 2 [28], the mechanical properties of a wire specimen properties of metals processed by SPD processes are shown
made by SPD is plotted against the ratio of wire diameter D to the in Section 3, the combined processes developed recently are
grain size d, D/d. The proof stress decreases with decreasing D/d explained in Section 4, and the applications of the ultra-fine
when D/d is less than 100. In particular, when D/d is less than 5, the grained metals are discussed in Section 5.
proof stress decreases abruptly with decreasing D/d. From these
observations, the ratio of D/d must be greater than 100 in order to 2. SPD processes
guarantee the safety and the reliability of metals for micro-parts.
This paper reviews the severe plastic deformation processes 2.1. Equal channel angular press (ECAP) process
to create metals with ultra-fine grains. In the following, the
fabrications of the SPD processes are shown in Section 2. Then, the 2.1.1. Conventional ECAP processes
Fig. 3 shows the schematic representation of side extrusion
processes, which are a kind of double axis extrusion or side
extrusion [29]. Fig. 3(d and e) indicates the process in which pure
shear deformation can be repeatedly imposed on materials so that
an intense plastic strain is produced with the materials without
any change in the cross-sectional dimensions of the workpiece.
These processes are named as ECAE (Equal channel angular
extrusion) or ECAP.
Segal [8,30] proposed this process in 1977 in order to create an
ultra-fine grained material. Although ECAP is generally applied to
solid metals, it may also be used for consolidation of metallic
powder. Kudo and coworkers [31] employed repetitive side
extrusion with back pressure to consolidate a pure aluminum
powder. In the 1990s, developments of ultra-fine grained materials
were carried out with this method by Valiev et al. [9,10,32], Horita
and coworkers [33–45] and Azushima et al. [46–48] and others
Fig. 1. Relationship between proof stress and grain size of pure iron [6]. [49–51].
The schematic representation of the ECAE process is shown in
Fig. 4. The specimen is side extruded through the shear
deformation zone with the dead zone in the outer corner of the
channel. When the workpiece is side extruded through the
channel, the total strain is
    
1 f c f c
e ¼ pffiffiffi 2cot þ þ c cosec þ (2)
3 2 2 2 2

Fig. 2. Material behavior during forming processes of micro-parts of a wire Fig. 3. Schematic illustration of side extrusion process, which are a kind of double
specimen with diameter to grain size D/d [28]. axis extrusion or side extrusion [29].
718 A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735

where F is the angle of intersection of two channels and C is the


angle subtended by the arc of curvature at the point of intersection.
When F = 908 and C = 08, the total strain from the above equation
is e = 1.15. After n passes, it becomes n  e.
Fig. 5 shows the fundamental process of metal flow during ECAP
[6]. The channel is bent through an angle equal to 908 and the
specimen is inserted within the channel and it can be pressed
through the die using a punch. There are four basic processing
routes in ECAP. In route A, the specimen is pressed without
rotation, in route BA the specimen is rotated by 908 in an alternate
direction between consecutive passes, in route BC the specimen is
rotated 908 counterclockwise between each pass, and in route C the
specimen is rotated by 1808 between passes.
From these macroscopic distortions shown in Fig. 5, the
influence of the processing route on the development of an
ultra-fine grained microstructure can be considered [33,36]. Horita
and coworkers [42] reported that the ultra-fine grained micro-
Fig. 4. Schematic representation of ECAE process.
structure of pure aluminum after 10 passes in route A was the same
as that after 4 passes in route BC.

2.1.2. Developed ECAP processes


Azushima et al. [46–48] proposed the repetitive side extrusion
process with back pressure. It is a process in which a high back
pressure is applied in the process as shown in Fig. 6, in order to
produce uniform shear deformation and prevent defects in the
workpiece. The specimen is side-extruded between the punches A
and B, while the punches C and D are fixed. In this process, the total
strain becomes 1.15 after one pass. The punch A, controlled by the
function generator, moves at a constant speed and the punch B
generates a constant back pressure. Recently, ECAP die-sets have
been developed to conduct the ECAP process with a back pressure
which is controlled by computers [46,47].
Nishida et al. [52–57] developed a rotary-die ECAP shown in
Fig. 7, which consists of a die containing two channels with the
same cross-sections intersecting at the center with a right angle in
order to remove the limitation in the conventional ECAP, i.e. the
sample must be removed from the die and reinserted again in each
step. At first, the sample is inserted into the die with the plunger as
shown in Fig. 7(a), and after pressing the sample as Fig. 7(b), the die
is then rotated by 908, and the sample is pressed again as Fig. 7(c).
By using this ECAP apparatus, a sample can be pressed by the
punch A with a back pressure from the punch B, similarly to that
shown in Fig. 6. Repetitive pressings may be carried out with the
rotary ECAP. This process is equivalent to route A in Fig. 5.
In the same way as the repetitive ECAP process, a method to
reduce the repetitive number by increasing the number of channel
turns in the die [58–61] was developed. Using the two-turn
channels the strain in one pass becomes double and the
productivity of the ECAP process increases. A counterpunch for

Fig. 5. Fundamental process of metal flow during ECAP. (a) The deformation of a
cubic element on a single pass [33]. (b) Shearing characteristics for four different Fig. 6. Schematic representation of repetitive side extrusion process with the back
processing routes [36]. pressure [46].
A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735 719

Fig. 7. The ECAP process using a rotary-die: (a) initial state, (b) after one pass and (c)
after 908 die rotation [52].

Fig. 10. The principle of the con-shearing process [64].

Fig. 11. The principle of the ECAR process for use in continuous production [68].
Fig. 8. Schematic representation of 2 turn ECAP [61].

providing additional pressure as shown in Fig. 8 may become a process is represented schematically in Fig. 11. The strip is fed
viable option available on common hydraulic presses. Presses with between two rolls and extruded to reduce the thickness of the
two opposite and equally powerful rams could be used for a cyclic strip. Then, the strip flows into the outlet channel. The principle of
process. In this process, the total strain becomes 2.3 after one pass. the ECAP conform process is represented schematically in Fig. 12.
These ECAP processes have been used only in the laboratory The workpiece is driven forward by frictional forces on the three
because of their low productivity. For mass production, continuous contact interfaces with the groove. The workpiece is constrained to
processing techniques must be developed. First, in order to the groove by the stationary constraint die, which restricts the
produce long metal bars and strips, equal channel angular drawing workpiece and forces it to turn by shear deformation similarly to
(ECAD) [62] and con-shearing were developed. the ECAP process.
The principle of ECAD is represented schematically in Fig. 9. In Fig. 13 shows an Al workpiece at every stage of the ECAP
the ECAD process, the material in the form of a bar is drawn conform process, from the initial feeding stock with a round cross-
through the two channels. The rods are preformed by bending section to the rectangular rod after the first ECAP pass. For the
them 1358 to fit to the die, and are drawn through the ECAP die ECAR process and the ECAE conform process, the total strain after
using as Instron tensile testing machine. one pass operation is given by Eq. (2), and the accumulated total
The principle of the con-shearing process is represented strain is n  e after n passes.
schematically in Fig. 10 [63–65]. An equal-channel die with a The Incremental ECAP (I-ECAP) was developed by Rosochowski
channel angle is located at the exit of a satellite mill. Satellite rolls et al. [70–72]. Fig. 14 explains the principle of this process; it is
and a central roll are used as feed rolls. All the rolls are driven at an based on incremental feeding of the billet by a distance ‘‘b’’
equal peripheral speed to generate large extrusion forces and the and using a reciprocating die ‘‘C’’ whose movement is synchro-
strip is extruded through the die continuously. This process uses nized with feeding. This enables feeding to take place during
friction between rolls to push the workpiece through an ECAP die. the withdrawal phase of die ‘‘C’’. When the billet stops at a pre-
In this process, the shear deformation is given to the strip determined position, die ‘‘C’’ approaches it and deforms a small
continuously, and the total strain after one pass is given by Eq. (2).
Recently, equal channel angular rolling (ECAR) [66–68] and
ECAP conform [69] were developed. The principle of the ECAR

Fig. 9. Schematic of the equal channel angular drawing process (ECAD) [62]. Fig. 12. Schematic illustration of the ECAP– Conform process [69].
720 A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735

Table 2
Summarizes the geometrical changes of the specimen during the ARB process
where roll-bonded by 50% reduction per cycle [81]
Number of Cycles, n 1 2 3 5 10
Number of layers, m 2 4 8 32 1024
Total reduction, r (%) 50 75 87.5 96.9 99.9
Equivalent strain, e 0.80 1.60 2.40 4.00 8.00

[81,82]. Stacking of sheets and conventional roll-bonding are


repeated in the process. First, a strip is neatly placed on top of
another strip. The interfaces of the two strips are surface-treated in
advance in order to enhance the bonding strength. The two layers
are joined together by rolling, as in the conventional roll-bonding
Fig. 13. Al workpiece undergoing processing by ECAP–Conform: the arrow marks process. Then, the length of the rolled material is sectioned into
the transition to a rectangular cross-section [69]. two halves. The sectioned strips are again surface-treated, stacked
and roll-bonded. These procedures can be repeated limitlessly in
principle, so that very large plastic strain can be applied to the
material.
The strain after n cycles of the ARB process can be expressed as,
pffiffiffi
3 t 1
e¼ lnðrÞ; r ¼ 1  ¼ 1  n (3)
2 t0 2

where t0 is the initial thickness of the stacked sheets, t the


thickness after roll-bonding and r the reduction in thickness per
cycle. Table 2 summarizes the geometrical changes of the
specimen thick sheets are stacked and roll-bonded by a 50%
reduction per cycle. The number of the initial sheets included in the
specimen processed by n cycles of ARB becomes 2n. After 10 cycles
of the ARB process, the number of layers becomes 1024 so that the
Fig. 14. Schematic representation of I-ECAP [70]. mean thickness of the initial sheet is smaller than 1 mm.
Optical micrographs of the ARB processed IF steel are shown in
volume of the billet. The mode of deformation is that of simple Fig. 17. In the material processed by two cycles ARB (Fig. 17(c)), the
shear and, provided the feeding stroke is not excessive, interface introduced in the second cycle is seen clearly. However, it
consecutive shear zones overlap resulting in a uniform strain is difficult to find the interface of the first pass at a quarter of the
distribution along the billet. Separation of the feeding and thickness. After five cycles, the whole thickness is covered by very
deformation stages reduces or eliminates friction during feeding; thin and elongated grains. This process has been used by many
this enables processing of infinite billets, both bars and plates/ researchers in order to create ultra-fine grained metals [84–88].
sheets.
On the other hand, the friction-reduced ECAP processes were 2.3. High Pressure Torsion (HPT) Process
developed in order to produce long bulk bars with square cross-
sections [73,74]. The principle of this process is schematically The HPT process was first investigated by Bridgman [89]. In his
represented in Fig. 15 [73]. By moving the tool, the friction forces experiments, attention was not paid to the microstructure change
over the three contacting interfaces become zero and the extrusion taking place in severely deformed metals. Another implementation
load decreases. of HPT was carried out by Erbel [90]. The specimen was a short ring
The ECAP process may be used for the consolidation of metallic with conical faces whose virtual extensions met at the axis of the
powder [31,75–79]. An aluminum powder and a steel powder at apparatus as shown in Fig. 18. The conical matching faces of the
room temperature was pressed using the ECAP facility as shown in
Fig. 4.

2.2. Accumulative roll-bonding (ARB) process

The ARB process was first developed by Saito et al. [80–83]. The
principle of the ARB process is represented systematically in Fig. 16

Fig. 16. Diagrammatic representation of the accumulative roll-bonding (ARB)


Fig. 15. The principle of friction-reduced ECAP processes [73]. process [81].
A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735 721

Fig. 17. Longitudinal cross-section of initial and ARB processed IF steel strips [82].

Fig. 20. Schematic illustration of the bulk-HPT process [94].

production of large bulk materials. Another disadvantage is that


the microstructures produced are dependent on the applied
pressure and the location within the disc. In order to solve the
problem, Horita and coworkers developed an HPT process for use
of the bulk sample as shown in Fig. 20 [94]. This process is
designated as Bulk-HPT for comparisons with conventional Disk-
HPT [95–104].
The severe plastic torsion straining (SPTS) process can be used
for the consolidation powders using a similar apparatus as shown
in Fig. 19 [105–107]. By using this process at room temperature,
the disk type samples with a high density close to 100% were
developed. The SPTS consolidation of powders is an effective
technique for fabricating metal–ceramic nano-composites with a
Fig. 18. Schematic diagram of ring tension device and dimensions of ring
specimens [90]. high density, ultra-fine grain size and high strength.

punches have radial teeth to facilitate the application of torque. 2.4. Other processes
The ring specimens were constrained from all directions which
created a condition closer to hydrostatic pressure. The principle of the cyclic extrusion compression (CEC) process
Recently, Valiev et al. conducted the HPT process using devices developed by Korbel et al. is represented schematically in Fig. 21
under high pressure as shown in Fig. 19 [15,16,89,91–104]. The [18,108–111]. In the CEC process, a sample is contained within a
design is a further development of the Bridgman anvil type device. chamber and then extruded repeatedly backwards and forwards.
In this device, a very thin disk is compressed in a closed die by a This process was invented to allow arbitrarily large strain
very high pressure. The torque is provided by the punch with deformation of a sample with preservation of the original sample
contact friction at the interface between the punch and disk. The shape after n passes. The accumulated equivalent strain is
strain in torsion is given by approximately given by

2pnr  
g ðrÞ ¼ (4) D
l e ¼ 4nln (6)
d
where r is the distance from the axis of the disk sample, n the number
where D is the chamber diameter, d the channel diameter and n the
of rotation and l the thickness of the sample. The equivalent strain
number of deformation cycles. Since the billet in the CEC process is
according to the von Mises yield criterion is given by
compressed from the both ends, a high hydrostatic pressure is
g ðrÞ imposed. The extrusion–compression load becomes high so that
eðrÞ ¼ pffiffiffi ; (5)
3 the special pre-stressed tools are required, otherwise the tool life
will be short. This process is better suited for processing soft
This method has the disadvantage that it utilizes specimens in material such as aluminum alloys. However, the strain introduced
the form of relatively small discs and is not available for the in the forward extrusion may be cancelled by the strain introduced
on the backward extrusion.
The principle of the cyclic closed-die forging (CCDF) process
developed by Ghosh et al. is represented schematically in Fig. 22
[21,112,113]. A billet is first compressed in the vertical direction
and then in the horizontal direction. The equivalent strain per
operation is given by

lnðH=WÞ
e¼2 pffiffiffi (7)
3

where W is the width of specimen and H the height of specimen.


The strain distribution is not uniform after strain accumulation.
The principle of the repetitive corrugated and straightening
Fig. 19. Schematic illustration of the thin disc-HPT process. (RCS) process developed by Huang et al. is represented schema-
722 A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735

Fig. 24. Principle of linear flow splitting [114].

Fig. 21. Schematic of cyclic extrusion compression (CEC).

Fig. 22. Schematic of cyclic closed-die forging (CCDF). Fig. 25. Principle of spin extrusion [115].

tically in Fig. 23 [17]. The technique consists of bending a straight of this approach is the opportunity to create a changed structure in
billet with corrugated tools and then restoring the straight shape of the surface region, keeping the lower region or core unchanged.
the billet with flat tools. The equivalent strain per one operation is The incremental forming method of the spin extrusion as shown in
given by Fig. 25 is used to create cup shaped or tube shaped parts from solid
billets. The hollow shape is created by the concurrent partial
½ðr þ tÞ=ðr þ 0:5tÞ
e ¼ 4ln pffiffiffi (8) pressure of three rolls on the surface of the workpiece and the
3 pressure of the forming mandrel acting in the axial direction. The
where t is the thickness of sample and r is the curvature of bent material flows axially and a cup wall is created between the
zone. By repeating these processes in a cyclic manner, high strains forming tools [116].
can be introduced in the workpiece. The principle of the severe torsion straining (STS) process
Linear flow splitting developed by Groche et al. is another developed by Nakamura et al. is represented schematically in
possibility to obtain ultra-fine grained metal [114]. The principle of Fig. 26 [20]. The process consists of producing a locally heated zone
this process is shown in Fig. 24. A sheet metal is compressed and creating torsion strain in the zone by rotating one end with the
between the splitting roll and the supporting rolls. Under this state other. The rod is moved along the longitudinal axis while creating
of stress two flanges are formed into the gap between the splitting the local straining. Therefore, a severe plastic strain is produced
and the supporting rolls. The material flow is mainly associated by continuously throughout the rod. In order to create the torsion
a surface enlargement of the band edge. Several hundred percent of strain efficiently, the locally heated zone should be narrow and the
plastic strain occur. As a consequence, the outer surface areas of rotation of the rod should be fast with respect to the moving speed
the flanges consist of ultra-fine grained metal. The properties of the of the rod. Moreover, a modification is made for the cooling system
metal in this state can be used for an increase of load bearing so that the heated zone is more localized to create torsion strain.
capability, e.g. bearings for rollers. The principle of the torsion extrusion process developed by
The applicability of incremental bulk forming processes with Mizunuma et al. is represented schematically in Fig. 27. This
high deformation for grain refinement in the sub-micrometer process is characterized by rotation of a die or a container during
range was investigated by Neugebauer et al. [115]. A specific aspect an extrusion process for introducing a very large strain in to the
metal. As high hydrostatic pressure involved in the extrusion raises
the ductility of the metals, a very large torsion straining can be
introduced to the workpiece. The mean value of representative

Fig. 23. Principle of repetitive corrugating and straightening [17]. Fig. 26. Principle of the severe torsion straining (STS) process [20].
A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735 723

Fig. 29. TEM Micrograph of ultra-low carbon steel after ECAPed 10 passes by route
A [46].

Fig. 27. Principle of the torsion extrusion process [19]. low carbon steel an ultra-fine grain size with a major axis length of
0.5 mm and a minor axis length of 0.2 mm was developed by 10
strain on a cross-section of a column can be calculated as below. passes of repetitive side extrusion at room temperature as shown
in Fig. 29 [46]. At the same time, they showed the relationship
4pRN
e ¼ pffiffiffi (9) between the area fraction and the mis-orientation angle by the
3 3H EBSP analysis [46]. They reported that most of the boundaries are
where R is radius of column, H is the height of the column, N is the high-angle grains, so that the processed steel is considered to be a
number of rotation. kind of ultra-fine grain structured metal.
Fig. 28 [19] shows a magnified view of the longitudinal section In the ARB processes, it was noted that the evolution of
of the etched aluminum specimen after the torsion extrusion microstructure and the increase in mis-orientation of boundaries
process, compared with that of the conventional extrusion. The were much faster than those when using conventional rolling
torsion extruded part of the specimen is clearly observed to be [117,118]. A typical TEM micrograph of the ultra-fine structure in
more severely strained than that of the conventional extrusion. the interstitial free (IF) steel ARB processed by 7 cycles at 500 8C is
shown in Fig. 30. From the crystallographic analysis by Kikuchi-
3. Properties of metals processed by SPD line analysis, they reported that most of the boundaries were at a
high angle.
The SPD-processed metals normally have ultra-fine grained From these TEM microstructures, it is expected that the
structures that cannot be obtained through conventional thermo- hardness and the tensile strength of metals with ultra-fine grains
mechanical processing. As a result, the SPD metals exhibit unique become higher. A number of studies have been conducted on the
and excellent properties such as high strength, compared with the strength and ductility of various kinds of metallic materials
conventional materials having a coarse grain size of over several processed by various SPD processes. The SPD-processed materials
tens of micrometers. generally have very high strength compared with conventional
In the optical microstructure of metals over 5 passes of the ECAP metals. Fig. 31 illustrates a general tendency of the change in
processes, it is observed that the strong filamentary microstructure strength and ductility during SPD. The strength of the materials
is developed with an increasing number of passes. In these continuously increases with increasing the applied strain and then
conditions, observed microstructure must use a TEM analyzer. gradually saturates. On the other hand, the ductility drops greatly
From the TEM microstructure, it is confirmed that many metals with a relatively small strain, and then keeps a nearly constant
with an ultra-fine grain size (under 1 mm) are developed by ECAP value or slightly decreases as the strain increases.
processes. Fig. 32 shows the relationship between the tensile strength,
The ultra-fine grains of sub-micron size were created by ECAP elongation and number of passes in ECAP for Armco steel [30]. The
processes in many of the metals and the grain size of the Al–4%Cu– tensile strength increases with increasing pass number. The tensile
0.5%Zr alloy became about 200 nm by ECAP with a plastic strain of strength is increased from 300 to 750 MPa after one pass. The
7 at 160 8C [2]. Aluminum and aluminum alloys with a sub-micron tensile strength is increased by a factor of 2 after one pass in
grain size were developed by ECAP processes [45]. For the ultra- comparison with the specimen before the ECAP process, and
increases with increasing pass number up to 8 passes. The tensile
strength is higher than 800 MPa after 8 passes. On the other hand,
the elongation decreases from 20% for the specimen before the
ECAP process to several percents after 8 passes.

Fig. 28. Magnified view of a longitudinal section of the etched aluminum specimen Fig. 30. TEM microstructure of the IF steel ARB processed by 7 cycles (e = 5.6) at
[19]. 500˚ C [118].
724 A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735

Fig. 31. Illustration showing the general tendency of the change in strength and
ductility during SPD. Fig. 34. Relationship between total elongation and pass number for carbon steels
based on ref. [121].

Horita et al. [33–35] reported the same results for the after 10 passes are plotted in the Hall–Petch relationship of the
aluminum alloys, and Azushima et al. [46–48,119–121] and Shin yield stress against the root grain size as shown in Fig. 2. In this
et al. [122–129] also reported for the steels. In particular, Aoki and figure, the results for these specimens show good agreement with
Azushima [121] reported the relationship between nominal stress the standard Hall–Petch relationship of iron obtained by Takaki
and nominal strain of specimens of ultra-low carbon steel, 0.15%C and coworkers [130].
steel, 0.25%C steel and 0.50%C steel processed by ECAP of 1, 2, 3, 5, Fig. 34 shows the relationship between total elongation and the
and 10 passes in route A at room temperature. They reported that pass number for the carbon steels. For the low carbon steel, the
the as-received material exhibits a stress–strain curve that elongation decreases to 20% after 3 passes, and for the other carbon
indicates normal strain hardening, while the specimens after steel, it decreases to 10% after 3 passes.
ECAP do not exhibit strain hardening. The stress for each specimen Moreover, Shin and coworkers [128] also reported the stress–
increases rapidly with increasing strain and reaches a maximum at strain curve of low carbon steel processed by ECAP at elevated
lower strain. temperatures as shown in Fig. 35. The tensile strength decreases
Fig. 33 shows the relationship between the tensile strength and with increasing processing temperature of ECAP and the total
the pass number for the carbon steels. The tensile strength elongation increases.
increases with increasing number of passes of ECAP. The tensile In the ARB process, Saito, Tsuji et al. [131–142] reported the
strength of ultra-low carbon steel after 10 passes was greater than mechanical properties of many metals processed by ARB. The
1000 MPa and was increased by a factor of 3 in comparison with relationship between the tensile strength, elongation and cycles of
the as-received material. The experimental data of the specimen a commercially pure aluminum (JIS-1100) SPD processed by the
ARB process is shown in Fig. 36 [132]. The tensile strength of the
1100-Al greatly increases to 185 MPa while the total elongation
drops down to 13% by the 1 ARB cycle (equivalent strain of 0.8). As
the number of the ARB cycles (strain) further increases, the flow
stress continuously increases and reaches 340 MPa, which is four
times higher than that of the starting material having a
conventionally recrystallized microstructure.
On the other hand, the elongation of the 1100-Al does not
change as much after the second ARB cycle. As was illustrated in
Fig. 29, this is the typical change in the mechanical properties
during SPD, which seems to occur regardless of the kind of SPD
process and material.
The decrease in ductility is a general feature of strain-hardened
metallic materials. Thus, it is not surprising that the SPD-processed
materials, i.e., ultra-high strained materials show limited tensile
Fig. 32. Relationship between tensile strength, elongation and pass number of ECAP ductility. It can be expected that the ductility can be recovered by
for Armco steel [30]. subsequent heat treatment, as is the case with deformed and
annealed materials. However, this has proven to be not so simple.

Fig. 33. Relationship between tensile strength and pass number for the carbon Fig. 35. Stress–strain curves of the CS steel after ECA pressing at 350, 480, 540 and
steels based on ref. [121]. 600 8C [128].
A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735 725

Fig. 36. Tensile strength and elongation of the 1100 commercially pure aluminum Fig. 38. Yield strength and UTS vs. accumulated strain for AA-6061 SPD processed
ARB processed by various cycles at RT [131]. by ECAP, MAC/F and ARB at room temperature [149].

Fig. 37 shows the stress–strain curves of the 1100-Al and ultra- Besides the mechanical properties, the fatigue property
low-carbon interstitial free steel SPD processed by the ARB and [120,150–154] and superplasticity property [133,155–167] were
then annealed at various temperatures for 1.8 ks [132]. In the investigated by many researchers.
figures, true stress and true strain are indicated by assuming
uniform elongation. Also the mean grain size of the specimens 4. Combined process and properties
measured from the microstructure observations are superimposed
in the figures. The strength of the materials decreases with 4.1. SPD process and conventional process
increasing grain size, i.e., with increasing annealing temperature.
However, large elongation can be obtained only after the strength In order to improve the strength of the ECAP processed metals,
decreases. In particular, the curves clearly show that the flow stress cold deformation can be combined with the ECAP process to
reaches its maximum at an early stage of tensile test and is then introduce crystalline defects and refine the grains. Recently, two
necked down to fracture in the UFG specimens. combined processes, the ECAP process and cold rolling, and the
The limited tensile ductility of the ultra-fine grained materials is ECAP process and cold extrusion were developed.
understood in terms of early plastic instability. As is well-known, the The principle of the combined process of ECAP and cold rolling
plastic instability condition (i.e., necking condition in tensile test) for is represented schematically in Fig. 39. Azushima et al. carried out
strain-rate insensitive materials, for example, is expressed as experiments in which the specimens of ultra-low carbon steel
were processed by ECAP in route A at room temperature and then
ds
s (10) the specimens processed by ECAP were rolled repetitively at room
de
temperature in order to increase the strength. Fig. 40 shows the
where s and e are true stress and strain, respectively. Ultra-grain tensile strength after the combined process [168]. After 10 passes
refinement greatly increases the strength, especially yield of ECAP, the tensile strength of ultra-low carbon steel is 1000 MPa
strength, of the materials. When the strain-hardening rate and after cold rolling with a reduction in thickness of 95% it
coincides with the flow stress, plastic instability, in other words becomes 1300 MPa.
necking, starts in the tensile test, which demonstrates a uniform Next, warm ECAP process was first used to refine the grain size
elongation. of commercially pure Ti billets and the billets were further
The mechanical properties of the metals with ultra-fine grain processed by repetitive cold rolling. The properties of the pure Ti
processed by SPD have been investigated [143–149]. Cherukuri processed by the two-step method are summarized in Table 3
et al. reported a comparison of the properties of SPD-processed AA- [169]. ECAP increased the yield and tensile even strength to 640
6061 by ECAP, CCDF and ARB as shown in Fig. 38 [149]. and 710 MPa, respectively. After a cold reduction of 35%, the yield
Commercially available AA-6061 in the annealed condition was and tensile strengths increased to 940 and 1040 MPa which are
subjected to severe plastic deformation processing by ECAP, CCDF higher than those for the Ti–6Al–4V alloy. Further cold rolling to a
and ARB at room temperature to approximately the same reduction of 55% resulted in even higher yield and tensile
accumulated strain (4). From Fig. 38, it is understood that the strengths.
SPD technique used did not show much effect on the flow behavior The principle of the combined process of ECAP and cold
of AA-6061. extrusion is represented schematically in Fig. 41. Stolyarov et al.
[170] carried out experiments in which the billet of commercially
pure Ti were first processed by ECAP in route BC at about 400 8C and
then the billets processed by ECAP were further processed by cold
extrusion to the accumulative reduction. The properties of the pure

Fig. 37. True stress–strain curves of (a) the 1100-Al ARB processed by 6 cycles at
200 8C and then annealed at various temperatures ranging from 100 to 400 8C for
1.8 ks and (b) IF steel ARB processed by 5 cycles at 500 8C and then annealed at
various temperatures from 200 to 800 8C for 1.8 ks [132]. Fig. 39. Principle of the combined process of ECAP process and cold rolling.
726 A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735

Fig. 40. Transition of tensile strength after combined process [168].


Fig. 42. Elongation to failure of the ECAP (4 passes) and ECAP (4 passes) + CR(70%)
samples as a function of initial strain rate at 450 8C [172].

a reduction in thickness of 70%. The comparison of the dependence


of elongation on strain rat e between ECAP and ECAP + cold rolling
(70%) samples is shown in Fig. 42. The elongations of the
ECAP + cold rolling samples were higher than that of the ECAP
sample at all strain rates. The maximum elongation was 812% at
5  103 s1 and it was much higher than that of the eight passes
ECAPed sample (595%). For the purpose of comparison, an
appearance of the ECAP and ECAP + cold rolling (70%) samples
elongated to failure is shown in Fig. 43. Similarly, the super-
plastic properties of 7075 aluminum alloy processed by ECAP
of one pass and isothermal rolling at 250 8C were examined and
Fig. 41. Principle of the combined process of ECAP process and conventional
a the alloy processed exhibited a maximum elongation of 820%
extrusion.
at a temperature of 450 8C and an initial strain rate of 5.6 
103 s1.
Ti processed by warm ECAP and cold extrusion are summarized in
Table 4. After cold extrusion to 47% reduction in cross-section, the 4.2. SPD process and annealing
yield and tensile strengths were increased to 910 and 930 MPa
respectively, which are higher than those of Ti–6Al–4V. Further The high strength of metal processed by SPD is obtained, but the
cold extrusion in cross-section of 75% yielded even higher yield and ductility of the metals after SPD becomes very low. In order to
tensile strengths. Next, in order to increase the strength of improve the ductility of the metal processed by SPD, the metals
aluminum alloy (AA-6101) this combined process was conducted. were annealed after SPD process.
The experimental results show that improved properties after cold
extrusion are heavily dependent upon the prior ECAP processing
routes.
On the other hand, in order to improve the superplastic
properties of metals processed by ECAP, cold deformation can be
combined with ECAP to refine the grains. Park et al. [171,172]
examined the superplastic properties at 450 8C of Al–Mg alloy
(A5154) processed by ECAP to 4 passes at 200 8C and cold rolling at

Table 3
Properties of pure Ti processed by two-step [169]

Processing state s0.2 (MPa) su (MPa) d (%)


Coarse grain (10 mm) 380 460 27
ECAP(8) a 640 710 14
ECAP(8) + CR(35%) 940 1040 7
ECAP(8) + CR(55%) 1020 1050 6
ECAP(12) + CR(35%) 920 955 15
CR(35%) b 660 670 16
a
ECAP route BC was used for all samples.
b
The value inside parentheses is cross-section reduction.

Table 4
Properties of pure Ti processed by warm ECAP and cold extrusion [170]

Processing state s0.2 (MPa) su (MPa) d (%) RA (%)

Coarse grain 380 460 27 69


ECAP(8) a 640 710 14 61
ECAP(8) + Cold extrusion(47%)b 910 930 – 55
ECAP(8) + Cold extrusion(75%) 1020 1050 6 42
Ti–6Al–4Vc 920 955 10 25
a
ECAP route BC was used for all samples.
b
Reduction in cross-section area from cold extrusion. Fig. 43. Appearance of (a) ECAP sample and (b) ECAP + CR(70%) sample tested up to
c
From ASTM F 136-96. failure at 450 8C [172].
A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735 727

Fig. 45. Tensile strength and elongation of ECA pressed low carbon steel annealed at
480 8C for various times [173].

In order to improve the ductility of metals processed by ARB, an


annealing process was conducted. Tsuji et al. carried out
experiments in which the aluminum and iron samples were first
processed by ARB at a warm temperature and then the samples
processed by ARB were further processed by annealing for 600 s or
1.8 ks from 200 to 800 8C. Fig. 37 shows the stress–strain curve of
commercially pure aluminum (1100-Al) and ultra-low carbon
Fig. 44. Relationship between tensile strength and hardness of specimens of ultra-
low carbon steel, 0.15%C, 0.25%C and 0.50%C steel after ECAP of 3 passes and then interstitial free steel specimens processed by various annealing
heat treatments of annealing [121]. conditions. The mean grain size is also indicated in this figure.
The flow stress of both metals increases with decreasing mean
grain size. Once the mean grain size becomes smaller than 1 mm,
Aoki and Azushima [121] carried out experiments in which the elongation of both Al and Fe suddenly reduced, though the strength
carbon steel samples were first processed by ECAP of 3 passes in still increased with decreasing grain size. On the other hand, as the
route A at room temperature and then the samples processed by grain size became larger than 1 mm, typical strain-hardening was
ECAP were further processed by annealing at a temperature of observed and the elongation increased with increasing grain size.
600 8C and changing annealing times. Fig. 44 shows the relation- Stolyarov et al. [169] carried out experiments in which the
ship between nominal stress and nominal strain of specimens of commercially pure Ti billets were first processed by warm ECAP
ultra-low carbon steel, 0.15%C steel, 0.25%C steel and 0.50%C steel and repetitive cold rolling and further the billets processed by
after the ECAP of 3 passes and after annealing. The tensile strengths annealing at temperatures of 200 and 300 8C. The properties of the
become lower and the total elongations increase with decreasing pure Ti billets processed are summarized in Table 5. Annealing
tensile strength. The uniform elongations increase with decreasing pure Ti processed by SPD at temperatures below 300 8C generally
tensile strength for all carbon steel samples. For example, a 0.5%C improves the ductility without decreasing the strength.
steel sample with a tensile strength 900 MPa and a total elongation
of over 20% is obtained. 4.3. SPD process and cooling
Shin et al. [129,173,174] investigated static annealing after
warm ECAP with a view to thermal stability. The low carbon steel: Fig. 46 shows the strip thermo-mechanical control process
0.15C–0.25Si–1.1Mn (in wt.%) (hereafter CS steel) was used. ECAP (TMCP), or combined strip fabrication process, to manufacture fine
was carried out on the samples at 350 8C up to 4 passes by Route C, grained plain carbon steel with a ferrite grain size of 3 mm [175].
then samples for subsequent annealing were encapsulated in a TMCP and micro-alloying technology is widely used to manufac-
glass tube with Ar atmosphere in order to minimize the possible ture precipitation-hardened high-strength steel sheets. The same
decarburization. The static annealing treatment was conducted at process may be used in the rolling of strip, but precipitates are not
480 8C up to 72 h. Stress–strain curves of the as-received, as- easily controllable during rolling because strip rolling mills are
pressed and annealed samples are shown in Fig. 45. The as-pressed arranged in tandem to gain higher productivity and constant
and annealed samples exhibited no strain hardening behavior. It is quality rather than flexibility.
of interest to note that stress–strain curves of the samples To manufacture fine-grained steel strips, the rolling tempera-
annealed for 24 and 72 h were almost identical. This observation ture must lie just above the transformation temperature or in the
implies that the sample annealed for 24 h was mechanically stable supercooled austenite state to accelerate transformation in the
although the microstructural examination revealed that recovery run-out table. This type of combined process can be used to
was in progress after 24 h annealing. manufacture plain carbon fine-grained steel sheets since the

Fig. 46. Super short interval multi-pass rolling process.


728 A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735

Table 5
Properties of pure Ti processed by warm ECAP and cold rolling with subsequent annealing [169]

Processing state s0.2 (MPa) su (MPa) d (%)


Coarse grain 380 460 27
ECAP(8) a 640 710 14
ECAP(8) + Cold rolling(35%)b + Annealing 200 8C, 0.5 h 985 990 8
ECAP(8) + Cold rolling(73%) + Annealing 300 8C, 1 h 942 1037 12.5
ECAP(12) + Cold rolling(35%) + Annealing 300 8C, 0.5 h 920 1000 14
Cold rolling(35%) 660 670 16
a
ECAP route BC was used for all samples.
b
Reduction in cross-section area by cold rolling.

micro-alloying technology is difficult to be applied to this increased from 350 to over 700 MPa with in decreasing grain size
process. The temperature of the strip is controlled throughout 4.5–1 mm, which is in good agreement with the Hall–Petch
the combined process to accumulate the dislocations in the grains relationship. It is also confirmed that the uniform elongation
before accelerated transformation. deceases.
An example of such combined processes is shown in Fig. 46. Another example of the combined process for producing the
This process can be used to produce ultra-fine grained C–Si–Mn ultra-fine grained steel is warm rolling and cooling, which uses
steel with a grain size of 1 mm [175]. A strip with a width of ferrite recrystallization during warm rolling [177–183]. Torizuka
300 mm was successfully produced by this process. Fig. 47 shows et al. [177,180–183] carried out multi-pass warm caliber rolling of
an example of ultra-fine grained C–Si–Mn steel obtained by hot two low carbon steel (SM490) specimens with a microstructure of
extrusion. Fig. 48 shows the yield strength of the steel sheet ferrite and Pearlite.
produced by the SSMR process as a function of ferrite grain size The specimen of the square bar with a side width of 80 mm was
[176]. Some previous studies and Hall–Petch equation are used. The warm caliber rolling schedule is summarized in Fig. 49.
also shown in the figure as a comparison. The yield strength is The caliber rolling at 500 8C was conducted in five stages to obtain
specimens of different cumulative strains for different micro-
structure and mechanical properties. The cumulative reduction
and the cumulative strain at each stage of rolling are also shown in
Fig. 49.
Fig. 50 shows the relationship between nominal stress and
nominal strain of specimens subjected to different cumulative
strains. The yield and tensile strengths of the caliber rolled
specimen increase monotonically with increasing cumulative
strain. There is a reduction in the elongation to failure of the
caliber rolled specimens compared to the undeformed specimen,
but there is almost no change among the specimens with different
accumulative strains.

Fig. 47. Ultra-fine grained steels obtained by SPD process.

Fig. 49. Caliber rolling schedule with cumulative reduction and cumulative strain at
each stage [180].

Fig. 50. Nominal stress–strain curves of undeformed specimen (e = 0) as well as


Fig. 48. Yield strength as a function of ferrite grain size [176]. caliber rolled specimens to various cumulative plastic strains (e = 0.7–3.8) [180].
A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735 729

Fig. 51. High strength thread articles out of SPD Ti alloy [184].

Fig. 54. View of article of ‘‘Piston’’ type fabricated from nanostructured Al1420 [2].
5. Applications

The properties of the metals processed by SPD exhibit high numerous laboratory-based SPD methods will emerge as the most
strength, ductility and fatigue characteristics. UFG metals are used appropriate for industrial implementation.
as a structural material due to these properties. Bolts are also As a result, potential producers of UFG metals hesitate to
manufactured with titanium alloys processed by ECAP as shown in commit themselves to any particular method. They are also
Fig. 51 [184] and are widely used in the automobile and aircraft concerned about the commercial viability of UFG metals, which
industries. Micro bolts using the UFG carbon steel processed by depends on the demand from potential markets and the cost of
cold ECAP have also been manufactured as shown in Fig. 52 [185]. production. Both of them are difficult to assess because of the low
Long carbon steel bars, of over several kilometers, with ultra- availability of UFG metals and uncertainty regarding the SPD
fine grains are manufactured by the warm continuous caliber technology. There is also a lack of knowledge regarding post-SPD
rolling and cooling process, from which the micro bolts are processing or shaping of UFG metals.
manufactured. Recently, in a Japanese National Project, sheets of Nevertheless, there are some applications which, with a high
low carbon steel of 2 mm thickness with ultra-fine grains were degree of probability, will be leading the introduction of UFG
manufactured by the TMCP process. The deep drawing ratio of each metals into commercial markets. Initially, those applications are
sheet was 1.9 and the parts were used in sheet metal forming as likely to be in the niche markets producing low volume specialty
shown in Fig. 53 [186]. products (e.g. sputtering targets). The next step will be the medium
It is well known [187,188] that superplastic forming is a highly volume markets with the emphasis put on product’s performance
efficient method of processing complex shape articles. An example rather than price (medical implants, defense applications, aero-
of a possible practical application for nanostructured Al alloys is space components, sports equipment). Eventually, the mass
shown in Fig. 54 [2]. It presents a complex shape article of ‘Piston’ production of components may be undertaken by the automotive
type which was fabricated from the nanostructured Al1420 alloy and construction industries.
by superplastic forming using the high strain rate superplasticity. With the exception of sputtering targets, the examples
In practice, despite a range of improved mechanical and presented below refer to potential applications rather than the
physical properties of bulk UFG metals produced by SPD, the current ones. Despite the focus of this paper on SPD-produced UFG
uptake of these materials by industry has been very slow so far. metals, applications using UFG consolidated powders and nanos-
There are several reasons for this; one is the lack of industrial tructured electrodeposited metals will also be considered as these
awareness of UFG metals. This is despite a large number of are indicative of what can be achieved with all types of UFG metals.
academics being engaged in research on SPD and UFG metals. The first commercial application of bulk UFG metals was in
Another reason is the scarcity of appropriately sized UFG samples sputtering targets for physical vapour deposition (Fig. 55).
for industrial trials; those produced by laboratories are usually too Honeywell Electronic Materials, a division of Honeywell Interna-
small because they are intended for metallurgical observations or tional Inc., offers UFG Al and Cu sputtering targets up to 300 mm in
basic mechanical testing. Finally, it is still not clear which of the diameter which are produced from plates by ECAP [189,190]. They
are used for metallization of silicone wafers in the production of
semiconductor devices. The main advantages of UFG sputtering
targets, compared to their coarse grained (CG) counterparts, are:
(1) the life span increased by 30% due to stronger material which
allows the use of monolithic targets and (2) a more uniform
deposited coating which results from reduced arcing. Another
company offering UFG Cu targets is Praxair Electronics, which
claims better sputter performance and 75% reduction in the
ownership cost of such targets.
Fig. 52. Overview and cross-section of micro bolts manufactured UFG Carbon steel
processed by cold ECAP [185].

Fig. 53. Examples of ultra-fine-grained C-Mn steel sheet forming [186]. Fig. 55. Worn out UFG 300 mm sputtering target [189].
730 A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735

of 600–700 MPa and elongation of 11%, the material exhibited a 33%


improvement in the ballistic performance or a similar mass
reduction compared to the standard plate.
Improvements in ballistic performance are also reported for the
electrodeposited nanocrystalline nickel-iron alloys produced by
Integran Technologies. Armor structures are usually fabricated by
welding of plates. However, traditional welding based on melting
is destructive to the UFG material. An alternative technique is a
solid state process of friction stir welding, which has the ability to
refine grain structure. This results in the weld hardness being only
marginally reduced compared to the initial hardness of a UFG
material [194].
Health issues surrounding the use of depleted uranium for
armor penetrators resulted in a search for alternative materials
with similar performance characteristics. One of those character-
istics is an inherent ability of depleted uranium to self-sharpen on
impact which is due to the generation of adiabatic shear bands.
Tungsten, sometimes considered as a replacement for depleted
uranium because of its high density, does not have this ability; thus
penetrators made of tungsten undergo mushrooming on impact,
which results in less penetration. UFG metals are known to have
reduced strain hardening capacity, which promotes localized
Fig. 56. Plate implants made of nanostructured titanium [192]. plastic deformation; at high deformation rates this leads to
adiabatic shear banding. This was confirmed by producing UFG
tungsten (by ECAP with a die angle of 1208 at 1100–1000 8C and
The next highly anticipated application is in the area of medical subsequent rolling at 600–700 8C), which exhibited adiabatic shear
implants. These include hip, knee and dental implants as well as banding when subjected to a dynamic load [195].
various screws, plates (Fig. 56) and meshes used in orthopaedic The aerospace industry values even small weight reductions
applications. Popular materials usually used in these applications which might be achieved by the introduction of new materials or
are cobalt-chrome alloys, stainless steel and titanium alloys. technologies. However, this industry is very cautious because of
Titanium alloys are used for implants because of their strength, low the safety concerns, and slow in implementing any changes.
modulus of elasticity (better matching that of bones), corrosion Introducing a new material may take 10–20 years, which results
resistance and good biocompatibility. Commercial pure (CP) from the requirements of the well established technology and a
titanium has better compatibility than titanium alloys but it is fully developed supply chain. UFG metals are not chemically
not used for load bearing implants because it is not strong enough. different from their CG precursors, so there should be no
However, when nanostructured by SPD and subjected to further fundamental obstacles to their use.
thermo-mechanical treatment, CP titanium can be strengthened to On the other hand the new properties of UFG metals have to be
achieve the yield stress of 1100 MPa, which is comparable with the well documented with respect to aerospace applications and the
yield strength of titanium alloys [191]. Traditional titanium SPD and post-SPD processes have to be commercially available. All
implants do not perform well with respect to wear resistance these requirements mean that we will have to wait a few more
and fatigue life. Therefore, improvements in these properties, years for the first aerospace applications. These, most likely, will be
reported for UFG titanium, will be appreciated. Some Russian [192] associated with light UFG metals used for structural components of
and USA laboratories report that the UFG CP titanium implants are the fuselage and wings. Regarding the engines, some external
being already tried. elements (e.g. shields) and less thermally demanding internal
The defense industry could benefit from two large scale elements (e.g. titanium blades for the low pressure compressor
applications of UFG metals, which are armor plates and armor section) can also be considered. There has only been limited
penetrators. Lighter armor for military vehicles (Fig. 57) is crucial for information published so far on the potential use of UFG metals by
the reduction of fuel consumption, higher speed, better maneuver- the aerospace industry; Boeing, filed a few patents on friction stir
ability, longer operation range and air-transport of vehicles to welding used as a means of nanostructuring metals for fasteners
remote locations. At the same time the ballistic performance and other parts [196] while EADS is interested in UFG aluminum
must not be reduced. This can be achieved by the nanostructuring sheets.
of aluminium or titanium alloys traditionally used for light Users of sports equipment will also benefit from UFG metals,
armored vehicles. A good example is a UFG Al 5083 plate, which particularly where high strength and low weight is required. UFG
was obtained by cryogenic ball milling, consolidation by HIP, metals could find applications in high performance bicycles, sailing
forging or extrusion and finally rolling [193]. With the yield strength equipment, mountaineering equipment, golf, tennis, hockey, etc.
One example is NanoDynamics high performance (NDMX) golf
balls, which have a hollow nanostructured titanium core (Fig. 58).
The core material is manufactured using the UFG chip machining

Fig. 57. AAV7A1 Amphibious Assault Vehicle (image courtesy of BAE Systems). Fig. 58. NDMX golf ball (image courtesy of NanoDynamics).
A. Azushima et al. / CIRP Annals - Manufacturing Technology 57 (2008) 716–735 731

Fig. 59. Metallix racquet (image courtesy of HEAD).

technology licensed from Purdue University. Another example of


using UFG metals in sporting goods is the commercial activity of
PowerMetal Technologies, a company with an exclusive license to
use Integran’s electrodeposition technology in consumer products.
They cooperate with HEAD in the production of their new Metallix
(Fig. 59) and Airflow racquets, which use a composite of carbon
Fig. 61. SEM pictures of a micro-bulged sheet made of CG and UFG Al 1070 [200].
fibres and nanocrystalline metal.
UFG metals can be beneficial to some products through
improvements in their manufacturing processes. The most promis- substantial reduction of the orange peel effect [200]. Another
ing one is superplastic forming which is currently confined to a low advantage of using UFG metals is better surface finish resulting
volume production because of a very low process speed, necessary from micro-milling [201], micro-EDM [202] and diamond turning
when forming classical superplastic metals. UFG metals possess [203].
better superplastic properties, which allow a tenfold increase of the The above applications of UFG metals are only a fraction of the
forming speed, and some temperature reduction [197]. Superplastic possible uses. Since the SPD technology can convert all CG metals
UFG metals exhibit higher ductility which makes them suitable for into UFG metals, it is only a matter of time when new, sometimes
forming more complex components. Despite large volume of unexpected, applications will be discovered. For this to happen,
research on SPF of UFG metals, practical applications are still a information dissemination among industrial engineers, transfer of
matter for the future. One possible application has been presented reliable SPD technologies to industry and commercialization effort
by the Institute for Metals Superplasticity Problems, Ufa, Russia. is required [204].
They made models of hollow blades by diffusion bonding (DB) and
SPF using UFG Ti–6Al–4V sheets (Fig. 60). By using sheets with the 6. Conclusion
grain size down to 0.2 mm they were able to decrease the
temperature of the process from 900 to 800 8C for DB and to Processes of severe plastic deformation, defined as metal
700 8C for SPF [198]. The temperature reductions observed will forming processes in which an ultra-large plastic strain was
improve technical feasibility and the economics of the process. imposed on a bulk material in order to make ultra-fine grained
Among many interesting properties of UFG metals is their metals, were reviewed in this keynote paper. As processes used for
ability to flow easier and at lower temperatures when forged into this purpose, various methods such as, ARB, HPT, RCS, CEC, STS,
complex shapes. It is claimed that energy savings up to 30% could CCDF, etc. were developed, and combined SPD processes with
be achieved due to: lower forging temperature, shorter heat-up conventional processes were also proposed.
time, smaller forging stock size, fewer number of hits and lower The properties of the metals processed by SPD are also
forging load [199]. A very small grain size can be a virtue of its own. reviewed. The SPD-processed metals have very high strength,
This is the case with metal micro-parts having geometrical sizes and in order to increase the strength further, conventional cold
comparable with coarse grains of classical materials. Using UFG forming processes are combined with SPD processes. Since the
metals in microforming allows micro-billets to behave as ductility of metals is reduced by relatively low strain, the heat
polycrystalline billets. This refers to both the inner body and the treatment of annealing is conducted after the SPD process in order
surface of the billet. The latter is illustrated in Fig. 61 as a to improve the ductility. The properties of the metals processed by
the SPD processes exhibit high strength and ductility that lead to
good fatigue characteristics.
The UFG metals could be used as structural materials due to
these properties, but the area of application is limited at the
moment because the available size of billet is small. Since SPD
technology can convert all metals into UFG metals, it is expected
that new methods of producing larger billets will enlarge the area
of applications.

Acknowledgment

The authors wish to thank Prof. K. Osakada and Dr. J. Allwood for
checking the manuscript of keynote paper.

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