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