Grain Refinement of a Cold Rolled TRIP Assisted Steel after Ultra Short

Annealing

PETROV Roumen1,3, a, SIDOR Jurij1b, KALUBA Wlodzimierz2c

and KESTENS Leo1,3d
1
Gent University, Dept. of Materials Science and Engineering, Technologiepark 903, Gent,
Belgium
2
Laboratoire de Thermophysique de la Matiére Condensée, Université de Littoral Côte d'Opale,
France
3
Technical University of Delft, Departmentv of Materials Scienice and Engineering, Mekelweg 2
2628CD Delft, the Netherlands

a
roumen.petrov@ugent.be, b jurij.sidor@ugent.be, c kaluba@univ-littoral.fr, dleo.kestens@ugent.be

Keywords: Grain refinement, Recrystallization, Phase transformation, Texture, Ultra fast

reheating.

Abstract. Recrystallization and austenite formation in a TRIP-assisted steel during conventional

and ultra fast reheating for intercritical annealing are studied with the purpose to clarify the
possibility for the grain refinement. Partially recrystallized (or transformed) samples were prepared
by reheating and water quenching to temperatures between 650 and 1050°C at reheating rates of 10,
50, and 3000 °C/s, respectively, without isothermal soaking from 95% cold rolled steel sheet with
ferrite-pearlite microstructure. By monitoring the hardness and microstructure was shown that the
increase of the reheating rates from 10, to 3000°C/s causes grain refinement from 5µm to 1µm in
diameter and the final ferrite grain size depends significantly on both reheating temperature and
reheating rate. It was observed that after extreme reheating rate of 3000°C/s the α-γ phase
transformation starts before the completion of the recrystallization. This opens up possibilities for
further structural refinement and alternative texture control.

Introduction
Cold rolled TRIP-assisted steels (TRIP-TRansformation Induced Plasticity) obtain their functional
properties by a two-stage heat treatment, which consist of an intercritical annealing stage followed
by interrupted isothermal quenching at temperatures in the bainitic region. This treatment creates a
microstructure of ferrite, bainite and mechanical unstable retained austenite which determines their
properties by creating a composite like material in which the ferrite matrix contributes to ductility,
whereas the distribution of bainite and the transformational stability of the retained austenite offer
both strength and ductility. The grain size of the both BCC and FCC phases plays a key role in the
formation of the final properties of the steel sheet and could be controlled effectively via the
parameters of the intercritical annealing cycle [1] or initial microstructure [2]. In industrial
conditions reheating rates are usually limited up to 10-50°C/s which allows first recrystallization of
the cold rolled material to be completed and only after that the BCC-FCC phase transformation
takes place i.e. in industrial conditions the intercritical austenite originates from completely
recrystallized ferrite [1,2].
The reheating rate can influence significantly the recrystallization and the texture formation in cold
rolled steel sheets [3]. However, the number of studies concerning the recrystallization and
transformation behaviour in the conditions of fast reheating of cold rolled steel sheets with heating
rates higher than 100°C/s is limited [3-6] and they consider the recrystallization of iron [6] or extra
low carbon steels [3] after reheating with a reheating rate of 1000 °C/s [3] or 5000 °C/s [6], whereas
other threat the α-γ transformation [5] with a reheating rate up to 2000 °C/s in a high carbon steel or
in a dual phase steel but under the condition of a comparably low heating rate of 200°C/s [4]. In a
previous works [7, 8] a strong grain refining effect in a Si-Mn steel after reheating at 3000 °C/s to
the intercritical region was reported for the initial microstructure of ferrite and tempered martensite.
The present study aims to answer the question if the ultrafast reheating can contribute to grain
refinement in cold rolled TRIP steel grades with hot band ferrite –pearlite microstructure and what
are the mechanisms which control this effect.

Experimental
Steel with a hot band ferrite –pearlite microstructure and a chemical composition (in mass%) of
0.11%C, 1.26%Si, 1.53% Mn 0.013%P and 0.029%Al was cold rolled to a reduction of 95%. The
value of the critical temperatures Ac1 =736°C and Ac3=903°C was determined by dilatometry test on
the hot rolled specimens with a heating rate of 10°C/s. By applying local EDX mapping of the
chemical elements no trace of segregation of substitutional elements was found.
Samples of size 80x30x1 mm were cut parallel to the rolling direction of the cold rolled sheet.
They were reheated with heating rates of 10°C/s, 50°C/s and 3000°C/s and subsequently water
quenched from different temperatures in the temperature interval 500 to 1000 °C without isothermal
soaking. The reheating of the samples with 10 and 50 °C/s was implemented in an infrared furnace
whilst the temperature was measured and controlled by a K1 type thermocouple welded to the
surface of the sample. The reheating with average reheating rate of 3000 °C/s was carried out by
passing a high intensity electrical current through the strip specimen. The temperature measurement
and control were done using an infrared pyrometer (IMPAC IW5) with an operating range between
400 and 1200°C and a response time of 1ms. With such equipment it is possible to produce the
thermal cycles at heating rates between 200 and 7000 °/s with satisfactory temperature control and
the possibility of the immediate water quenching. The detailed parameters of the annealing treatment
are shown in table 1, whereas a schematic representation of the time- temperature cycle and a record
of the real “reheating –quenching” cycle are shown in Fig. 1.

Table1. Reheating temperatures used in this work

Reheating rate, °C/s Reheating temperature,

°C
10 625 650 674 700 725 750 775 800
50 700 750 800 850
3000 650 760 790 860 880 930

Specimens from the thermally controlled zone (by means of thermocouple or infrared pyrometer)
were cut and investigated in transverse plane by means of optical microscopy (OM), scanning
electron microscopy (SEM), electron backscatter diffraction (EBSD) and hardness measurements
(HV02) after an appropriate sample preparation. The appearance of the martensite phase in the final
microstructure (after quenching) is used as a tracer of the α-γ phase transformation. The latter was
observed directly in the high resolution SEM. Averaged grain size was evaluated on the base of the
EBSD measurement considering as a grain each region with misorientation of more than 5° and
containing more than 4 pixels. The high resolution EBSD data, collected with a step size of 40nm
and 25nm were used also for local texture measurement of the martensite phase and the surrounding
matrix.

Results and discussion

 900
T, °C
800
Ac3=903°C 700

Temperature, °C
TIA~800°C 600
Tqi 500
Ac1=736°C
400 10 °C/s
300 50 °C/s
200
3000 °C/s
100
0
a Time, s b 0.01 0.1 1 10
Time, s
Fig.1: (a) Schematic representation of reheating –quenching cycle with variable reheating rates; (b)
record of real cycle for samples reheated to 800°C with 10 and 50°C, and sample reheated to 865°
with 3000°C/s.

500 The hardness evolution (HV02) of the

samples reheated with 10°C/s and
450
I II III IV 3000°C/s is shown in Fig. 2. The hardness
changes in samples reheated with 50°C/s
are identical to the one of the samples
400
reheated with 10°C/s. The data in Fig. 2
Hardness, HV02

are averaged among 5 measurements per

350
sample for the samples reheated with
3000°C/s and 10 measurements per
300
10°C/s
samples for samples reheated with 10°C/s.
Initial slight increase in the hardness of
250
3000°C/s the samples reheated with 10°C/s after
annealing at ~550°C can be associated to
200 the strain aging effects (stage I, Fig.2).
0 200 400 600 800 1000 After 600°C (stage II) due to recovery and
Temperature, °C
Fig.2: Vickers hardness (HV05) as a function of the recrystallization the hardness of the
reheating temperature obtained with a rate of 10°C/s samples reheated with 10°C/s decreases
and 3000°C/s. Stage I –strain aging, stage II- gradually from 351HV02 to 220HV02 at
recovery and recrystallization and stage III – phase 750°C. The next increase in the hardness
transformation. (stage III) is a result of α-γ transformation
which after quenching results in
appearance of martensite in the microstructure when the reheating temperatures are above the Ac1.
With increase of the reheating rate up to 3000°C/s the softening stage (stage II) which is associated
to the recovery and recrystallization disappears from the hardness-temperature curve.
This is an indication that at 3000°C/s the recrystallization is strongly suppressed and there is no
softening stage in the hardness –temperature curve. The hardness of the fast reheated samples
increases after quenching at temperatures above 800°C and the hardness increase could be
associated with the progress of α-γ-α’ phase transformation in unrecrystallized ferrite matrix. This
assumption is directly confirmed by the metallographic observation (cf.Fig.3c, d) and the high
resolution EBSD data (cf. Fig. 4). The arrows in the figures display the ferrite (F) and martensite
(M) phases. The hardness increase in the ultrafast reheated samples is larger than in the samples
reheated with 10 and 50°C/s in the temperature interval 790°C-900°C, due to two simultaneously
acting effect which both contribute to the hardness: (i) progressing martensite transformation and (ii)
strong grain refinement.

Fig.3 (left):Microstructure after reheating with: (a) 10°C/s at 800°C; (b) 50°C/s at 805°C; (c)
3000°C/s at 790°C and (d) detail from (c) displaying martensite as an evidence for the
transformation. Fig.4 (right): Combined IQ and ND IPF maps of samples after reheating with
3000°C/s to: (a)760°C; (b)790°C; (c) 860°C and (d) 880°C

0.2
6
3000°C/s@760°C
0.18
Average grain diameter, µm

3000°C/s@860°C
0.16 5
3000°C/s@880°C
0.14
Area fraction

3000°C/s@790°C 4
0.12
10°C/s@790°C
0.1 3
850°C@50°C/s
0.08
0.06 2

0.04
1
0.02
0 0
0.01 0.1 1 10 1 10 100 1000 10000
Average grain diameter, µm Reheating rate, °C/s

Fig.5 (left): Variation in the grain size distribution (area fraction) for different reheating rates and
temperatures. Fig.6 (right): Variation in average grain diameter as a function of reheating rate for
T=850±10°C without isothermal holding
The hardness increase in the ultrafast reheated samples is shifted to elevated temperatures due to
the increase of AC1 as a consequence of high reheating rate. At reheating temperatures 790°C and
860°C the martensite forms form austenite with higher carbon content. It is harder but still
structurally heterogeneous in comparison to the one formed at 880°C and higher temperatures
because the carbide dissolution in the austenite is not complete (cf. Fig.3,d). At temperatures 880°C
and higher the α-γ transformation proceeds very fast and almost completely and the microstructure is
fully martensitic but still with very small grains with average diameter of 1.3µm (cf. Fig. 4, d and
Fig.7). The grain size is strongly dependent on the reheating rate as it is demonstrated in Fig. 6, and
Fig.7.
The size of the martensite zones is close to the size of the cells in the recovered ferrite matrix which
indicates that the austenite phase nucleates in the subgrain boundaries of the recovered matrix. It
 grows by carbon diffusion trough the subgrain cells and might inherit the crystallographic

Fig.7: Microstructure of sample reheated to 930°C

at a rate of 3000°C/s displaying martensite and
Fig.8: ODFs of the steel in: (a) as cold rolled
remaining cellular structure of the recovered but
condition; (b) after reheating to 800°C at a rate of
not recrystallized ferrite. The dimensions of the
10°C/s; (c) to 800°C at a rate of 50°C/s; and to
largest grains are shown.
760°C(d), 860 (e) and 880°C at a rate of 3000°C/s.
orientation of the deformed ferrite.
However, all the above reported results are
obtained in conditions of ultrafast reheating but
practically without isothermal soaking and there
are no experimental data about the grain size
evolution in the isothermal soaking conditions
M which are applied usually in industry.
Additional approval for overlapping of the α-γ-α’
phase transformation with the recrystallization is
found in the evolution of the crystallographic
textures. Fig. 8 displays the changes in the
crystallographic texture as a function of the
reheating rate and the reheating temperatures for
a reheating rate of 3000°C/s. All texture data are
collected by EBSD except the texture of the cold
rolled sample Fig. 8a which is measured by X-ray
diffraction. The RD-ND fibre and the rotated cube
texture component appear in the as cold rolled
sheet (Fig. 8a). After slow reheating (10 and
50°C/s) the cold rolling texture changes to
recrystallization type texture which is
characterised by strong {111}〈uvw〉 (ND fibre)
with specific curvature, and in which the RD fibre
component {hkl}〈110〉 is almost vanished or quite
b c weak. In contrary the texture of the cold rolled
Fig.9: (a) Image quality map of sample samples reheated with 3000°C/s remains almost
reheated to 790°C at a rate of 3000°C/s; unchanged even after reheating up to 880°C (cf.
(b)martensite texture; (c) texture of
unrecrystallized ferrite matrix.
Fig 8d, e, f) keeping the characteristic features of the BCC cold rolling texture. Therefore, it is quite
likely that at the temperatures to 880 °C the ferritic matrix is still not recrystallized. Separation of
the EBSD signal from martensite and ferrite allow calculating separately the martensite and ferrite
textures. As it was shown in the Fig. 9 a, b, the martensite texture is the same as the ferrite one
which is an indication for the texture memory effect i.e. the martensite phase inherits the texture of
the deformed ferrite.

Conclusions

The results of the study of the transformation behaviour of a 95% cold rolled TRIP assisted steel
during its reheating for intercritical annealing with reheating rates of 10, 50, and 3000°C/s, without
isothermal soaking could be summarized as follow:
1. The recrystallization is completely suppressed in the samples reheated with 3000°C/s in
comparison to the samples reheated with 10 and 50°C/s up to reheating temperatures of 880°C.
2. After ultra-fast reheating at 3000 °C/s the austenite formation starts in a not recrystallized
matrix The austenite phase nucleates in the subgrain boundaries of the recovered matrix. It
grows by carbon diffusion trough the subgrain cells and might inherit the crystallographic
orientation of the deformed ferrite.
3. Grain size of ~1 µm is obtain in ultrafast reheated samples in the temperature interval 790-
880°C but the question for grain growth in isothermal conditions after ultrafast reheating still
remain to be investigated.

Acknowledgements
This research was supported by the FWO-Odysseus Program within a project: “Engineering of 3D
microstructures in metals: bridging ten length scales of functionality”.

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