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www.elsevier.com/locate/actamat

ultraﬁne-grained metastable austenitic stainless steel

S. Rajasekhara, P.J. Ferreira ⇑

Materials Science and Engineering Program, The University of Texas at Austin, TX 78712, USA

Available online 31 October 2010

Abstract

A generalized phase transformation kinetics model is used to understand the martensite to austenite transformation in a cold-rolled

and annealed metastable AISI 301LN ultraﬁne-grained austenitic stainless steel. The model shows that the presence of interstitial nitro-

gen and heavy cold-rolling is important to promote fast transformation kinetics, through rapid nitrogen-diﬀusion and austenite nucle-

ation at austenite/martensite phase boundaries.

Ó 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

and Cohen [10] demonstrated for the ﬁrst time, the reverse

The process of heavy cold-rolling and subsequent short- martensite transformation (a0 ? c) in a Fe–33.5% Ni alloy.

time annealing of metastable austenitic stainless steels (SS) Subsequently, Breedis [11] showed that in Fe–Cr–Ni alloys

has generated considerable interest in the research commu- the reversion products consisted of thin austenitic twins

nity and industry because SS with ultraﬁne austenite grains formed in a martensitic matrix. Jana and Wayman [12],

may be achieved. The presence of ultraﬁne grains results in Kessler and Pitsch [13] and Guy et al. [14] showed

SS with high strength and ductility, making these materials experimentally that, depending on the SS composition and

desirable for use in structural and automotive industries. heating rates, the a0 ? c transformation may be a time-

This concept has been demonstrated in specialty non- dependent phenomenon where the austenite phase fraction

commercial SS grades [1,2], and more recently in commer- increases as a function of annealing time. Montaneri [15]

cial AISI 301, 301LN and 304 SS grades [3–9]. In fact, performed internal friction and dynamic modulus experi-

excellent mechanical properties with yield strengths exceed- ments on a 95% cold-rolled and annealed AISI 304 SS,

ing 700 MPa and elongation of approximately 35% were and observed that an incubation time preceded the start of

reported in cold-rolled and annealed AISI 301LN SS [8,9]. the a0 ? c transformation. The occurrence of this incuba-

The basis for these properties relies on initially cold rolling tion period was attributed to the stress relaxation of the

a metastable austenitic SS to form lath- and dislocation- parent martensite phase and the diﬀusion of interstitial

cell-type martensite (a0 ) which, upon annealing, transform atoms to the a0 /a0 interface during annealing.

into ultraﬁne austenite (c) grains. More recently, Tomimura et al. [16] demonstrated that,

In the past, several studies have qualitatively discussed depending on the alloy composition, austenite nucleates at

the a0 ? c phase transformation in various SS grades, martensite grain boundaries and grows in size when heated

for long annealing durations. According to Tomimura

⇑ Corresponding author. Tel.: +1 512 471 3244; fax: +1 512 471 7681. et al. [16], the initial shape of the austenite grains depends

E-mail address: ferreira@mail.utexas.edu (P.J. Ferreira). on the morphology of the parent martensite phase. If the

1359-6454/$36.00 Ó 2010 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

doi:10.1016/j.actamat.2010.10.012

S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748 739

cold-rolled martensite structure is lath-type, the austenite where they assume that the embryos of a new phase nucle-

phase nucleates at the lath boundaries and intersections, ate randomly from the time-dependent parent phase. In the

and grows from these sites into the martensite lath. On the case of the a0 ? c phase transformation, this relationship

other hand, if the parent martensite morphology is disloca- may be expressed as:

tion-cell-type (comprising dislocation forests and ultraﬁne Z

4p t 3 3

lath martensite), equiaxed ultraﬁne austenite grains nucleate lnð1 nc ðT ; tÞÞ ¼ v ðT ; tÞJ ðT ; tÞðt sÞ ds ð1Þ

3 0

at martensite grain boundaries. The present authors and

other research groups have consistently observed these ﬁnd- where nc(T, t) is the time (t) and temperature (T) dependent

ings in several cold-rolled and annealed commercial and spe- austenite phase volume fraction, v(T, t) the austenite grain

cialty SS grades [17–20]. Qualitatively, this time-dependent growth velocity, J(T, t) the austenite phase nucleation rate

“diﬀusion-type” mechanism is characterized by: (i) a wide and s the incubation time for the formation of the ﬁrst aus-

annealing temperature range; (ii) the formation of defect- tenite nuclei. For simplicity, we assume the nucleation rate

free equiaxed austenitic grains which grow in size with time; to be independent of annealing duration. Eq. (1) thus re-

(iii) a wide austenite grain size distribution; and (iv) possible duces to:

formation of secondary phase precipitates [18]. Z

4pJ ðT Þ t 3 3

Clearly, there is experimental and phenomenological lnð1 nc ðT ; tÞÞ ¼ v ðT ; tÞðt sÞ ds ð2Þ

3 0

evidence that seem to conﬁrm the diﬀusion-type phase

transformation mechanism in cold-rolled and annealed While the term J(T) will be discussed later, the integral in

ultraﬁne-grained austenitic SS. However, despite the avail- Eq. (2) may be solved by using an explicit time and temper-

able work, there is a lack of quantitative understanding ature dependence relationship for v(T, t), which is given by

regarding the kinetics of the a0 ? c phase transformation. [20]:

In addition, several fundamental concepts involved in this 1

phase transformation, such as: (i) the type of the diﬀusing ðktÞn

vðT ; tÞ ¼ ð3Þ

species driving the phase transformation; and (ii) the nat- nt

ure of austenite/martensite grain boundary junctions where where k is the austenite grain growth parameter, n is the

the transformation occurs are not yet known. An under- austenite grain growth exponent and t is the annealing

standing of these factors is critical for tailoring the compo- time. As has been discussed elsewhere [20,23–26], the grain

sition of metastable austenitic SS grades, as well as for growth parameter k is a measure of the material’s grain

optimizing the cold-rolling procedure and subsequent boundary mobility, which depends on annealing tempera-

annealing to promote an eﬃcient a0 ? c transformation, ture and grain growth activation energy, while the grain

which can lead to the production of ultraﬁne-grained SS. growth exponent n depends on the annealing temperature,

In this work, we apply the general phase kinetics rela- grain orientation, texture, residual strain and soluble impu-

tionship proposed by Erukhimovitch and Baram [21,22], rities. By combining Eqs. (2) and (3), the generalized phase

and quantitatively address the a0 ? c phase transformation transformation kinetics relationship can be rewritten as:

in a cold-rolled and annealed metastable ultraﬁne-grained Z 1

!3

austenitic AISI 301LN SS grade, the composition of which 4pJ ðT Þ t ðktÞn 3

lnð1 nc ðt; T ÞÞ ¼ ðt sÞ ds ð4Þ

is shown in Table 1. The AISI 301LN SS is an ideal candi- 3 0 nt

date for this study because: (i) it has a wide commercial use;

(ii) it exhibits a very rapid (1–100 s) diﬀusion-driven a0 ? c Solving Eq. (4) for nc(T, t), we obtain the expression

transformation within a wide annealing temperature range 3 3

!

(700–1000 °C) [8,18]; and (iii) there is experimental phase 4pJ ðT Þk n tnþ4

nc ðt; T Þ ¼ 1 exp ð5Þ

fraction and grain size data against which our analysis 3n3

may be compared [8,18,20].

Eq. (5) gives the austenite phase fraction nc as a function of

2. Kinetics model grain growth kinetic parameters k, n and the nucleation

rate J(T). Not surprisingly, Eq. (5) has a form similar to

2.1. Basis for the model the kinetics relationships developed by Avrami [27,28]

and Johnson and Mehl [29]. However, Eq. (5) is written

Erukhimovitch and Baram [21,22] proposed a general in terms of experimental parameters, namely the nucleation

kinetics relationship for solid-state phase transformations rate J(T) and the grain growth parameters k and n.

Table 1

Weight percent and mole fractions of the various elements present in AISI 301LN SS.

C N Ni Cr Mn Si Cu Mo Fe

wt.% 0.017 0.15 6.5 17.3 1.29 0.52 0.2 0.15 Balance

Mole fraction 0.0008 0.006 0.063 0.186 0.013 0.005 0.002 0.002 0.744

740 S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748

According to classical nucleation theory, the time- grain boundary area of the eliminated a0 /a0 interface and

dependent nucleation rate J(T, t) in solid-state transforma- the volume free energy change DGv(T). Thus, DG(T)

tions is given by [30,31]: may be expressed as [33]:

s

DG 4ðbra0 =c ara0 =a0 Þ

3

J ðT ; tÞ ¼ ZbC 1 exp exp ð6Þ DG ðT Þ ¼ ð10Þ

kBT t 27c2 ðDGv ðT ÞÞ

2

where Z is the Zeldovich non-equilibrium factor that ac- where a is the eliminated martensite grain boundary area

counts for the nuclei that exceed the critical nucleus size, during the a0 ? c phase transformation, b is the new aus-

b is the rate at which atoms are added to the critical nu- tenite/martensite grain boundary area, c is the new austen-

cleus, C1 is the concentration of available nucleation sites, ite nucleus volume [33] and DGv(T) is the volume free

DG is the activation energy for heterogeneous austenite energy change due to the martensite to austenite transfor-

nucleation and s is the incubation time. As mentioned pre- mation. The parameters a, b and c depend on the geometry

viously, we initially assume the nucleation rate to be con- of the nucleating grain (to be discussed later). On the basis

stant within 1–100 s of annealing. Later, in Section 3, we of Eqs. 7, 8a, 8b, 9, 10, Eq. (5) may be rewritten as:

will show that this assumption is justiﬁed. Thus, the time- 3 1

0 DG ðT Þ

independent nucleation rate may be written as: 4pZðT ÞbðT ÞC gb exp

3

k n tnþ4

1

@

nc ðt; T Þ ¼ 1 exp

kB T

A

DG 3n3

J ðT Þ ¼ ZbC 1 exp ð7Þ

kBT

ð11Þ

The relationships for Z and b have been developed by

Johnson et al. [31], and modiﬁed for the speciﬁc case of where all the terms retain their previous deﬁnitions. At this

austenite nucleation as shown below: point, to calculate nc(t, T) we still need to determine

DG(T). Therefore, the values for the a0 /c interfacial

2

V a0 Fe ½DGv ðT Þ energy, the a0 /a0 interfacial energy, the volume free energy

ZðT Þ ¼ pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ ð8aÞ

8p k B TK j ra0 =c change DGv(T), the martensite grain boundary width d gb a0 ,

the grain size da0 and the magnitudes of a, b and c for dif-

16pr2a0 =c DðT ÞLj ferent austenite/martensite grain junctions in Eq. (10) must

bðT Þ ¼ 2

ð8bÞ

a4a0 ðDGv ðT ÞÞ be found. We estimate these parameters in the subsequent

sections.

where Va 0 Fe is the average volume of an iron atom in the

martensite phase, DGv(T) is the Gibbs free energy change

2.2. Estimation of the interfacial energies ra0 /a 0 and ra/c

per unit volume of martensite to austenite phase transfor-

mation, Kj and Lj are geometric parameters that depend

When an austenite grain nucleates within the martensite

on the a0 -phase and c-phase interfacial energies, D(T) is

matrix, the martensite grain boundary is eliminated and a0 /

the temperature-dependent diﬀusion coeﬃcient of the spe-

c interface is created. Prior research has shown that

cies that govern the martensite to austenite transformation,

h1 1 0i-type austenite (fcc) boundaries form at h1 1 1i-type

ra 0 /c is the martensite–austenite interfacial energy, and aa 0 is

martensite (bcc) boundaries [34,35]. Keeping this in mind,

the martensite lattice parameter.

and based on theoretical grain boundary calculations per-

To calculate J(T) in Eq. (7), we further need to estimate

formed by Shibuta et al. [36] for a specialty Fe–Cr alloy,

C1, the concentration of nucleation sites available for aus-

the bcc phase h1 1 1i-type grain boundary energy ra0 /a 0 is

tenite nucleation, which depends on the type of nucleation

assumed to be approximately 1.3 J m2 [35]. Furthermore,

sites considered. On the basis of several studies on cold-

because the interfaces are crystallographically related

rolled SS grades and Fe–X alloys [7,8,16,17,32], we have

through the Nishiyama–Wasserman (½110c ==½11 1a0 ) rela-

assumed that the austenite nucleates on martensite grain

tionship [34,35,37], we assume that the energy of the new

boundaries. The concentration of martensite grain bound-

a0 /c interface is equal to the eliminated a0 /a0 interface. This

aries C gb 1 available for austenite nucleation is estimated

is a reasonable assumption, as discussed by Gjostein et al.

according to [26]:

[38], who have experimentally determined the bcc/fcc inter-

dgb facial energy ratio for Fe–C alloys to be approximately 1.

a0

C gb

1 ¼ C 0 ; ð9Þ

da0

2.3. Estimation of the volume free energy change DGv(T)

where C0 is the total equilibrium concentration of nucle-

ation sites available, d gb

a0 is the martensite grain boundary DGv(T) is the free energy change per unit volume

width and da0 is the average martensite grain size. between the product-phase austenite and the parent-phase

Finally, to determine J(T) in Eq. (7), the activation martensite. It can be expressed (in J m3) as:

energy for heterogeneous nucleation DG(T) must be calcu-

0

lated. DG(T) depends on the volume of the austenite Gc ðT Þ Ga ðT Þ

DGv ðT Þ ¼ ð12Þ

nucleus, the grain boundary area of the a0 /c interface, the Vc Va

0

S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748 741

0

where Gc(T) and Ga (T) are the free energies per mole of the parameters describing the interaction between the ith and

0

austenite and martensite phases respectively, and Vc, Va the jth element in the respective phases. Miettinen has

the molar volumes of austenite and martensite phases tabulated the ﬁrst-order interaction parameters Lij, for

respectively. The free energy per mole contribution of an the bcc and the fcc phases in commercial SS, to determine

element j in the martensite and austenite phases can be the excess free energy in the respective phases [40,42].

written as [39,40]: Finally, we ignore the magnetic ordering contribution to

Xn X

n the free energy because, as has been discussed elsewhere

0 0 0 0

Ga ðT Þ ¼ xj Gaj ðT Þ þ xj RT lnðxj Þ þ Gaxs ðT Þ þ Gam ðT Þ [40], their values are close to zero above room temperature.

j¼1 j¼1 Thus Eq. (11) may be rewritten as:

ð13aÞ Pn Pn P Pn

c

j¼1 xj Gj ðT Þ þ lnðxj Þ þ n1

j¼1 xj RT i¼1

c

j¼iþ1 xi xj Lij

DGv ðT Þ ¼

X

n X

n V c

j¼1 xj Gj ðT Þ þ j¼1 xj RT lnðxj Þ þ i¼1 j¼iþ1 xi xj Lij

j¼1 j¼1 0 ð17Þ

Va

ð13bÞ The mole fractions of the elements (xi and xj) present in

where xj is the mole fraction of the jth element present in AISI 301LN SS are shown in Table 1. The relationships for

0

the SS grade, Gaj ðT Þ and Gcj ðT Þ are thePstandard free energy the free energy contributions by individual elements to the

n

of the jth element in a0 and c phases, j¼1 xj RT lnðxj Þ is the a0 and c phases, as well as various interaction parameters,

free energy contribution due to the entropy of mixing in the are shown in Appendix A. Finally, since the lattice param-

0

respective phases, Gaxz ðT Þ and Gcxs ðT Þ are the excess free en- eters of the c and a0 phases are ac 3.56 Å and aa0 2.85 Å

ergy due to the interaction between the various elements respectively [7], the molar volumes of austenite and

0 0

present in SS with each other, and Gam ðT Þ and Gcm ðT Þ are martensite phases, Vc and Va were determined to be 5

6 6 3 1

the magnetic ordering contributions by the various ele- 10 and 4.7 10 m mol , respectively.

ments to the respective phases. According to Dinsdale On this basis, DGv(T), given by Eq. (17), was determined

[41], the free energy of any ith phase as a function of tem- as a function of temperature. Not surprisingly, its value is

perature, is given by the power series expansion in terms of negative and decreases with temperature (Fig. 1a), which

temperature (T): implies that the a0 ? c transformation is favored as the

X annealing temperature is increased. Aaronson et al.

Gij ðT Þ ¼ A þ BT þ CT lnðT Þ þ DT n þ Gpres ð14Þ [43,44] have observed a similar trend for nucleation kinetics

in Fe–X alloys. To validate whether the DGv(T) values

where A, B, C and D are coeﬃcients of the power series shown in Fig. 1a were realistic, we have calculated the typ-

expansion, n represents a set of integers 2, 3 and 1, and ical austenite nuclei radius formed during the a0 ? c phase

Gpres the pressure dependent contribution to the Gibbs free transformation according to [31]:

energy respectively. Dinsdale [41] has determined the mag-

nitudes for constants A, B, C and D for the bcc and fcc 2ra0 =c

rðT Þ ¼ ð18Þ

phases due to individual elements.

P We have ignored the DGv ðT Þ

higher order terms given by DTn because calculations re-

The results are shown in Fig. 1b. The austenite nuclei radii

veal that their contribution is negligible. Furthermore, we

for the temperature range 700–1000 °C is estimated to lie

have ignored Gpres because its contribution is negligible at

between 9 and 10.5 Å, which is typical for diﬀusion-driven

atmospheric pressure conditions under which the cold-

phase transformations [26,45].

rolling and annealing of the SS grades was performed.

Thus, Eq. (14) may be rewritten as follows:

2.4. Estimation of Z(T) and b(T)

Gij ðT Þ ¼ A þ BT þ CT lnðT Þ ð15Þ

Knowing ra0 /a 0 , ra 0 /c and DGv(T), we are now in a posi-

The free energy contributions from individual elements

tion to determine the Zeldovich factor Z(T) and the rate at

present in AISI 301LN SS for the fcc and bcc phase are

which atoms get added to the critical nucleus, b(T). As

reproduced from Dinsdale [41] in Appendix A. The excess

mentioned earlier in Eqs. (8a) and (8b), the geometric

free energy contribution, as described in Eq. (13), for the

factors Kj and Lj depend on the interfacial energies, and

martensite and austenite phases are given by [40]:

are given by [31]:

0

n1 X

X n

0

Gaxs ¼ xi xj Laij ðT Þ ð16aÞ 1

Kj ¼ 3 3 cosðhÞ þ cos3 ðhÞ ð19aÞ

i¼1 j¼iþ1 2

n1 X

X n Lj ¼ 1 cosðhÞ ð19bÞ

Gcxs ¼ xi xj Lcij ðT Þ ð16bÞ

i¼1 j¼iþ1 r 0 0

where cosðhÞ ¼ 2ra =a0 and h is the dihedral angle for three

a =c

where xi and xj are the mole fractions of elements present in typical nuclei shapes (2-, 3- and 4-grain junctions with

0

a multi-component alloy, Laij ðT Þ and Lcij ðT Þ the interaction the parent martensite phase) shown in Fig. 2. As shown

742 S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748

annealing temperature in cold-rolled and annealed AISI 301LN SS grade

and (b) calculated austenite nuclei size as a function of annealing Fig. 2. Austenite nucleation at (a) 2-grain, (b) 3-grain and (c) 4-grain

temperature. austenite/martensite junctions (adapted from Clemm and Fisher [33]).

DGv(T) and Va 0 Fe, but a weak dependence on the type of 2.5. Estimation of the concentration of martensite nucleation

austenite/martensite nucleation sites (2-, 3- or 4-grain junc- sites, C1

tions) available. Since Va0 Fe is constant and DGv(T) changes

gradually with temperature (Fig. 1a), Z(T) is also expected As discussed in Eq. (9), the nucleation rate parameter

to change gradually with annealing temperature and with C gb

1 depends on the equilibrium nucleation sites C0, the

the shape of austenite nuclei. Not surprisingly, the Z(T) martensite grain boundary width d gb a0 and the average mar-

values calculated between 700 and 1000 °C for 2-, 3- and 0 . For AISI 301LN SS, C0 is determined

tensite grain size da

4-grain junction-type nucleation sites range between to be approximately 8:8 1025 atoms m3. The martensite

approximately 0.015 and 0.02, which are comparable to grain boundary width d gb a0 is assumed to be approximately

the values obtained by Johnson et al. [31]. On the other 5 Å [26] and the grain size of martensite grains da0 is deter-

hand b(T), given by Eq. (8b), exhibits a strong dependence mined by analyzing the transmission electron microscopy

on DGv(T) and D(T) but a weak dependence on the type of (TEM) images of heavily cold-rolled AISI 301LN SS

available nucleation sites. (Fig. 3). Image J software (National Institute of Health,

In this work, we assume nitrogen to be the interstitial ele- Bethesda, MD) was used on the scanned TEM negatives

ment driving the a0 ? c transformation. However, for com- of the cold-rolled sample to estimate the martensite grain

parison, we also perform calculations based on chromium size. Keeping in mind that the morphology of lath-type

(substitutional element with the highest concentration and martensite (comprising martensite platelets) is signiﬁcantly

relatively large size) diﬀusion as the rate-limiting factor for diﬀerent from dislocation-cell-type martensite (ultraﬁne

the a0 ? c transformation. With these assumptions, and martensite), area measurements were obtained from a total

knowing that the diﬀusivities of nitrogen DN(T) and of 200 grains comprising both lath-type and dislocation-

chromium DCr(T) (m2 s1) in the bcc phase of a commercial cell-type martensite. Subsequently, based on the average

SS grade are approximately 8 106 expð 0:82 kB T

Þ and area from 200 grains, the average martensite grain size

3 2:48

2:4 10 expð kB T Þ respectively [40], where k B ¼ 8:62 da0 was estimated to be approximately 0.17 lm. By employ-

105 eV =K, bN(T) and bCr(T) are determined to be approxi- ing the average area to determine da0 instead of directly

mately between 1010 and 1011 s1 and between approxi- measuring the size of individual martensite grains, we min-

mately 2.5 103 and 5 107 s1, respectively, for the imized any bias towards grains of a particular morphology

temperature range of 700–1000 °C. (lath-type or dislocation-cell-type). On this basis, the

S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748 743

function of annealing temperature for 2-, 3- and 4-grain austenite/

martensite junctions.

Table 2

Kinetic parameters for grain growth n and k at diﬀerent annealing

temperatures [22].

Annealing Kinetic parameters

temperature (°C)

n k

Fig. 3. TEM bright-ﬁeld image of cold-rolled AISI 301LN SS [18]. The 800 2.8 0.1

lath martensite size da0 was determined to be approximately 0.17 lm. 900 2.8 1.6

1000 2.4 3.6

1 were determined

to be approximately 2.6 1023 m3.

nucleation, DG*(T)

by Eq. (9) may now be determined. As shown in Eq.

(10), the magnitude of DG*(T) depends on the a0 /a0 and

a0 /c interfacial energies (determined in Section 2.2), the vol-

ume free energy change due to the a0 ? c phase transfor-

mation and the geometric parameters a, b and c. Clemm

and Fisher [33] have developed relationships that relate

these geometric parameters to the dihedral angle (h) for

the three typical nuclei shapes with 2-, 3- and 4-grain junc-

tions with the parent martensite phase (Fig. 2), which are

listed in Appendix B.

On the basis of previously calculated interface energies

(Section 2.2) and the volume free energy change, DG(T)

for diﬀerent austenite nuclei shapes has been determined

as a function of annealing temperature (Fig. 4). Clearly,

the activation energy for 4- and 3-grain austenite/martens-

ite junctions is signiﬁcantly lower than that for the 2-grain

austenite/martensite junction.

2.7. Determination of the kinetic parameters – k and n Fig. 5. (a) Exponential regression analysis to determine k value at 700 °C;

(b) linear regression analysis to determine n value at 700 °C.

Finally, to solve Eq. (11), the magnitudes of the grain

growth kinetic parameters k and n are also required. For information and solving the grain growth law for samples

the present work, the grain growth parameters have been annealed at 800, 900 and 1000 °C (Table 2) [20]. The grain

determined by using experimentally known grain size growth law was applied to only these samples because they

744 S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748

are assumed to comprise of only austenite phase [20]. determine its values at 700 °C (Fig. 5a). Determining n val-

According to Table 2, k1000 °C > k900 °C > k800 °C, which is ues is less trivial because of challenges associated with

expected because k is directly proportional to the probabil- modeling grain growth parameter as a function of temper-

ity of atoms moving from one grain to the next [26]. We ature and material system. Burke and Turnbull [46], who

also note that n800 °C n900 °C > n1000 °C. The higher n have evaluated grain growth in various metallic systems

value at 800 and 900 °C is likely due to residual strains (microalloyed carbon steels, aluminum, brass), have sug-

and the high texture from the parent martensite phase. gested that n values increase with decreasing temperature.

Additionally, these samples contain chromium nitride pre- Atkinson [47] reviewed that n values depend on the grain

cipitates [18], which inhibit grain growth and contribute to growth mechanism; speciﬁcally n-values for grain growth

a higher n value. On the other hand, annealing at higher in an impure system by lattice or grain boundary diﬀusion

temperatures relieves the residual strains, dissolves the pre- were 3 or 4, respectively. Vandemeer and Hu [48] tabulated

cipitates and increases the atomic migration along the grain that grain growth exponents in zone-reﬁned Fe alloys to

boundaries, which promote the loss of grain curvature and range between 2 and 4. Gavard et al. [49] experimentally

texture; all of which lead to a decreased n value. Indeed, determined n values in ultra-pure stainless steels to range

samples annealed at 1000 °C exhibit a lower n value. between 2 and 6. In the present context, we have obtained

The samples annealed at 700 °C contain signiﬁcant n-values from linear regression (Fig. 5b). This is a reason-

amounts of martensite, and therefore reliable k and n val- able ﬁrst assumption because it empirically takes into

ues cannot be obtained by applying the grain growth law. account experimental observations of increasing n-values

Therefore, k and n values for samples annealed at 700 °C with decreasing annealing temperatures. Under these con-

have been obtained by applying regression analysis to the ditions, n and k values at 700 °C are found to be approxi-

k and n kinetic parameters at 800, 900 and 1000 °C. k is mately 3.1 and 0.007 respectively.

shown to have an exponential dependence on temperature Naturally, a possible error in calculating the austenite

[26], and thus an exponential regression is employed to phase fraction is introduced by using k and n values for

Fig. 6. Calculated (curves) and experimental (scatter points) austenite phase percentage as a function of annealing time and temperature. (a–c) show the

phase percentage when nitrogen-diﬀusion is assumed to be the rate-limiting step, whereas (d–f) show the phase percentage when chromium diﬀusion is

assumed to be the rate-limiting step.

S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748 745

detailed calculations (not shown here) reveal that changing

the values of k and n (obtained from regression analysis) by

as much as ±50% does not signiﬁcantly inﬂuence the phase

fractions of austenite.

The values of C gb1 , DG (T), Z(T), bCr(T) and bN(T) have

been used in Eq. (11) to determine the percentage of

austenite phase at the annealing temperatures of 700–

1000 °C for the rate-limiting cases of nitrogen and

chromium diﬀusion, when austenite nucleates at 2-, 3-

and 4-grain austenite/martensite junctions (Fig. 6). The

experimental data is also plotted for comparison.

Based on the calculations performed, when the a0 ? c

phase transformation is driven via the expected nitrogen-

diﬀusion, two distinct observations may be made. For the

annealing temperatures of 900 and 1000 °C, calculations

show that complete a0 ? c transformation occurs irrespec-

tive of the type of the a0 /c junction geometry, which agrees

with the available experimental data (Fig. 6a–c). However,

for the lower annealing temperatures of 700 and 800 °C,

the results show that the nature of the a0 /c geometry plays

an important role in the a0 ? c transformation kinetics.

The following observations can be made: (i) the phase

transformation is sluggish relative to the experimental data

when austenite nucleates at 2-grain junctions (Fig. 6a); (ii)

the a0 ? c phase transformation is faster and agrees

reasonably well with the experimental data when austenite

nucleates at 3-grain austenite/martensite junctions

(Fig. 6b); and ﬁnally (iii) for the case of austenite nucle-

ation at 4-grain martensite junctions, our calculations

predict the a0 ? c transformation to be considerably faster

than the experimental observations (Fig. 6c).

For comparison, calculations were also performed for

the case of chromium driven diﬀusion. In this case, the

phase transformation is considerably sluggish relative to

experimental data when austenite nucleates at 2- and 3- Fig. 7. (a) Incubation times preceding the a0 ? c transformation when

grain a0 /c junction geometries (Fig. 6d and e). On the other nitrogen and chromium diﬀusion are the rate-limiting factors. (b, c)

hand, the phase transformation kinetics is considerably fas- Austenite nucleation rates, normalized with respect to a maximum

ter relative to the experimental observations when austenite nucleation rate for a given temperature, as function of annealing time

and temperature assuming nitrogen and chromium diﬀusion, respectively,

nucleates at 4-grain junctions (Fig. 6f). Clearly, in all the

as the rate-limiting factors.

three cases just discussed, the calculated phase transforma-

tion data with chromium diﬀusion as the rate-limiting fac-

tor does not agree with the experimental observations. nitrogen-diﬀusion-controlled austenite nucleation at 3-

The results also show that the a0 ? c transformation, grain martensite junctions appears to agree reasonably well

regardless of the nature of the diﬀusing species, strongly with the experimental data (Fig. 6b).

depends on the geometry of available nucleation sites. In So far, in order to determine the phase concentration

particular, it is sluggish when austenite nucleates at 2-grain nc(t, T), we have assumed the austenite nucleation rate

martensite junctions and faster when it nucleates at 3- or 4- J(T) to be constant. However, if a time-dependent nucle-

grain martensite junctions (Fig. 6). This is expected because ation rate were assumed in our calculations, the incubation

the austenite phase fraction, given by Eq. (10), depends time in Eq. (6) would need to be determined. This can be

strongly on the activation energy for heterogeneous nucle- done by solving by the following expression [32]:

ation DG(T), which is large for 2-grain martensite junc-

tions relative to that for 3- or 4-grain martensite 8k B T ra0 =c a4a0 K j

s¼ 2 ð20Þ

junctions (Fig. 2). In summary, our calculations show that V a0 DG2v Di xi Lj

746 S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748

where Di and xi are the diﬀusivity and the mole fraction of Appendix A

the diﬀusing species, and all the terms retain their previous

deﬁnitions. The incubation times for the rate-limiting cases The free energy of pure elements that are used in this

of nitrogen and chromium diﬀusion as a function of work have been obtained from the work of Dinsdale [41]

annealing temperatures (700–1000°C) were calculated and Miettinen [42], and are shown below. Gibbs free ener-

(Fig. 7a). The incubation time with nitrogen-diﬀusion as gies of pure elements in the bcc phase:

the rate-limiting factor is approximately 5–6 ls, while it is

Gbcc o

C ðT Þ GC ¼ 107; 350 þ 35:76T

much higher (several hundred milliseconds) with chromium

diﬀusion as the rate-limiting factor. This should not be sur- 1 o

Gbcc

N ðT Þ GN 2 ¼ 31; 187 þ 59:8T

prising because of the inverse dependence of the incubation 2

time on the diﬀusivities (Eq. (20)). bcc

Gnickel ðT Þ ¼ 3535 þ 114T 22 lnðT Þ

Based on the incubation times for the above-mentioned

annealing conditions, the nucleation rates for austenite Gbcc

chromium ðT Þ ¼ 8856 þ 157T 27 lnðT Þ

manganese ðT Þ ¼ 8115 þ 130T 23 lnðT Þ

junctions were determined. For each annealing tempera-

ture and diﬀusing species scenario, the nucleation rate Gbcc

iron ðT Þ ¼ 1226 þ 124T 23 lnðT Þ

was normalized with respect to the maximum possible Gbcc

copper ðT Þ ¼ 3753 þ 129T 24 lnðT Þ

value for that case. The results are shown in Fig. 7b and

c. Clearly, the normalized nucleation rate is constant for Gbcc

molybdenum ðT Þ ¼ 7746 þ 132T 24 lnðT Þ

all annealing temperatures and times when nitrogen- Gbcc

silicon ðT Þ ¼ 38; 857 þ 114T 23 lnðT Þ

diﬀusion is the rate-limiting factor (Fig. 7b). Thus, our

assumption of constant nucleation rate for the case of Gibbs free energies of pure elements in the fcc phase:

nitrogen-diﬀusion is valid. Gfcc GoC ¼ 155; 006 þ 13:7T

C ðT Þ

For the case of chromium diﬀusion, calculations indi-

cate that the normalized nucleation rate is not constant 1 o

Gfcc

N ðT Þ GN 2 ¼ 23; 066 þ 274T 20:15T lnðT Þ

for the time of interest (1–100 s) at 700 °C annealing tem- 2

perature (Fig. 7c). At 1 s of annealing duration, the nor- Gfcc

nickel ðT Þ ¼ 5179 þ 117T 22 lnðT Þ

malized nucleation rate is approximately 80% of its

Gfcc

chromium ðT Þ ¼ 1573 þ 157T 27 lnðT Þ

maximum value. In the context of the analysis presented,

this means that we overestimated the austenite phase con- Gfcc

manganese ðT Þ ¼ 3429 þ 132T 25 lnðT Þ

centration at 700 °C. In other words, if a time-varying

Gfcc

iron ðT Þ ¼ 237 þ 132T 24 lnðT Þ

nucleation rate were employed to estimate austenite phase

concentration at 700 °C, the predicted nucleation kinetics Gfcc

copper ðT Þ ¼ 7770 þ 131T 24 lnðT Þ

would be even more sluggish than the one shown in

Fig. 6d. Therefore, for the case of chromium diﬀusion as Gfcc

molybdenum ðT Þ ¼ 7454 þ 133T 24 lnðT Þ

silicon ðT Þ ¼ 42; 837 þ 115T 23 lnðT Þ

ation rate is justiﬁed. This result also conﬁrms that the

a0 ? c transformation is driven by the fast diﬀusion of The interaction parameters the interaction parameters

interstitial nitrogen atoms. describing the interaction between the ith and the jth ele-

ments in the bcc and fcc phases have been obtained from

4. Conclusions Miettinen [42], and are shown below. First-order interac-

tion parameters in the bcc phase:

We have applied a generalized phase transformation

Lbcc

FeCr ¼ 20; 500 9:68T

kinetics model to understand the a0 ? c transformation

in cold-rolled and annealed metastable austenitic stainless Lbcc

FeMn ¼ 2759 þ 1:237T

steel, in order to achieve ultraﬁne-grained austenite. The Lbcc

FeMo ¼ 36; 818 9:141T þ ð362 5:724T ÞðxFe xMo Þ

classical nucleation theory [30,31,33,43] explains reason-

ably well the diﬀusion-driven a0 ? c transformation in Lbcc

FeNi ¼ 957 1:287T þ ð1789 1:929T ÞðxFe xNi Þ

heavily cold-rolled and annealed metastable austenitic SS. Lbcc

FeSi ¼ 153; 141 þ 46:48T þ ð92; 352ÞðxFe xSi Þ

In particular, we found that nitrogen-diﬀusion is responsi-

ble for the rapid a0 ? c transformation, while the process þ ð62; 240ÞðxFe xSi Þ2

of heavy cold-rolling provides heterogeneous nucleation Lbcc

FeCu ¼ 41; 003 6:022T

sites for the formation of austenite. In this regard, the

geometry of the austenite/martensite grain junctions is a Lbcc

CrMn ¼ 20; 328 þ 18:734T þ ð9162 þ 4:418T ÞðxCr

signiﬁcant parameter for promoting fast kinetics. The xMn Þ

results indicate that the a0 ? c transformation appears to

occur at austenite/martensite 3-grain junctions. Lbcc

CrMo ¼ 28; 890 7:962T þ ð5974 2:428T ÞðxCr xMo Þ

S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748 747

Lbcc

CrNi ¼ 17; 170 11:82T þ ð34; 418 11:858T ÞðxCr xNi Þ Lfcc

FeN ¼ 92; 779 56:509T þ ð28; 554 þ 24:734T ÞðxFe xN Þ

2

þ ð3805 5:203T ÞðxFe xN Þ

Lbcc

CrSi ¼ 102; 085 þ 9:543T þ ð49; 125 þ 14:11T ÞðxCr xSi Þ

Lbcc

CrCu ¼ 77; 107 Appendix B

Lbcc

NiMn ¼ 51; 785 þ 3:5T þ ð6600ÞðxNi xMn Þ

The geometric parameters a, b and c for diﬀerent types of

Lbcc

NiMo ¼ 46; 422 martensite grain junctions as a function of the dihedral angle

Lbcc

NiSi ¼ 100; 000

between the surface bounding the austenite nucleus [33].

ra0 =a0

Lbcc

NiCu ¼ 8366 þ 2:802T k ¼ cosðhÞ ¼

2ra0 =c

Lbcc

MnMo ¼ 7500

2-grain junction:

Lbcc

MnSi ¼ 89; 621 þ 2:941T þ ð7500ÞðxMn xSi Þ

a ¼ pð1 k 2 Þ

Lbcc

MoSi ¼ 70; 900

b ¼ 4pð1 kÞ

Lbcc

FeC ¼ 119:04T þ ð43:89T ÞðxFe xC Þ þ ð7:89T ÞðxFe xC Þ2 2p

c¼ ð2 3k þ k 3 Þ

Lbcc 2 3

FeN ¼ 19:12T þ ð6:22T ÞðxFe xN Þ þ ð1:02ÞðxFe xN Þ

3-grain junction:

pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

First-order interaction parameters in the fcc phase:

a ¼ 3dð1 k 2 Þ k 3 4k 2

p

Lfcc

FeCr ¼ 10; 833 7:477T þ ð1410ÞðxFe xCr Þ

b ¼ 12 v kd

12

Lfcc qﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

c ¼ 2 p 2v þ ð3 4k Þ dkð3 k Þ

Lfcc

FeMo ¼ 28; 347 17:691T

3

Lfcc

FeNi ¼ 12; 054 3:274T þ ð11; 082 4:45T ÞðxFe xNi Þ

where

2

þ ð726ÞðxFe xNi Þ 1

v ¼ sin1 pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

2 1 k2

Lfcc 0 1

FeSi ¼ 12; 5248 þ 41:116T þ ð142; 708ÞðxFe xSi Þ

2 B k C

þ ð89; 907ÞðxFe xSi Þ d ¼ cos1 @qﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃA

2

Lfcc 3ð1 k Þ

FeCu ¼ 53; 360 12:626T þ ð11; 512 þ 7:095T ÞðxFe xCu Þ

4-grain junction:

Lfcc

CrMn ¼ 19; 088 þ 17:542T 8 20sﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ1 39

< 2 2 =

Lfcc

CrMo ¼ 28; 890 7:962T þ ð5974 2:428T ÞðxCr xMo Þ

K K

a ¼ 3 2/ð1 k 2 Þ K 4@ 1 k 2 A pﬃﬃﬃ5

Lfcc : 4 8 ;

CrNi ¼ 8090 12:88T þ ð33; 080 16:036T ÞðxCr xNi Þ

p

Lfcc

CrSi ¼ 102; 085 þ 9:543T þ ð49; 125 þ 14:11T ÞðxCr xSi Þ b ¼ 24 k/ u

3

8 20sﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ1 3

Lfcc

CrCu ¼ 53; 196 3:312T < p 2 2

K K

Lbcc c ¼ 2 4 u þ kK 4@ 1 k 2 A pﬃﬃﬃ5

NiMn ¼ 51; 785 þ 3:5T þ ð6600ÞðxNi xMn Þ : 3 4 8

Lfcc

NiMo ¼ 4804 5:96T þ ð10; 800ÞðxNi xMo Þ )

Lfcc

NiSi ¼ 161; 150 þ 43:799T þ ð118; 251 þ 43:33T ÞðxNi xSi Þ

2k/ð3 k 2 Þ

Lfcc

NiCu ¼ 8366 þ 2:802T þ ð4360 1:812T ÞðxFe xCu Þ where

Lfcc ¼ 22; 300 sﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

MnMo

4 3 2

Lfcc K¼ 2k 2 k

MnSi ¼ 95; 600 þ 2:941T þ ð7500ÞðxMn xSi Þ 3 2 3

Lfcc

MoSi ¼ 70; 900 K

/ ¼ sin1 pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ2ﬃ

Lfcc

FeC ¼ 162; 316 43:512T þ ð60; 803 þ 17:24T ÞðxFe xC Þ 2 1k

pﬃﬃﬃ pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

þ ð10; 957 3:306T ÞðxFe xC Þ2 1 2 k 3 K2

u ¼ cos pﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃﬃ

K 1 k2

748 S. Rajasekhara, P.J. Ferreira / Acta Materialia 59 (2011) 738–748

phenomena. 2nd ed. Oxford: Elsevier; 2004. p. 333–9.

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