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Special Issue on Strength of Fine Grained Materials ® 60 Years of HallPetch ®

© 2013 The Japan Institute of Metals and Materials OVERVIEW

of Ultraﬁne-Grained and Nanocrystalline Metals

Masaharu Kato+

Department of Materials Science and Engineering, Interdisciplinary Graduate School of Science and Engineering,

Tokyo Institute of Technology, Yokohama 226-8502, Japan

Models and theories to explain the HallPetch relationship are reviewed brieﬂy. Then, a dislocation model to incorporate some

characteristic mechanical properties of ultraﬁne-grained and nanocrystalline metals will be introduced and used to explain some experimental

results. The model is based on the idea that dislocations emitted from grain boundaries and bow out into grain interiors during their propagation

are responsible for plastic deformation and thermally-activated depinning process at grain boundaries is regarded to be rate controlling. Some

implications of the model are discussed in the light of recent experimental results. [doi:10.2320/matertrans.MA201310]

(Received July 31, 2013; Accepted August 26, 2013; Published December 25, 2013)

Keywords: HallPetch relationship, yield stress, dislocation, grain boundary, strength, ultraﬁne-grained metal, strain rate, temperature,

thermal activation

1. Introduction τ

It is well known that ultraﬁne-grained (UFG) and nano- FR

crystalline (NC) metals and alloys show characteristic GB source

mechanical properties different from those of conventional 1 2 3 np

coarse-grained (CG) counterparts.16) For example, as grain Lp

size becomes smaller, (1) strength becomes higher (the Hall τ

Petch (HP) behavior) and then lower (the inverse HP

Fig. 1 Dislocations generated from a FrankRead (FR) source pile up at a

behavior). (2) strength of fcc metals becomes more sensitive grain boundary (GB). Lp is the pile-up length and np is the number of pile-

to temperature and strain rate. (3) grain boundaries (GBs) up dislocations.

play more important roles on plastic deformation. A theory

on the mechanical properties of UFG and NC materials

should reasonably explain these characteristics. 2.1 Dislocation pile-up model

For the purpose of this special issue and in order to This model was adopted by both Hall and Petch in their

understand the general role of GBs in the strength of original papers7,8) and has been the most commonly quoted

materials, several representative models to explain the HP model ever since. It is based on the idea of dislocation pile up

relationship will be reviewed brieﬂy in the present study. at a GB,17) as shown in Fig. 1. The pile-up length Lp and the

Then, a dislocation model to incorporate the above char- number of dislocations np are related to each other as18,19)

acteristic mechanical properties of UFG and NC metals

Lp ¼ np ®b=A¸ e ; ð2Þ

will be introduced and used to explain some experimental

results. where ® is the shear modulus, b the magnitude of the Burgers

vector, A a dimensionless constant of about two and ¸ e is a

2. Representative Models and Theories of the Hall part of the applied shear stress ¸ which contributes to the

Petch Relationship dislocation pile up. It is known that the stress concentration

at the pile-up front is ¸ e times the number of piled-up

Following the pioneering work by Hall7) and Petch,8) many dislocations np, i.e., np ¸ e .18,19) If this stress concentration

experimental and theoretical studies2,916) have been con- reaches a critical value ¸ c which is enough for the nucleation

ducted to show the linear relationship between yield or ﬂow of a new dislocation in the adjacent grain, yielding of the

stress and inverse square root of grain size. polycrystal is considered to occur. The condition of the

yielding thus becomes

· ¼ · 0 þ kHP d 1=2 ; ð1Þ

¸ c ¼ np ¸ e : ð3Þ

where · is the yield or ﬂow stress, · 0 the friction stress,

kHP the HallPetch coefﬁcient and d the grain size. Although With eqs. (2) and (3) together with the assignment of Lp =

main focus in recent studies may be placed on the behavior d/2 and ¸ ¼ ¸ 0 þ ¸ e where ¸ 0 is the friction shear stress,

of UFG and NC materials including the so-called HP we have

breakdown or inverse HP phenomena, only models to

¸ c ¸ 2e d=®b; ð4Þ

explain the classic HP law of eq. (1) will be reviewed in

this study. and

+

¸ ¼ ¸ 0 þ ¸ e ¼ ¸ 0 þ ð¸ c ®bÞ1=2 d1=2 : ð5Þ

Corresponding author, E-mail: kato@materia.titech.ac.jp

20 M. Kato

md d

2t

forests in a grain.

d

Therefore, we arrive at

· ¼ · 0 þ · e ¼ Mð¸ 0 þ ¸ e Þ ¼ · 0 þ kHP d1=2

Fig. 3 Cross section of cubic grains of grain size d with work-hardened GB

with kHP ¼ Mð¸ c ®bÞ1=2 ; ð6Þ layers of thickness 2t.

where M is the Taylor orientation factor, · = M¸, · 0 ¼ M¸ 0

and · e ¼ M¸ e ¼ kHP d1=2 .

·ð¾Þ ¼ · 0 ð¾Þ þ kHP ð¾Þd1=2 ; ð10Þ

2.2 Boundary source model

Although the pile-up model originally developed for iron where ¾ is tensile (or compressive) plastic strain which is

has been frequently quoted to explain the HP relationship, related to the shear plastic strain £ as £ ¼ M¾.

some concerns of this model in early 1960’s were that (1) Meakin and Petch22) assumed that the average slip distance

s

the FrankRead source was generally accepted but not very L of glide dislocations was comparable to the grain size and

frequently observed, and (2) no dislocation pile-ups were the shear plastic strain could be written as

found in iron. These led Li to propose the boundary source

£ ¼ μbLs : ð11Þ

model.20) He has considered that dislocations are generated at

GB ledges and all these dislocations form dislocation forests Combining eq. (11) with eq. (8), one readily obtains

in grain interiors.

· ¼ · 0 þ M¡®fbð£=¢Þg1=2 d 1=2

As shown in Fig. 2, suppose that a grain has a cubic shape

with side length d and there are m ledges per unit length of ¼ · 0 þ M¡®fbðM¾=¢Þg1=2 d 1=2 ; ð12Þ

a boundary. Since each GB has two abutting grains and the by assigning

left and right GBs in Fig. 2 have md ledges each, they

Ls ¼ ¢d with 0 < ¢ 1: ð13Þ

generate md dislocations of length d per grain. When these

dislocations move and form forest dislocations in the grain At a given grain size, this model predicts parabolic work

interior, the forest dislocation density μ f becomes hardening (eq. (12)). Furthermore, at a given plastic strain,

the model assumes that the dislocation density is inversely

μ f ¼ md 2 =d3 ¼ m=d: ð7Þ

proportional to the grain size, as can be seen from eqs. (11)

On the other hand, the well-known Taylor equation is written and (13). In fact, Conrad and co-workers showed that these

as were really the case.2325)

pﬃﬃﬃ

· ¼ · 0 þ M¡®b μ ; ð8Þ

2.4 Composite model

where ¡ is a constant of about 0.3 to 0.5 and μ the dislocation Models belonging to this category consider that a

density. Regarding μ f and μ in eqs. (7) and (8) are the same, polycrystalline material is made of two regions; grain

we obtain interiors with lower ﬂow stress · i and GB work-hardened

layers with higher ﬂow stress · b .2629) When a composite

· ¼ · 0 þ M¡®bm1=2 d1=2 : ð9Þ

made of cubic grains with grain size d and GB layer thickness

Aside from slight numerical difference, eq. (9) is the same 2t are considered, as shown in Fig. 3, the ﬂow stress · of this

as eq. (7) in Li’s paper:20) · ¼ · 0 þ ¡®bð8m=³ Þ 1=2 d1=2 . In composite can be written from a simple rule of mixture as

fact, Li compared the magnitude of · in his model with that 2

ðd 2tÞ2 d ðd 2tÞ2

of the pile-up model and reasonable agreement was found.20) ·¼ ·i þ ·b

d2 d2

Since no dislocation pile up is needed, the boundary source t 2

model has been paid much attention, too. t

¼ · i þ 4ð· b · i Þ 4ð· b · i Þ : ð14Þ

d d

2.3 Work hardening model Meyers and Ashworth29) considered a more detailed

The above two models do not contain plastic strain in the geometry for spherical grains to obtain

formulation. In this sense, the derived HP eqs. (6) and (9) are t t 2

applicable to the yield stress of polycrystalline materials. On · ¼ · i þ 8ð· b · i Þ 16ð· b · i Þ : ð15Þ

d d

the other hand, models have been developed to explain the

HP relationship for ﬂow and fracture stresses. For example, The ﬁrst and second terms of the right-hand side of eq. (15)

the HP equation at an arbitrary plastic strain can be written are dominant for large grains of d º t which is usually

as21) the case for coarse-grained materials. Then, not the d 1=2

HallPetch Relationship and Deformation Model of UFG Metals 21

Grain size, d / μm

100 10 1.0 0.5 0.2 0.1 (a) d

300

250

Stress, σ / MPa

200 τ

void

150 (b) γ 0 γ

overlap

100 τ

50

0

0 0.5 1.0 1.5 2.0 2.5 (c)

− 1/2 − 1/2

d / (μm)

Statistically stored (SS) Geometrically necessary (GN)

Fig. 4 Relationship between stress · and inverse square root of grain size d

predicted from eqs. (15) and (16). Numerical values of · i ¼ 20 MPa, Fig. 5 (a) Deforming three cubic grains. (b) If the plastic strain of the

· b ¼ 280 MPa and ² ¼ 0:125 µm1/2 were chosen. center grain happens to be smaller than that of the other two grains, voids

and overlaps are created at the GBs of the center grain. (c) Uniform

deformation £ creates statistically stored (SS) dislocations while non-

uniform deformation causes generation of geometrically necessary (GN)

dependence but the d1 dependence of the ﬂow stress is dislocations to accommodate the voids and overlaps.

naturally expected from the composite model.

For the composite model to explain the HP relationship,

it is necessary to assume that GB layer thickness 2t is an From eqs. (8), (17) and (19), the ﬂow stress of the dislocation

increasing function of grain size such as29) density model becomes31)

t ¼ ²d1=2 ; ð16Þ pﬃﬃﬃ C1 C2 1=2

·ð¾Þ ¼ · 0 þ M 3=2 ¡®b ¾ þ : ð20Þ

where ² is an adjustable parameter. This assumption may be bLs bd

justiﬁed since larger grains can accumulate more dislocations If GB contribution dominates, GN dislocations govern

in work-hardened GB layers so that the layer thickness the strength and the above equation reduces to the HP

increases with increase in grain size. Then, from eqs. (15) relationship:

and (16), we ﬁnd that d1=2 dependence of · is satisﬁed for pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

larger grain size and as grain size becomes smaller, the slope ·ð¾Þ ¼ · 0 þ M 3=2 ¡® C2 b¾ d1=2 : ð21Þ

of the curve becomes smaller, as shown in Fig. 4. This equation has been compared with the ﬂow stress of

many metals and satisfactory agreement was found.32,33)

2.5 Dislocation density model Ashby’s idea of SS and GN dislocations has led to the

This model is based on the idea that dislocations in establishment of so-called strain-gradient plasticity.3439)

materials are divided into two categories; statistically stored With this approach, a length scale is introduced in the classic

(SS) dislocations and geometrically necessary (GN) ones.30) size-independent plasticity theory. Since GN dislocations

Uniform deformation accumulates SS dislocations in grain are associated with non-uniform deformation, they can be

interiors whereas non-uniform deformation creates GN dis- connected with local gradient of strain, i.e.,

locations to accommodate material overlaps or voids at GBs.

1 @£ ©

Suppose applied shear stress ¸ has induced plastic strain £ μg ¼ ; ð22Þ

in the left and right grains and no plastic strain in the center b @l b

grain, as schematically shown in Fig. 5. The SS dislocation where l is a length scale and © the strain gradient.3439) If the

density is expressed, similar to eq. (11), as length scale can be taken proportional to grain size d so that

l ¼ C3 d (0 < C3 1), and when the average strain gradient

C1 £ C1 ¾

μs ¼ s

¼M s; ð17Þ over a grain is expressed as © ¼ £=C3 d (£: strain

bL bL amplitude over the length l), eq. (22) becomes

where C1 is a constant depending on the shape, orientation

£

and distribution of grains. Equation (17) indicates that the SS μg ¼ : ð23Þ

dislocation density is independent of the grain size. On the C3 bd

other hand, the number of GN dislocations ng near the GBs This is similar to eq. (19) showing that GN dislocation

of the center grain can be written as30) density is inversely proportional to grain size. Therefore, the

HP type d1=2 dependence of ﬂow stress can be obtained

ng ¼ C2 £d=b; ð18Þ

from eqs. (8) and (23).

where C2 is another geometrical constant. Therefore, GN Though the idea of SN and GN dislocations and the

dislocation density in the center grain becomes30) discussion based on the scale-dependent plasticity are very

n g d C2 £ C2 ¾ useful, it cannot be applied to the initial yield stress of well-

μg ¼ ¼ ¼M : ð19Þ annealed materials since SS and GN dislocations are not

d3 bd bd

accumulated before the onset of plastic deformation.

22 M. Kato

To explain the temperature and strain-rate dependence of

yield and ﬂow stresses of polycrystals, thermally-activated A

deformation processes have been discussed in conjunction

with the HP equation. Using the pile-up model and differ-

entiating both sides of eq. (6) with respect to ln ¾_ where ¾_ is

the tensile (compressive) strain rate, we have depinning GB

L

@· @· 0 @¸ 1=2

¼ þ Mð®bÞ1=2 c d1=2 : ð24Þ Fig. 6 Schematic of dislocation depinning at a GB. Bowing-out dislocation

@ ln ¾_ @ ln ¾_ @ ln ¾_ A under applied stress is pinned by two GB pinning points of separation

On the other hand, activation volume is generally deﬁned L. If thermally-activated depinning occurs at one of the two GB pinning

as points, dislocation A changes into dislocation B keeping the same radius

of curvature. The area surrounded by the two dislocations A and B is the

@ ln £_ @ ln ¾_ activation area.

v kB T ¼ MkB T ; ð25Þ

@¸ @·

where kB ¼ 1:381 1023 J K1 is the Boltzmann constant.

From eqs. (24) and (25), we arrive at the following investigators have found that experimentally observed rate

expression16,4042) parameters, such as activation volume and strain-rate

sensitivity for fcc UFG and NC metals, can be explained

1 1 kHP

þ d1=2 ; ð26Þ reasonably by this model.6467)

v v0 2M¸ c vc

Analytical formulation of the dislocation bow-out and

where v*0 MkB T ð@ ln ¾_ =@· 0 Þ represents thermally-activated depinning model is summarized as follows.57,58) The yield

deformation in grain interiors and v*c MkB T ð@ ln ¾_ =@· c Þ stress · y of a UFG or NG material consists of athermal ð· a Þ

with M¸ c ¼ · c is for the GB region. When the term ¸ c v*c is and thermal ð· Þ stress components as

constant, eq. (26) predicts the HP-type relationship between

· y ¼ · a þ · ¼ Mð¸ a þ ¸ Þ: ð27Þ

v1 and d. In fact, from experimentally found such HP

behavior in fcc polycrystals, Armstrong and co-workers have Here, the athermal component is written as

interpreted that v*0 values represent the in-grain dislocation

®b d

intersection with forest dislocations and v*c values represent ¸a ¼ ln ; ð28Þ

cross slip enhanced by stress concentration near GBs16,4042). 2³d 10b

For UFG metals, Conrad and co-workers have also and the thermal component as

conducted thermal activation analysis4347) and essentially " #

_ 2=3

kB T lnð£_ 0 =£Þ

the same equation as eq. (26) has been obtained.14) They ¸ ¼ ¸m 1 ; ð29Þ

have concluded that deformation kinetics of UFG metals with G0

d between 10 and 100 nm (Regime II in their studies) is with

controlled by GB shear promoted by the dislocation pile-up.

3®b d þ 2

It appears that despite the fact that dislocation pile-ups are ¸m ¼ ln ; ð30Þ

2³ðd þ 2 Þ 30b

not necessarily observed, the pile-up model has been used

most extensively, in particular to discuss thermally-activated and

deformation processes in polycrystals.

Gð¸ Þ

£_ ¼ £_ 0 exp : ð31Þ

kB T

3. Deformation Kinetics of UFG and NC Materials

In the above equations, £_ is the shear strain rate, Gð¸ Þ and

As mentioned in Introduction, discussion on thermally- G0 are the activation energies with and without ¸ ,

activated deformation kinetics is indispensable to understand respectively, the minimum GB source length of dislocations

mechanical properties of UFG and NC materials. Further- that emit and bow out from GBs and £_ 0 ¼ 1 107 s1 is

more, for these materials, many studies have pointed out that assumed.58)

partial or perfect dislocations emitted from GBs play essential Geometrically-derived activation volume v*d of the

roles in the plastic deformation.4858) Some investigators depinning process in Fig. 6 can be obtained as58)

believe that dislocations once nucleated at a GB would cross

sﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

the grain rapidly without stopping in a grain.51,59,60) On the L þ w L þ w L þ w 2

vd ¼ r2 b sin1 r2

other hand, it has been pointed out that as a propagating 2r 2 2

2 3

dislocation traverses the grain towards the opposite boundary, sﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

2ﬃ

L L L 5

its two ends may be pinned by GB impurities or 4r2 b sin1 r2 ; ð32Þ

ledges.56,61,62) When such pinning occurs, the depinning 2r 2 2

process can be a rate-controlling step of the thermally-

activated deformation of UFG materials.5658,6163) where L is the distance between the pinning points,

Using the simpliﬁed geometry shown in Fig. 6, Kato

®b L

analyzed the thermally-activated depinning process at a GB r¼ ln ð33Þ

4³¸ 10b

as a glide dislocation bows out into a grain.58) Later, some

HallPetch Relationship and Deformation Model of UFG Metals 23

d / nm 100

250 K

0.12 400 100 25 10 Ni

350 K

80 calculated

0.10

Ni

450 K

calculated

vd* / b 3

300 K 60 d = 100 nm

0.08

−3

d = 300 nm 50 K

/b

150 K 150 K

40

0.06 250 K

−1

10 K d = 30 nm

350 K

vd*

20 150 K

0.04 350 K 50 K

250 K

0.02 0

0 0.5 1.0 1.5 2.0

0

0 0.05 0.1 0.15 0.2 0.25 0.3 σ y / GPa

− 1/2 − 1/2

d / (nm) Fig. 8 Stress dependence of the activation volume v*d predicted by the

bow-out and depinning model58) with numerical values of Ni for three

Fig. 7 Calculated relationship between the reciprocal activation volume grain sizes. At a ﬁxed grain size, the yield stress ·y is calculated as a

v*1

d and square root of grain size d by using the bow-out and depinning function of temperature. Note that anomalous positive stress dependence

model58) with numerical values of Ni. Note that near HP relationship found by Conrad et al.14,4547,68) can be reproduced by the present model.

holds between vd*1 and d and that the activation volume is a decreasing

function of temperature.

dislocations.14,4547,68) Kapoor and Chakravartty have also

is the radius of curvature for the bowing-out dislocation found the anomalous stress dependence of v from an

and experiment using UFG Al-Mg alloy.69) They pointed out that

dislocation-solute interaction may be a possible origin of this

w ¼ bf1 ð¸ =¸ m Þg1=2 ð34Þ

v · behavior.

is the activation distance. The relationship between v*d and · y can also be derived

Since this model is already known to predict the HP-type from the present bow-out and depinning model since v*d can

relationship between yield stress and grain size at a chosen be expressed as a function of ¸ from eqs. (29), (32) and (33).

deformation temperature,57,58) some new implications of The calculated results are shown in Fig. 8. Indeed, we

the model relating to the thermally-activated deformation ﬁnd that v*d becomes an increasing function of · y

process will be discussed below. First, let us examine (¼ M ð¸ a þ ¸ Þ). It is encouraging to know that not only

whether the reciprocal of the activation volume deﬁned the vd · y relationship but also the predicted values of v*d

in eq. (32) shows the HP-type behavior with respect to the are in quantitative agreement with experimental data obtained

grain size. For this purpose, numerical values for Ni for Ni.56) In conclusion, we can say that the present model

will be chosen as in the previous study:58) ® ¼ 79 GPa, of dislocation bow-out and depinning can explain many

b ¼ 0:249 nm, G0 ¼ 2:0 eV ð¼ 3:20 1019 JÞ, £_ ¼ 1 observed characteristics of deformation kinetics of fcc UFG

104 s1 , £_ o ¼ 1 107 s1 , L ¼ ðd þ 2 Þ=3 and = and NC materials.

10 nm. Figure 7 shows the relationship between v*1 d and

d1=2 calculated from eq. (32). Three curves are for three 4. Concluding Remarks

different temperatures; 10, 150 and 300 K. It can be seen

that the curves are nearly straight, in particular, when d is This paper consists of two parts. In the ﬁrst part, several

larger than about 25 nm. Therefore, the HP-like behavior, representative models to explain the HP relationship were

as discussed in section 2.6, approximately holds between reviewed. In the second part, recently developed dislocation

the reciprocal activation volume and grain size in Kato’s bow-out and depinning model has been used to explain some

model, too. aspects of deformation kinetics in UFG and NC materials

It should be noted from Fig. 7 that for a given grain size, together with the HP-like behavior of reciprocal activation

vd*1 is an increasing function or v*d is a decreasing function volume as a function of grain size.

of temperature. This unique and anomalous behavior, Although it appears that the dislocation pile-up model is

different from that for coarse-grained polycrystals, has been still the most frequently adopted one to explain the HP

noted14,45,56) and some researchers discussed it using Kato’s relationship, the other models have their own merit and

model.6467) advantages. Furthermore, seeing the fact that the HP

Relating to the above anomalous temperature dependence relationship applies not only to yield stress but also to ﬂow

of activation volume, Conrad14,45) and Conrad and Yang68) and fracture stresses and even to fatigue and creep,70)

have shown for their regime II of the grain size (d µ it appears that the HP-type size dependence of strength is

101000 nm) that the activation volume v becomes an a rather general result of natural dislocation behavior.

increasing function of the applied stress. According to them, Revealing various aspects of physics behind the HP law

this anomalous stress dependence of v is also consistent with certainly remains to be an attractive and challenging research

their proposed rate-controlling process for fcc UFG materials subject.

24 M. Kato

Acknowledgement 33) N. Hansen: Strength of Metals and Alloys, ed. by P. Haasen, (Pergamon

Press, Oxford, 1979) pp. 849854.

34) E. C. Aifantis: Int. J. Plasticity 3 (1987) 211247.

This study was supported by a Grant-in-Aid for Scientiﬁc 35) N. A. Fleck and J. W. Hutchinson: J. Mech. Phys. Solids 41 (1993)

Research on Innovative Area “Bulk Nanostructured Metals” 18251857.

through the Ministry of Education, Culture, Sports, Science 36) N. A. Fleck, G. M. Muller, M. F. Ashby and J. W. Hutchinson: Acta

and Technology, Japan (contract No. 22102006). Metall. Mater. 42 (1994) 475487.

37) H. Gao, Y. Huang, W. D. Nix and J. W. Hutchinson: J. Mech. Phys.

Solids 47 (1999) 12391263.

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