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DOI 10.1007/s10973-014-4054-2
Received: 29 October 2013 / Accepted: 27 July 2014 / Published online: 4 September 2014
The Author(s) 2014. This article is published with open access at Springerlink.com
Abstract The work deals with dilatometric studies of a Keywords Dilatometric analysis AHSS steel Bainitic
new-developed advanced high-strength bainitic 3Mn–1.5Al transformation Multiphase microstructure Retained
steel. Ferritic, bainitic and martensitic phase transforma- austenite Carbide-free bainite
tions are investigated in detail in respect of their temper-
ature range forming and microstructures produced under
various conditions of both continuous and isothermal Introduction
cooling. The equilibrium temperatures of Ae1 and Ae3 and
phase composition of the investigated steel were initially The beneficial combination of high strength, ductility and
calculated whereas critical temperatures of Ac1 and Ac3 as technological formability of steel sheets for the automotive
well as the decomposition of retained austenite were industry can be achieved using advanced high-strength steels
determined upon heating. The major tests consisted of (AHSS). They consist of different soft and hard structural
controlled cooling of undeformed or plastically deformed constituents in various proportions, which enable to obtain a
austenite using the dilatometer within the cooling rate very wide range of mechanical and technological properties.
range of 2–0.5 C s-1. The effects of the cooling rate and The microstructure of dual phase (DP) steel contains soft
deformation at temperatures of 900 and 1,050 C on the ferrite and hard martensite whereas the multiphase micro-
phase transformation behaviour and microstructure were structure of TRIP (Transformation Induced Plasticity) steel
explained. The final experiment was carried out using a consists of ferrite, bainite and retained austenite [1–6]. New
thermo-mechanical simulator under conditions of multi- demands of the automotive industry for relatively low-cost
step deformation and isothermal holding of the steel at steel sheets characterized by tensile strength above
400 C. Microstructural features were revealed using light 1,000 MPa require further searching of new chemical com-
microscopy and scanning electron microscopy techniques. position strategies. Advanced ultra-high-strength steels con-
tain a higher fraction of hard phases, i.e. acicular ferrite,
bainite or martensite [7–10] compared to AHSS containing
polygonal ferrite as a matrix. A key microstructural constit-
uent of advanced multiphase steels is retained austenite with
A. Grajcar (&) P. Skrzypczyk A. Kowalski S. Kołodziej the amount from 10 to 30 %. This phase ensures a required
Institute of Engineering Materials and Biomaterials, Silesian ductility level by its strain-induced martensitic transformation
University of Technology, 18a Konarskiego Street, during cold forming operations. Recently, a high amount of
44-100 Gliwice, Poland
retained austenite is obtained in different bainitic alloys con-
e-mail: adam.grajcar@polsl.pl
taining from 1.5 up to 8 mass% Mn, being a main austenite
W. Zalecki stabilizer [8–14]. These steels are dedicated to the automotive
Institute for Ferrous Metallurgy, 12–14 K. Miarki Street, industry for different crash-relevant elements, especially in
44-100 Gliwice, Poland
the side zone of a car (B-pillars, roof rails, side-impact beams,
A. Kilarski etc.). Their wide use requires improved forming technologies
General Motors, 1 Adama Opla Street, Gliwice, Poland and special welding procedures.
123
740 A. Grajcar et al.
Monitoring of phase transformations and the knowledge bottom-[ 122 mm, top-[ 145 mm, height-200 mm. The
of continuous cooling transformation (CCT) diagrams are ingot was subjected to forging at a temperature range from
of primary importance for proper design of bainite–aus- 1,200 to 900 C to a thickness of 22 mm. Then, tubular
tenite microstructures with an optimal morphology. samples, [4 9 [3 9 7 mm, and [3 9 7 mm cylindrical
Decomposition of retained austenite on heating or cooling specimens for dilatometric investigations were machined.
from the c region is often monitored by dilatometry, dif- Finally, the [10 9 12 mm specimens were prepared for
ferential thermal analysis (DTA) or differential scanning multi-step hot compression tests.
calorimetry (DSC) [11, 15–17]. Results of these investi- Dilatometric analyses were conducted with the use of
gations have often to be confirmed by detailed microscopic DIL805 dilatometer produced by Bähr Thermoanalyse
research because phase transformations in multiphase GmbH, equipped with LVDT type measuring head with
steels are very complex. In medium-Mn steels, the bainite theoretical resolution of ±0.057 lm. Investigation and
is particularly difficult for unequivocal identification analysis of dilatograms and determination of critical tem-
because it can contain carbides or may form carbide-free peratures were made according to recommendations of
bainite [8, 18–22]. Films of retained austenite instead of Standard Practice issued by ASTM International [24] using
carbides occur between laths of bainitic ferrite. The the technique of applying the tangent to the dilatation curve
destabilization of the austenite can happen during heating near the beginning and the end of phase transition. In case
and cooling through precipitation of carbides, martensitic of inseparable transformations (occurring one after
transformation, etc. Monitoring the volume fraction of all another), numerical differentiation of dilatation curves was
microstructural constituents and their morphology is a key used for the analysis. In case of examination of ferritic
to obtain optimal mechanical properties of multiphase transformation, the method based on linear transformation
steels. Beneficial mechanical properties and formability of of analysed section of dilatation curve was applied in order
steels with a bainitic–austenitic mixture are obtained for to determine the start and finish temperature of phase
fine, homogeneous bainite microstructures. Carbide pre- transition.
cipitates and a bimodal morphology of fine and coarse The non-deformed specimens were exposed to heat
bainite are detrimental for fracture toughness and ductility setting [24], i.e. heated up to the temperature of 650 C
of steel products [19, 20, 23]. with a rate of 10 C s-1 and successively held for 10 min,
The novelty of the present work includes the identifi- then cooled down with a rate of 30 C min-1 to ambient
cation of temperatures of phase transformations for a new- temperature (Fig. 1). This step is required by the standard
developed steel containing 3 % Mn, which was cooled to eliminate any internal stresses caused during manufac-
from the plastically deformed recrystallized and non-re- turing and sample’s preparing. The main study involved
crystallized austenite regions. conducting three types of experiment:
123
Dilatometric study of phase transformations 741
vol. %
temperature (Fig. 1); 50
Austenite
Mns
• heating cylindrical samples with a rate of 3 C s-1 up 40
Cementite
M2(C, N)
to the temperature of 1,100 C, their austenitizing for 30
300 s, cooling with a rate of 5 C s-1 to the temper- 20
ature of 900 C. The samples were isothermally held 10
within 20 s and compressed applying the logarithmic 0
strain of 0.5 with a stain rate of 1 s-1. Final cooling to 400 600 800 1000 1200 1400 1600
room temperature was carried out at a rate of 2, 1 and Temperature/°C
0.5 C s-1; and (b)100
• heating cylindrical samples with a rate of 3 C s-1 up
98
to the temperature of 1,100 C, their austenitizing for
96
300 s, cooling with a rate of 5 C s-1 to the temper-
94
ature of 1,050 C. The samples were isothermally held Austenite
92
vol. %
within 20 s and compressed applying the logarithmic
90
strain of 0.5 with a stain rate of 1 s-1. Final cooling to
88
room temperature was carried out at a rate of 2, 1 and
86
0.5 C s-1.
84
Various deformation of samples at the temperature of 82
900 and 1,050 C was to determine the effect of austenite 80
1100 1200 1300 1400
state (non-recrystallized and recrystallized) on temperatures
Temperature/°C
of phase transformations during cooling, as well as its
impact on steel microstructure. A final experiment was Fig. 2 Thermodynamic equilibrium diagrams determined using the
carried out using the ‘‘Hydrawedge’’ unit of Gleeble JMatPro software (a), a part of the diagram showing the austenite
3800 simulator to reflect a thermo-mechanical path applied fraction as a function of temperature (b)
for TRIP steel sheets. The test consisted of four-step com-
pression at temperatures of 1,150, 1,050, 950 and 850 C 40 kV and 30 mA, equipped with an X’Celerator detector.
followed by multi-step controlled cooling to room temper- Three alpha and four gamma peaks were quantified by
ature. After the final deformation, the specimens were scanning through a 2-theta range from 40 to 115 deg. To
rapidly cooled to 700 C and next slowly for 50 s within the minimize the effect of texture, the amount of retained
temperature range of 700–650 C. Then, the samples were austenite was quantified on the basis of the integrated
cooled at the rate of 40 C s-1 to 400 C and isothermally intensity of three pairs of diffraction lines using the
held for 300 s. Finally, the deformed specimens were cooled Averbach-Cohen approach.
with a rate of 0.5 C s-1 to room temperature.
Microstructure of steel in the initial state, after dilato-
metric analyses and after thermo-mechanical processing, Results and discussion
was examined with the use of light microscopy (LM) and
scanning electron microscopy (SEM). The specimens after Thermodynamic equilibrium diagrams
dilatometric investigations were etched in 5 % nital, while
after thermo-mechanical treatment they were etched in The first stage of the study was calculating the change of
10 % aqueous solution of sodium metabisulfite. Micro- volume fractions of individual phases as a function of
structure observations were carried out with the Leica MEF temperature. Calculations were performed with the use of
4A light microscope. Morphological details of micro- JMatPro programme under conditions of thermodynamic
structural constituents were revealed with the SUPRA 25 equilibrium [25]. The calculation results are shown in
scanning electron microscope at the accelerating voltage of Fig. 2. Determined solidus temperature is equal to
20 kV. 1,445 C, and liquidus temperature is equal to 1,507 C.
X-ray examination was carried out with filtered Co The equilibrium temperature of a phase transformation Ae1
radiation and an X-pert PRO diffractometer operating at into austenite is equal to 669 C. Area of austenitic phase is
123
742 A. Grajcar et al.
1100
1000
900
Fs
Temperature/°C
800
700
600 Ps Pf
500
Bs Bf
400
Ms
300
200
0.1 10 1000 100000
Time/s
123
Dilatometric study of phase transformations 743
Temperature/°C
643.8
0.967 641.0
ΔI/I0/%
Retained austenite 11.1 ± 1.2 17.5 ± 1.6
fraction/% 638.3
0.958 635.5
632.8
Table 1 indicate that the amount of c phase in the initial 0.949 630.0
state is equal to about 11 %. It is in good agreement with 627.3
microstructural results (Fig. 4). 0.940 624.5
30 102 173 245 316 388 459 530 602 673 745
Time/s
Determination of critical temperatures
Fig. 5 Dilatometric curve registered at 650 C during isothermal
Critical Ac1 and Ac3 temperatures were determined at a holding of steel
heating rate of 0.042 C s-1. The Ac3 temperature has not
been reached. The successive metallographic studies
revealed the presence of non-transformed ferrite, what is 0.059
consistent with the results of dilatometric analyses and
thermodynamic calculations. The Ac1 temperature of steel is
0.046
equal to 695 C. This confirms the dependence that under
real heating conditions, the Ac1 temperature is higher than
Ae1 equilibrium temperature. For accepted heating rate, the 0.033
ΔI/I0/%
123
which happens in a temperature range from 403 to 216 C.
In the similar temperature range also martensitic transfor-
mation took place in case of a specimen cooled after sta-
bilization (Fig. 6). Confidential limits for the Ms
temperature are ± 2 C within cooling rates between 550
and 0.5 C s-1.
Dilatograms registered at a lower cooling rate are very
similar. In case of the sample cooled at a rate of 1 C s-1,
Change in length/μm
Def. temp./C Trans. type Cooling rate/C s-1 –2680
2 1 0.5
0.00
510 °C
–3410 Conditions of plastic deformation and cooling essentially
–3415
–0.10
influence microstructure of steel. Figure 12 presents
microstructures of specimens cooled from 900 C without
–3420 –0.20
deformation (Fig. 12a, d, g), after deformation under con-
658 °C
–3425 ditions of austenite recrystallization at 1,050 C (Fig. 12b,
–3430
–0.30
123
746 A. Grajcar et al.
Fig. 12 Microstructures of undeformed samples (a, d, g) and samples deformed at 1,050 C (b, e, h) as well as at 900 C (c, f, i) followed by
their cooling within the rate range from 2 to 0.5 C s-1
of c phase. The high density of lattice defects in austenite upper bainite [18, 19]. Blocky grains larger than 1 lm were
has a positive effect on both increasing the rate of bainite partially transformed into martensite forming martensitic–
nucleation and growth as well as hampering of martensitic austenitic (M–A) islands. Nevertheless, a fraction of mar-
lamellas [7, 9, 19]. tensite is significantly lower than under conditions of
The result of thermo-mechanical processing and iso- continuous cooling, and developed steel is susceptible to
thermal holding of the specimens at 400 C are micro- form microstructure of carbide-free bainite with high
structures presented in Fig. 13. First of all, multi-step amount of retained austenite.
deformation leads to a distinct refinement of all structural The volume fraction of retained austenite determined by
components as compared to the initial state (Fig. 4) and XRD reaches 17.5 % (Table 1). It is higher when com-
single strain at the temperature of 900 or 1050 C pared to the samples in the initial state due to carbon
(Fig. 12). A fraction of polygonal ferrite (a) is negligibly partitioning from bainitic ferrite into residual austenite.
small, while the main structural constituent is bainite. The final grain refinement favours the stabilization of
However, there are fine, bright grains of cR retained aus- retained austenite too [19]. The thermal stabilization of the
tenite at the boundaries of bainite sheaves (Fig. 13a). In high volume fraction of retained austenite means that
addition to blocky grains with sizes of about 1 lm between increased concentration of Al advantageously prevents
laths of bainitic ferrite (aB), there are also continuous or precipitation of carbides during the isothermal bainitic
intermittent layers of c phase with diversified thickness. transformation step. The obtained results are in good
Such microstructure type is most often called a degenerate agreement with earlier literature data showing that Al is the
123
Dilatometric study of phase transformations 747
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