Scripta Materialia 51 (2004) 807812

www.actamat-journals.com

Fatigue and microstructure of ultrane-grained metals produced

by severe plastic deformation
H. Mughrabi *, H.W. H
oppel, M. Kautz
Institut f
ur Werkstowissenschaften, LS WW I, Universitat Erlangen-Nurnberg, Martensstr. 5, D-91058 Erlangen, Germany
Accepted 6 May 2004
Available online 17 June 2004

Abstract
The cyclic deformation and fatigue behaviour of ultrane-grained metals produced by the severe plastic deformation technique
ECAP (equal channel angular pressing) is discussed briey with respect to cyclic softening, macroscopic shear banding and fatigue
lives. Possibilities to enhance the LCF fatigue resistance by annealing are indicated.
2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Keywords: Ultrane-grained metals; ECAP; Microstructure; Fatigue damage; Fatigue life; Annealing

1. Introduction sporadically [710]. More recently, research focussing on

Nanocrystalline materials with extraordinary proper-
ties have attracted much attention since Gleiters rst
publication on the subject in 1981 [1]. With respect to
practical applications, the mechanical strength and duc-
tility are properties of prime importance. Since nano-
crystalline materials with grain sizes in the range of some
10 nm are not readily available in bulk form with mac-
roscopic dimensions, bulk ultrane-grained (UFG)
metallic materials with grain sizes of some 100 nm, pre-
pared by severe plastic deformation (SPD) techniques
such as, in particular, equal channel angular pressing
(ECAP) [24], are currently studied intensively. The
presentations at the recent Second International Con-
ference on Nanomaterials by Severe Plastic Deformation
[5,6] and at other Symposia on the preparation, micro-
characterization and properties of UFG materials are
good examples.
In the past, the extraordinary high strength of UFG
metals at low temperatures and their potential for high
strain rate and/or low temperature superplasticity at
higher temperatures, compare [26], received much
attention. Until the late nineties, the cyclic deformation
and fatigue behaviours, however, were studied only
*
Corresponding author. Tel.: +49-9131-8527482; fax: +49-9131-
8527504.
E-mail address: mughrabi@ww.uni-erlangen.de (H. Mughrabi).
1359-6462/$ - see front matter 2004 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.
doi:10.1016/j.scriptamat.2004.05.012
the cyclic deformation and fatigue properties, which can
be crucial for the use of UFG materials in practical
applications, has increased noticeably, see e.g. [1119].
The recent fatigue studies concentrated either on the
cyclic deformation, fatigue failure and life and the
underlying microstructural mechanisms, e.g. [719], or on
the eects of fatigue crack propagation [20,21]. This short
contribution will focus on the former topics, considering in
particular the UFG microstructure, its response to cyclic
deformation and possibilities to optimize the fatigue per-
formance by suitable annealing subsequent to ECAP
processing. One main objective of the current work of the
authors is to optimize the UFG microstructure of com-
mercial alloys with respect to their fatigue performance,
compare [19,22]. Nonetheless, this report will essentially
be conned to cyclic deformation and fatigue (under
conditions of symmetrical push-pull) of single-phase
metals such as copper, aluminium and a-brass, empha-
sizing the basic microstructural features and mechanisms.
2. Basic features of cyclic deformation and fatigue
resistance
2.1. Repeated cyclic microyieldingnon-linear unloading/
reloading and internal stresses
Metal fatigue is conveniently divided into low cycle
fatigue (LCF) and high cycle fatigue (HCF) with fatigue
808 H. Mughrabi et al. / Scripta Materialia 51 (2004) 807812

lives Nf (number of cycles to failure) roughly below and ering the successive (micro)yielding of the harder (un-
above Nf
104 cycles, respectively. With respect to tidy) grain boundary regions and the softer grain
cyclic deformation, it is important that, in LCF, the interior regions, the non-linear stressstrain unloading/
plastic strain amplitudes lie between some 103 to 102 reloading behaviour can be understood semi-quantita-
and exceed the elastic strain amplitudes considerably. In tively [23].
HCF, however, the plastic strain amplitudes are typi-
cally only some 104 , ranging down to some 105 , and
2.2. Cyclic deformation
are therefore generally smaller than the elastic strain
amplitudes. Cyclic deformation leading ultimately to
The early (strain-controlled) LCF cyclic deformation
fatigue failure is thus always a sequence of repeated
tests on UFG copper [7,9,1113] showed that, in the as-
microyielding in tension and in compression.
ECAP-processed state (grain size: ca. 200300 nm), the
In order to gain some insight into the microyielding
heavily predeformed microstructure is rather unstable
behaviour of UFG metals and to compare it with that of
and undergoes marked cyclic softening from the begin-
conventional grain (CG) size material, repeated tensile
ning. The responsible microstructural processes have
microyielding, unloading and reloading tests were per-
been identied as fatigue-induced grain coarsening
formed on high-purity UFG copper and on commercial
leading to grain sizes of some microns [7,11,12,18] and
purity UFG aluminium. As reported earlier for copper
to catastrophic macroscopic shear banding under an
[19,22], a surprising nding was that, in the as-ECAP-
angle of ca. 45 to the stress axis [79,11,12]. The grain
processed condition, the unloading and reloading stress
coarsening in fatigued UFG copper has been shown to
strain curves of the UFG copper were highly non-linear
be a thermally activated process of dynamic recrystalli-
with an appreciable microplastic back/forward ow
zation which occurs already at a rather low homologous
during unloading/reloading, whereas the CG material
temperatures of ca. 0.2 (room temperature) and which is
(grain size: ca. 40 lm) exhibited an essentially linear
enhanced at lower cyclic strain rates and at higher
elastic unloading/reloading stressstrain behaviour. In
temperatures [18]. In the as-ECAP-processed state, no
order to recover the heavily pre-deformed microstruc-
characteristic dislocation substructure can develop dur-
ture, an annealing treatment (170 C, 2 h) was per-
ing cyclic deformation in the original ultrane grains,
formed. The microyielding tests were repeated, yielding
since the substructural characteristic dimensions/spac-
essentially the same non-linear unloading/reloading
ings would be smaller than the grain size [15,24]. In the
characteristics, albeit at reduced stresses as a conse-
coarsened grains, however, substructural features such
quence of the annealing. In Fig. 1a and b, the results of
as di-/multipolar dislocation veins/walls, which are
similar tests on UFG aluminium (as-ECAP, 12 passes,
commonly observed in fatigued CG material, can de-
route Bc , cf. [4], grain size: ca. 800 nm) and on CG
velop [7,11,15].
aluminium (grain size: ca. 45 lm), respectively, are
shown. The results (also after annealing) are similar as
for copper. Hence, it is concluded that the non-linear 2.3. Low cycle and high cycle fatigue lives
unloading/reloading behaviour is characteristic of UFG
materials and that, in the UFG materials, much larger The fatigue lives of UFG copper, plotted as a W ohler
internal back stresses are induced during straining than SN plot (stress amplitude Dr=2 versus log Nf ) and in a
in CG material. In a simple composite model, consid- ConManson plot (log of plastic strain amplitude

120 120
(a)
(b)
100 100

80 80
/ MPa

/ MPa

60 60

40 40

20 20

0 0
0.000 0.001 0.002 0.003 0.004 0.000 0.001 0.002 0.003 0.004
pl pl
Fig. 1. Tensile microyielding stressstrain curves (plot of stress r versus plastic strain epl ) with repeated unloadings and reloadings. (a) UFG alu-
minium, as-ECAP; (b) CG aluminium. (after Ref. [19]).
 H. Mughrabi et al. / Scripta Materialia 51 (2004) 807812 809

Depl =2 versus log Nf ), are shown in Figs. 2 and 3, the conclusion of Wu et al. [26] that macroscopic shear
respectively. In Fig. 2 (stress-controlled tests), the data banding in fatigue originates always from ECAP-
are compared with earlier work of Thompson and induced bands, since the latter can be avoided by
Backofen [25] on CG copper of dierent grain sizes, appropriate processing.
showing only a small grain size eect. It is evident that Concerning the LCF ConManson data of strain-
the fatigue lives of UFG copper, studied by three dif- controlled fatigue tests on copper, Fig. 3 shows that the
ferent groups (Agnew and Weertman [7], H oppel et al. fatigue resistance of CG copper is superior to that of
[11,12] and Vinogradov and Hashimoto [13]) all exceed UFG copper in the as-ECAP-processed state. The same
those of CG copper appreciably but by dierent is true for the AlAg alloy AA 5056 from the work of
amounts. The latter is presumably related to details of Patlan et al. [14], for a-brass [22] and for aluminium [19].
the ECAP processing. Thus, the initial UFG micro- After an optimized annealing heat treatment, compare
structure can be equiaxed (type A) or it can sometimes Section 3, UFG copper exhibits a markedly enhanced
contain bands of elongated grains (type B), cf. [9,13]. fatigue life and is now superior to CG copper (data from
These bands, stemming from ECAP, can accelerate Mughrabi and Wang [27]). Attempts to improve the
damaging macroscopic shear banding. Thus, the UFG LCF fatigue resistance of UFG a-brass [22], UFG alu-
type A grain structure in the work of Vinogradov and minium [19] and the aluminium alloy 5056 [14] by
Hashimoto [13] and H oppel et al. [11,13] is more stable annealing treatments were less successful. As shown in
against cyclic softening and shear banding and exhibits Fig. 3 for a-brass and aluminium, the fatigue lives could
signicantly larger fatigue lives than the UFG type B be increased in all cases, without however attaining the
grain structure in the work of Agnew and Weertman [7]. fatigue lives of the corresponding CG materials. Finally,
Still, as emphasized earlier [19], these data do not justify it is noted that the slopes of the ConManson plots of
AA 5056 are unusually steep (slope
1). Patlan et al.
[14] do not comment on this fact.
UFG Cu, [Agnew & Weertman]
350 ..
UFG Cu, [Hoppel & Mughrabi]
CG Cu,3 grain sizes 115, 15, 3.4 m
stress amplitude /2/MPa

300 [Thompson&Backofen] 2.4. Rationalization of fatigue behaviour in terms of

UFG Cu, [Vinogradov and Hashimoto] fatigue strength and ductility
250
3.4 m
200 Two of the present authors [12] have proposed a
simple rationale to explain why the LCF behaviour of
150
15 m UFG metals is generally inferior to that of CG material
100 115 m although the HCF resistance is generally signicantly
50
enhanced. This explanation is based on the total strain
fatigue life diagram shown schematically in Fig. 4 for
4 5 6 7
10 10 10 10 UFG and CG material. The fatigue life relation shown
cycles to failure Nf
in the gure is based on the splitting of the total strain
Fig. 2. Wohler SN plot of fatigue life data of UFG copper, as-ECAP amplitude Det =2 into its elastic and plastic components,
[1113] and CG copper [25]. Deel =2 and Depl =2, respectively. The rst term refers to
HCF (Basquin relation) and is usually expressed in
terms of the fatigue strength coecient r0f 0 , the elastic
modulus E, the fatigue strength exponent b and Nf ,
UFG Cu, as-ECAP whereas the second term, referring to LCF (Con
plastic strain amplitude pl/2

UFG Cu, heat-treated,

170 C, 120 min Manson rule), is expressed via the fatigue ductility
-2 CG Cu, [Mughrabi & Wang]
10 UFG AA5056, [Patlan et al.] coecient e0f , the fatigue ductility exponent c and Nf .
CG AA 5056, [Patlan et al.]

10-3
CG -brass
UFG -brass, as-ECAP
UFG -brass, heat-treated, 300 C, 120 min
CG Al
UFG Al, as-ECAP
10-4 UFG Al, heat-treated, 220C, 60 min
2 3 4 5 6
10 10 10 10 10
reversals to failure 2Nf

Fig. 3. ConManson plot of fatigue life data of dierent UFG

materials in as-ECAP-processed state and after annealing and of Fig. 4. Schematic total strain fatigue life diagram for UFG and CG
corresponding CG materials. Data from [11,14,22,27]. material. After [12].
810 H. Mughrabi et al. / Scripta Materialia 51 (2004) 807812

Fig. 5. Comparison of experimental data and model predictions of fatigue life of UFG copper (initial state and after annealing) fatigued in strain
control and of UFG copper (initial state) fatigued in stress control. (a) ConManson plot; (b) Basquin plot. After [28].

After ECAP, UFG materials exhibit an enhanced value been achieved in a number of cases [10,11,13,17,22] by
of r0f =E, reecting their increased strength, but a reduced subjecting the UFG material to a suitable annealing
value of e0f 0 because of a loss in ductility [17]. An en- treatment after ECAP. The main problem then is to nd
hanced HCF resistance and a reduced LCF performance a strategy to optimize the annealing treatment. The
are a natural consequence (Fig. 4). Moreover, it is authors have pursued dierent routes [22]. The initial
concluded that a suitable annealing treatment which idea was to attempt to retain the UFG structure by
leads to an enhanced fatigue ductility (at the expense of applying only a recovery heat treatment that would not
some fatigue strength) should improve the LCF resis- induce recrystallization. This was attempted by heating
tance (and lower the HCF resistance somewhat). the UFG specimens very slowly (e.g. at 0.5 C/min) up
to a certain temperature so that most of the extra stored
energy and driving force for recrystallization would re-
2.5. A fatigue life model of UFG materials
cover before recrystallization could occur. In high-pur-
ity UFG copper, at least partial recrystallization always
In a detailed fatigue model, Ding et al. [28] viewed the
occurred below 170 C. Hence, in a series of isothermal
UFG material as a composite with soft grain interiors
annealing treatments for dierent times at 170 C, an
and hard grain boundaries and considered the resistance
optimum heating time (2 h) for achieving a maximum
of this microstructure to fatigue crack propagation. An
fatigue life (superior to that of CG material) was
essential ingredient of their model is the incorporation
determined [11,12,17], compare the results shown in
of the appropriate cyclic stressstrain curve (satura-
Figs. 3 and 5. All annealing treatments led to some sort
tion stress versus Depl =2). The results of the model can
of bimodal grain mixture with the larger grains embed-
be displayed either as a ConManson or a Basquin (or
ded in the original UFG structure. In UFG commercial
a W ohler SN) plot, as shown in Fig. 5a and b,
purity aluminium and in commercial purity UFG a-
respectively, for UFG copper tested in strain control in
brass, the original UFG structure could essentially be
the initial state after ECAP and after annealing and also
retained (with marginal coarsening) by the slow heating-
for UFG copper in the initial state, tested in stress
control (Dr=2 const:). With one and the same set of
parameters, the model provides a reasonable t to the
experimental data, taken from [11,12]. In particular, it
should be noted that, depending on the type of plot, the
sequence of fatigue lives for the three material states are
reversed.

3. Enhancement of LCF resistance by annealing treat-

ments

3.1. Annealing and subsequent fatigue of UFG materials

As discussed in Sections 2.3 and 2.4, an improvement Fig. 6. Schematic representation of the dierent kinetics of recovery
of the LCF performance of UFG materials can and has and recrystallization.
 H. Mughrabi et al. / Scripta Materialia 51 (2004) 807812
Fig. 7. Bimodal grain microstructure of high purity UFG copper after annealing (170 C, 2 h). (a) Prior to fatigue; (b) after fatigue at Depl =2 103 .
From [11,17].
up procedure, indicating that the purity can play an
important role. In a-brass, heating up to somewhat
higher temperatures, cf. [22] for details, led to a bimodal
structure. However, although the LCF performance was
enhanced in all cases, it remained below that of CG
material, compare [14,22] and Fig. 3.
3.2. Competition between recovery and recrystallization
In view of the above, it appears important to ratio-
nalize the strategies to optimize the annealing treatments
applied in order to enhance the LCF performance of
UFG materials. It is therefore instructive to consider the
competition between recovery and recrystallization,
compare [29]. Fig. 6, adapted schematically from stan-
dard textbooks, illustrates the dierent kinetics of the
two competing processes. Since recrystallization lags
behind recovery, the driving force for recrystallization
can be strongly diminished by preceding recovery which
will be favoured at lower temperatures and heating
rates. Since the precise behaviour will vary with purity,
compare Section 3.1, from material to material and
depend on the heating procedure, time-consuming sys-
tematic studies will be necessary in each case in order to
obtain a particular recovered UFG or a bimodal grain
structure for optimal fatigue strength.
3.3. The bimodal grain size distribution: an optimal
microstructure for high fatigue strength?
The bimodal initial grain size distribution which led to
an optimum LCF resistance of UFG copper is shown in
a TEM micrograph in Fig. 7a. As shown in Fig. 7b,
dislocation patterns typical of fatigued CG copper de-
velop in the larger grains of this bimodal grain distri-
bution during fatigue. Ma and co-workers have also
advocated the bimodal structure, obtained by ECAP and
a subsequent annealing treatment, as a microstructure
that provides an excellent combination of strength and
ductility in monotonic deformation [30]. It can be as-
811
sumed, for both monotonic and cyclic deformation, that
the strength of the bimodal structure is mainly related to
the ultrane grains, while the ductility is promoted by the
coarser (but still quite small) grains. However, cf. Section
3.2, annealing treatments can lead to a variety of bimo-
dal grain size distributions with dierent fractions of
ultrane and coarser grains. Hence, future studies should
clarify and quantify the nature of optimum bimodal
grain size distributions for particular applications
and the processing routes to obtain them.
4. Concluding remarks
The recent studies on the fatigue of UFG metals
prepared by ECAP have shown in several cases that the
HCF strength is enhanced, compared to CG material,
while the LCF performance is reduced because of the
lower ductility of the UFG material. Annealing treat-
ments to enhance the fatigue ductility and the LCF
strength appear promising but need more systematic
studies.
References
[1] Gleiter H. In: Hansen N et al., editors. Proceedings of Second
Risoe International Symposium on Metallurgy and Materials
Science. Roskilde: Risoe Nat. Lab.; 1981. p. 15.
[2] Lowe TC, Valiev RZ, editors. Investigations and applications of
severe plastic deformation. Dordrecht: Kluwer Academic Pub-
lishers; 2000.
[3] Valiev RZ, Islamgaliev RK, Alexandrov IV. Prog Mater Sci
2000;45:103.
[4] Furukawa M, Horita Z, Nemoto M, Langdon TG. J Mater Sci
2001;36:2835.
[5] M. Zehetbauer, editor. Proc of Second Internat Conf on
Nanomaterials by Severe Plastic Deformation, invited papers:
Adv Eng Mat 2003;5:291378.
[6] As Ref. [5], M. Zehetbauer, R.Z. Valiev, editors. All papers.
Weinheim: Wiley-VCH; 2004.
[7] Agnew SR, Weertman JR. Mater Sci Eng A 1998;244:145.
812 H. Mughrabi et al. / Scripta Materialia 51 (2004) 807812
[8] Vinogradov A, Kaneko Y, Kitagawa K, Hashimoto S, Valiev R.
Mater Sci Forum 1998;269272:987.
[9] Agnew SR, Vinogradov AY, Hashimoto S, Weertman JR.
J Electron Mater 1999;28:1038.
[10] Stolyarov VV, Alexandrov IV, Kolobov YuR, Zhu M, Zhu Y,
Lowe T. In: Wu XR, Wang ZG, editors. Proceedings of Seventh
International Fatigue Congress, Vol. 3. Beijing: Higher Education
Press; 1999. p. 1345.
[11] Hoppel HW, Brunnbauer M, Mughrabi H, Valiev RZ, Zhilyaev
AP. Proc of Materialsweek 2000. Available from: http://www.ma-
terialsweek.org/proceedings, Munich, 2001.
[12] Mughrabi H, H oppel HW. In: Farkas D et al., editors. Structure
and mechanical properties of nanophase materialstheory and
computer simulation vs experiment. Warrendale: MRS; 2001.
p. B2.1.1.
[13] Vinogradov A, Hashimoto S. Mater Trans 2001;42:74.
[14] Patlan V, Vinogradov V, Higashi K, Kitagawa K. Mater Sci Eng
A 2001;300:171.
[15] Thiele E, Holste C, Klemm R. Z Metallkd 2002;93:730.
[16] Vinogradov A, Hashimoto S. Adv Eng Mat 2003;5:351.
[17] Hoppel HW, Valiev RZ. Z Metallkd 2002;93:641.
[18] Hoppel HW, Zhou ZM, Mughrabi H, Valiev RZ. Philos Mag A
2002;82:1781.
[19] Hoppel HW, Xu C, Kautz M, Barta-Schreiber N, Langdon TG,
Mughrabi H. in Ref. [6], p. 676, and unpublished work.
[20] Chung CS, Kim JK, Kim HK, Kim WJ. Mater Sci Eng A
2002;337:39.
[21] Hanlon T, Kwon Y-N, Suresh S. Scripta Mater 2003;49:675.
[22] Mughrabi H, H oppel HW, Kautz M, Valiev RZ. Z Metallkd
2003;94:1079.
[23] Mughrabi H, H oppel HW, Kautz M. Trans Royal Soc South
Africa, in press.
[24] Mughrabi H. In: Lowe TC, Valiev RZ, editors. Investigations and
applications of severe plastic deformation. Dordrecht: Kluwer
Academic Publishers; 2000. p. 241.
[25] Thompson AW, Backofen WA. Acta Metall 1971;19:597.
[26] Wu SD, Wang ZG, Jiang CB, Li GY, Alexandrov IV, Valiev RZ.
Scripta Mater 2003;48:1605.
[27] Mughrabi H, Wang R. In: Lukas P, Polak J, editors. Basic
mechanisms in fatigue of metals. Prague/Amsterdam: Academia/
Elsevier; 1988. p. 1.
[28] Ding HZ, Mughrabi H, H oppel HW. Fatigue Fract Engng Mater
Struct 2002;25:975.
[29] St
uwe HP, Padilha AF, Siciliano Jr F. Mater Sci Eng A
2002;333:361.
[30] Wang Y, Chen M, Zhou F, Ma E. Nature 2002;419:912.