Professional Documents
Culture Documents
1093–1102
Department of Physical Metallurgy, Centro Nacional de Investigaciones Metalúrgicas (CENIM), CSIC, Avda. Gregorio del Amo,
8, 28040 Madrid, Spain. E-mail: cyda@cenim.csic.es
(Received on March 8, 2001; accepted in final form on June 6, 2001)
The main aim of this work is to study the mechanisms that control the austenitisation process in steels
with different initial microstructures. The compiled knowledge in literature regarding the isothermal forma-
tion of austenite from different initial microstructures (pure and mixed microstructures), has been used in
this work to develop a model for non-isothermal austenite formation in steels with initial microstructure con-
sisting of ferrite and/or pearlite. The microstructural parameters that affect the nucleation and growth kinet-
ics of austenite, and the influence of the heating rate have been considered in the modelling. Moreover,
since dilatometric analysis is a technique very often employed to study phase transformations in steels, a
second model to describe the dilatometric behaviour of the steel and calculate the relative change in length
which occurs during the austenite formation has been developed. Both kinetics and dilatometric models
have been validated. Experimental kinetic transformation, critical temperatures as well as the magnitude of
the overall contraction due to austenite formation are in good agreement with calculations.
KEY WORDS: modelling; continuous heating transformations; kinetics.
with pure and mixed initial microstructures. observation fields with an approximately equal weight.28)
The following heat treatments were carried out to yield
2. Materials and Experimental Procedure in PEARL steel (Table 1) fully pearlitic microstructures
with different scale parameters. Specimens were austeni-
2.1. Metallographic Characterisation of Initial Micro- tised for 5 min at 1 273 K, isothermally transformed at one
structures of two different temperatures and subsequently cooled
Table 1 lists the chemical composition of the studied rapidly to room temperature. Table 3 lists the temperatures
steels. FERR1–4 steels in Table 1 have a full ferrite initial and holding times used for the isothermal formation of
microstructure (Fig. 1). Specimens of those steels were pearlite with different morphological parameters in this
ground and polished using standardised techniques for met- steel. PEARL1 specimen was ground and polished using
allographic examination. Nital-2pct etching solution was standardised techniques and finished on 0.25 m m diamond
used to reveal the ferrite microstructure by optical mi- paste for metallographic examination. An etching solution
croscopy. The ferrite grain size was measured on micro- of picric acid in isopropyl alcohol with several drops of
graphs. The average ferrite grain diameter (D) (Table 2) Vilella’s reagent was used to reveal pearlite in this specimen
was estimated by counting the number of grains intercepted on a JEOL JXA-820 scanning electron microscope (SEM)
by one or more straight lines long enough to yield, at least (Fig. 2(a)). Pearlite in PEARL2 specimen was characterised
fifty intercepts in total. The effect of a moderately non- by transmission electron microscopy (TEM). For this, 3 mm
equiaxial structure was eliminated by counting the intersec- diameter cylindrical samples were sliced into 100 m m thick
tions of lines in four or more orientations covering all the
(a)
(a)
(b) (b)
Fig. 2. Electron micrographs of the two dif- Fig. 3. Initial microstructure of MIXT steel: (a)
ferent morphologies of pearlite in optical micrograph; (b) scanning electron
PEARL steel (Table 3): (a) PEARL1 micrograph.
(SEM); (b) PEARL2 (TEM).
S vPP5
(
6 112 3 ) (a ) 5 3(112 3 ) ............(1)
P
2
( )
3
8 2 aP 4 2 aP
Data for s o, SvPP and aP for PEARL and MIXT steels are
listed in Table 4.
2.2. Dilatometric and Metallographic Analysis of
Austenite Formation Fig. 4. Temperatures selected from heating dilatometric curves
to investigate the progress of pearlite-to-austenite trans-
The experimental validation of the austenite formation formation in a eutectoid steel.
kinetics and dilatometric models developed in this work
was carried out using an Adamel Lhomargy DT1000 high-
Table 5. Temperatures in K of heating interruption by quench-
ing in PEARL steel.
Table 4. Morphological characterisation of pearlite in PEARL
and MIXT steels.
δv DGact α →γ the edge length, and the grain corner number, all per unit
G5 exp2 Dg
kT kT volume. Assuming ferrite grains to be tetrakaidecahedra,23)
S/V, L/V and C/V can be expressed in terms of the average
δv DS D H α →γ ferrite grain diameter D by: S/V53.35/D; L/V58.5/D2; and
5 exp exp2 Dg {T } ...........(2)
kT k kT C/V512/D3.
The difficulties in treating non-isothermal reactions are
where d is the boundary thickness, v is the number of at- mainly due to the complex variations of growth rate with
tempts to jump the boundary activation barrier per unit temperature, described in Eq. (2). We can only deal with
time, k is the Boltzman constant, T is the absolute tempera- the problem when the rate of transformation depends exclu-
ture, DGact is the free energy for the activated transfer sively on the state of the assembly and not on the thermal
atoms across the ferrite/austenite interface, DS is the en- path by which the state is reached.25) Reactions of this type
tropy of activation per atom, DH is the enthalpy of activa- are called isokinetic. Avrami defined an isokinetic reaction
tion per atom, and Dga →g is the Gibbs free energy differ- by the condition that the nucleation and growth rates are
ence per atom between the a and g phases. The values proportional to each other (i.e. they have the same tempera-
of DH and v are uncertain but are generally assumed to ture variation). This leads to the concept of additivity and
be equal to the enthalpy of activation for grain boundary Scheil’s rule.38) Since Avrami’s condition for an isokinetic
diffusion33) and to kT/h (being h Planck constant), respec- reaction is not satisfied in the present case, a general equa-
tively. The value of DS is also uncertain and may be tion to describe the non-isothermal overall ferrite-to-austen-
negative or positive. If we consider that the maximum ite transformation in ferritic steels was derived integrating
ferrite/austenite interface velocity for a 200 m m ferrite the Eq. (3) over the whole temperature range where the
grain diameter is 0.016 m/s at 1 223 K,22) Dga →g 541.873 transformation takes place.17) In this sense, we have taken
10224 J per atom, d 55 Å, and DH5276.33310221 J per logarithms in Eq. (3), which then was differentiated,
atom, then v exp(DS/k) is equal to 1.6531017 s21. Figure 5
shows the Gibbs free energy change for the ferrite-to- 1 dVγ
5 12V 5( K s12 K et13K c t )dt ......(5)
2
austenite transformation Dga →g for all the studied steels. d ln
12Vγ γ
This energy has been obtained according to the thermo-
dynamic calculations proposed by Aaronson et al.34,35) and If we consider a constant rate, Ṫ, for the heating condition,
Kaufman et al.36) In order to account for the effects of al- time can be expressed as follows:
loying elements into calculation, Zener factorisation of the
free energy into magnetic and non-magnetic components dT DT
dt5 t5 ...........................(6)
has been performed.37) T˙ T˙
Assuming that site saturation occurs and the reaction is
substituting into Eq. (5) and integrating in [0, Vg ] and
controlled by growth, the kinetics law obtained for the three
[Ts, T] intervals on the left and on the right sides, respec-
different activated growth sites can be expressed as
tively, it can be concluded that:
follows:23,24)
Vg 512exp[2(Kst1Ket21Kct3)] .................(3) (DT )2 dT
∫ ∫
Vγ T
dVγ DT
5 K s12 K e ˙ 13K c
where Vg represents the formed austenite volume fraction, t 0 12Vγ Ts T (T˙ )2 T˙
is the time and Ks, Ke and Kc are given by,
...........................................(7)
S L 4 C
K s52G , K e5πG 2 , K c πG 3 ........(4) where Ts is the start temperature of the transformation or
V V 3 V temperature at which Dga →g 50 (root of the function repre-
where the growth rate of austenite (G) is given by Eq. (2) sented in Fig. 5). Therefore, the volume fraction of austen-
and S/V, L/V and C/V respectively are the boundary area, ite (Vg ) present in the microstructure as a function of tem-
perature can be calculated as follows, curves. In this sense, the measured values of austenite vol-
ume fraction as a function of temperature can be best de-
6.7
∫
T
53.4 scribed with n56, m51, p51/2 and r51/3.
Vγ 512exp2 ˙ G1 ˙ 2 G ( T 2Ts )
2
Austenite nuclei in pearlite grow when carbon atoms are
Ts TD ( TD )
transported by diffusion to the ferrite/austenite boundary
150.8 3 from the austenite/cementite boundary through the austen-
1 G ( T 2Ts ) 2 dT .....................(8) ite and from the ferrite/cementite boundary through the fer-
˙ )
3
( TD rite, resulting in a transformation of the ferrite lattice to an
austenite lattice.5) As in the case of the reverse transforma-
3.2. Modelling of Kinetics of Non-isothermal Austenite tion (austenite-to-pearlite transformation), the growth rate
Formation in a Steel with a Pearlite Initial Micro- of austenite is believed to be controlled by either volume
structure diffusion of carbon or by boundary diffusion of substitu-
Nucleation and growth processes under isothermal con- tional alloying elements.37,40,41) If the growth rate of austen-
dition can be described in general using the Avrami’s equa- ite is controlled by the bulk diffusion of atoms in austenite
tion:39) ahead of the interface, the diffusion of carbon may play a
more important role than that of substitutional alloying ele-
π ments. Diffusivity of the substitutional alloying elements in
˙ 3t 4 ......................(9)
Vγ 512exp2 NG austenite is far smaller than that of carbon. As a result, the
3
substitutional alloying elements may not diffuse a long
where Vg represents the formed austenite volume fraction, distance during the reaction. However, as described by
Ṅ is the nucleation rate, G is the growth rate and t is the Porter,42) when temperature decreases, boundary diffusion
time. According to Christian,25) with a spherical configura- of substitutional alloying elements is the dominant mecha-
tion, an exponent of 4 in time (t) in Avrami’s equation nism in the diffusion process. In that case, the partitioning
means that the nucleation rate (Ṅ) and the growth rate (G) of the substitutional alloying elements is substantial during
are constant in time. the growth of austenite and boundary diffusion of the alloy-
Roosz et al.14) proposed a temperature and structure de- ing elements may control the growth rate of pearlite.
pendence of Ṅ and G as a function of the reciprocal value The function f G in Eq. (11) representing the structure de-
of overheating (DT5T2Ac1) as follows: pendence on the growth rate can be expressed as follows:
1
2QN f G 5K G ..............................(13)
Ṅ 5 f N exp ........................(10) σ oi
kDT
where KG is a empirical constant, i51 if the growth rate of
2QG austenite is controlled by volume diffusion of carbon and
G5 f G exp .........................(11) i52 if the growth rate of austenite is controlled by bound-
kDT
ary diffusion of substitutional alloying elements.14)
where QN and QG are the activation energies of nucleation As in ferrite-to-austenite transformation, a general equ-
and growth, respectively, k is Boltzmann’s constant, and f N ation to describe the non-isothermal overall pearlite-to-
and f G are the functions representing the influence of the austenite transformation in pearlitic steel was derived inte-
structure and the heating rate on the nucleation and growth grating the Avrami’s equation over the whole temperature
rates, respectively. range where the transformation takes place.17) In this sense,
Several authors3,14,22) reported that the nucleation of we have taken logarithms and differentiated in Eq. (9).
austenite inside pearlite takes place preferentially at the Expressing time as t5DT/Ṫ leads to:
points of intersection of cementite with the edges of the dVγ 4π ˙ 3 DT 3
pearlite colony. Approximating the pearlite colony as a 5 NG dT ...................(14)
truncated octahedron, the number of nucleation sites per 12Vγ 3 (T˙ )4
unit volume is calculated as NC<1/{(aP)2s o} where aP is Integrating in [0, Vg ] and [Ac1, T ] intervals on the left and
the edge length of the pearlite colony and s o is the inter- on the right sides of Eq. (14), respectively, it can be con-
lamellar spacing.31) cluded that:
Bearing in mind that the rate of nucleation increases as
the pearlite interlamellar spacing decreases and the edge 4π ˙ 3 3
∫
T
length of the pearlite colony increases,1) and considering Vγ 512exp2 NG DT dT ..........(15)
3(T˙ )2
that the heating rate (Ṫ ) might influence on the nucleation Ac1
rate, the function f N in Eq. (10) is assumed to have the fol-
It has been assumed that at a heating rate higher than
lowing general form:
0.5 K s21 the growth rate of austenite would be mainly con-
(a P )n ˙ p ˙ trolled by the volume diffusion of carbon in austenite, due
f N 5K N (T ) ( N C ) rT ...................(12) to the fact that the transformation would take place mostly
σo m
at higher temperatures. Consequently, an i value of 1 is con-
where KN, n, m, p and r are empirical parameters. These pa- sidered in Eq. (13) for that case. On the contrary, at heating
rameters were adjusted in order to obtain good fit between rates lower than or equal to 0.5 K s21 the growth rate of
theory and the experimental austenite volume fraction austenite has been assumed to be controlled by boundary
diffusion of substitutional alloying elements and an i value isothermal conditions, we have differentiated both equa-
of 2 is considered in Eq. (13) for that case. The eutectoid tions, expressed time as t5(T2TC)/Ṫ , where Ṫ is the heat-
temperature Ac1 of the steel was obtained using Andrews’ ing rate, and integrated in [0, Vga ] and [TC, T ] intervals on
formula.43) the left and on the right sides of Eq. (17), respectively, and
in [VDa , Vga ] and [TD, T ] intervals on the left and on the right
3.3. Modelling of Kinetics of Non-isothermal Austenite
sides of Eq. (18), respectively. TC is the previously cited
Formation in a Steel with a Ferrite Plus Pearlite
temperature and TD the temperature at which the kinetics
Initial Microstructure
of ferrite-to-austenite transformation changes under non-
In the austenitisation of microstructures composed of fer- isothermal conditions. It should be noticed that these criti-
rite and pearlite, two different transformations are involved: cal temperatures do not have to correspond with those from
pearlite dissolution and ferrite-to-austenite transformation. Datta et al. study since their work was carried out under
Both transformations take place by nucleation and growth isothermal conditions. Therefore, it can be concluded that:
processes.
Vγα
dVγα
∫ ∫
T
3.3.1. Modelling of Kinetics of Dissolution of Pearlite B
5 dT for TC,T,TD ........(19)
The nucleation and growth processes that control the dis- 0 (Vαo 2Vγα )2 TC T˙
solution of pearlite in a steel with a ferrite plus pearlite mi-
crostructure are the same than those described above for a Vγα
dVγα
∫ ∫
T
2 B9
steel with a full pearlite initial microstructure. Therefore, 5 dT for T$TD ...........(20)
the austenite volume fraction obtained from pearlite disso- VDα (Vαo 2Vγα )2 TD (T˙ )2
lution, VgP, during continuous heating of a ferrite plus
where VDa is the austenite volume fraction formed from fer-
pearlite initial microstructure is expressed as follows:
rite at TD temperature.
4π ˙ 3 3 Thus, the volume fraction of austenite formed from fer-
∫
T
VγP5VPo 12exp2 NG DT dT .....(16) rite during continuous heating at a given temperature is ex-
˙ 4
Ac1 3(T ) pressed as follows:
where VPo is the volume fraction of pearlite present in the 5.6T˙
initial microstructure. VPo50.11 in MIXT steel. Vγα 5Vαo 12
6310212Vαo (T 2TC )5.615.6T˙
3.3.2. Modelling of Kinetics of Ferrite-to-Austenite for TC,T,TD .............................(21)
Transformation after Dissolution of Pearlite
Datta et al.26) carried out a quantitative microstructural (Vαo 2VDα )(T˙ )2
analysis of the austenitisation kinetics of pearlite and ferrite Vγα 5Vαo 2
(T˙ )211.231023 (Vαo 2VDα )[(T 2TC )22(TD2TC )2 ]
aggregates at different intercritical annealing temperatures
in a low-carbon steel containing 0.15 mass% C. At all the for T$TD .................................(22)
tested temperatures, pearlite-to-austenite transformation TC and TD temperatures were determined experimentally for
was complete in less than one second and the kinetics of the MIXT steel by means of dilatometric analysis. Figure 6
ferrite-to-austenite transformation at higher temperatures shows the experimental dilatometric curve of the MIXT
(T$1 143 K) were found to be different from those tested at steel for a heating rate of 0.05 K s21. TC and TD tempera-
lower temperatures (T,1 143 K). In this sense, the time (t) tures are displayed on the dilatation curve in accordance
dependence of the volume fraction of austenite Vg at differ- with their definition above. Ac1 and Ac3 critical tempera-
ent temperatures was described by the following linear rela- tures represent the starting and finishing temperatures of
tionships: the austenitisation process. The possibility to be able to dis-
Vγ Vγα 1VPo criminate the pearlite dissolution process and the ferrite-
5 5A1Bt for T,1 143 K ...........(17) to-austenite transformation on the dilatometric curve per-
12Vγ Vαo 2Vγα
mitted the experimental determination of TC in this steel.
Vγ Vγα 1VPo
5 5A91B9t 2 for T$1 143 K .......(18)
12Vγ Vαo 2Vγα
where Vga is the austenite volume fraction formed from fer-
rite after complete pearlite-to-austenite transformation and,
VPo and Va o are the volume fractions of pearlite and ferrite,
respectively, present in the initial microstructure. The para-
meters A, A9 and B9 are insensitive to temperature (A<0.20,
A950.25 and B951.231023 s22),26) whereas B changes sig-
nificantly with temperature. The temperature dependence of
the kinetic parameter B has been calculated from Datta et
al.26) experimental results, being B56310212(T2TC)4.6
where TC is the starting temperature of ferrite-to-austenite
transformation and T2TC the overheating for this transfor- Fig. 6. Experimental dilatation curve, average of four identical
mation. dilatometric tests, of the MIXT steel for a heating rate of
With the aim of adapting Eqs. (17) and (18) to non- 0.05 K s21.
Fig. 8. Calculated dilatation curve of FERR1–4 compared with their corresponding experimental curves obtained at a heating rate of 0.05 K s21.
heating rate of 0.05 K s21 in FERR1–4 steels are shown in Fig. 10. Experimental and calculated kinetics results for the for-
Fig. 8 in comparison with their corresponding experimental mation of austenite inside pearlite under continuous
results. In Fig. 9 the experimental and calculated results of heating conditions in PEARL steel.
start (TS) and finish (TF) temperatures of ferrite-to-austenite
transformation are compared. TS is considered to be the
to the predicted temperatures. The addition of manganese
temperature at which the relative change in length of the
clearly leads to much larger deviations from calculated re-
steel deviates from a linear relation with temperature during
sults. That may be explained by the fact that the presence of
heating due to the formation of austenite; TF has been de-
a substitutional solute retards the transformation to austen-
fined as the temperature at which the sample exhibits again
ite because it is necessary for the solute to diffuse during
a linear thermal expansion relation once the ferrite-to-
transformation.19)
austenite transformation is completed. Points lying on the
In general, the calculated relative change in length was
line of unit slope show a perfect agreement between experi-
consistent with the measured value at every temperature.
mental and calculated values.
The fact that both the modelled and the experimental
The calculated curves shown in Fig. 8 suggest that the
dilatometric curves run parallel is irrelevant as long as the
ferrite-to-austenite transformation takes place almost in-
adequate thermal expansion coefficients are calculated ade-
stantaneously (1 K). In contrast, the experiments reveal that
quately.17) The linear expansion coefficients of ferrite and
this transformation needs between 10 and 20 K to reach
austenite from Takahashi47) are in a good agreement with
completion at a heating rate of 0.05 K s21. Additionally,
those measured values.
Fig. 9 shows that experimental TS and TF temperatures are
higher than those predicted for all the studied steels. Any 3.5.2. Experimental Validation of the Pearlite Dissolution
difference between these represents some kinetic hindrance Model in a Steel with a Pearlite Initial Micro-
to transformation. Figure 9 shows that the FERR1 steel structure
transforms to austenite at temperatures which are similar Figure 10 shows the experimental and calculated austen-
peratures of the pearlite-to-austenite transformation are 7) G. Krauss: Steels: Heat Treatment and Processing Principles, ASM
more sensitive to the heating rate than start temperatures. International, OH, (1989), 274
8) A. Gustavsson, D. L. Mcdowell, A. Melander, and M. Larsson: Inst.
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(4) In a steel with mixed initial microstructure consist- 11) G. R. Speich, V. A. Demarest and R. L. Miller: Metall. Trans. A, 12A
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12) M. M. Souza, J. R. C. Guimaraes and K. K. Chawla: Metall. Trans.
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(1974), 1437.
dilatometric curves. Results show that experimental start
25) J. W. Christian: The Theory of Transformations in Metals and
and finish temperatures of the transformation are higher Alloys, Pergamon Press, Oxford, (1965), 19.
than those predicted for all the studied steels. Furthermore, 26) D. P. Datta and A. M. Gokhale: Metall. Trans. A., 12A (1981), 443.
the addition of manganese clearly leads to much larger de- 27) E. Navara and R. Harrysson: Scripta Metall., 18 (1984), 605.
viations from calculated results since the presence of a sub- 28) G. F. Vander Voort: Metallography. Principles and Practice,
McGraw-Hill, New York, (1984), 427.
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32) F. S. Le Pera: J. Met., 32 (1980), 38.
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35) H. I. Aaronson, H. A. Domian and G. M. Pound: Trans. TMS-AIME,
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40) M. Hillert: Jernkontorets Ann., 141 (1957), 757.
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