Materials Science & Engineering A 735 (2018) 475–486

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Materials Science & Engineering A

journal homepage: www.elsevier.com/locate/msea

Influence of the Al and Mn content on the structure-property relationship in T

density reduced TRIP-assisted sheet steels
⁎
S. Kaara, , D. Krizanb, J. Schwabec, H. Hofmannc, T. Hebesbergerb, C. Commendad, L. Sameka
a
University of Applied Sciences Upper Austria, Faculty for Engineering and Applied Sciences, A-4600 Wels, Austria
b
voestalpine Stahl GmbH, Research and Development, A-4020 Linz, Austria
c
ThyssenKrupp Steel Europe AG, Technology & Innovation, G-47166 Duisburg, Germany
d
voestalpine Stahl GmbH, Microstructure and Surface Analysis, A-4020 Linz, Austria

A R T I C LE I N FO A B S T R A C T

Keywords: In the present study four different density reduced TRIP steel concepts with varying Mn and Al contents were
Density reduction investigated with regard to their microstructure, mechanical properties and retained austenite (RA) stability. For
TRIP steel the hot rolled strips, scanning electron microscopy (SEM) revealed a microstructure consisting of ferrite and two
δ-ferrite types of carbides. Using both X-ray diffraction (XRD) and SEM with backscattered electron (BSE)-detection, the
RA stability
carbides were identified as cementite for the steel grades containing 2.8 and 3.3 wt% Al and κ-carbides for the
Mechanical property
compositions with 5.2 wt% Al. The microstructure of the laboratory continuously annealed cold rolled sheets
consisted of numerous inclusions of bainite and RA, embedded in a ferritic matrix. As an aftermath of the
increased Al content, resulting in an increased ferrite content, the bainitic transformation was significantly
reduced, which led to a destabilization of RA and in turn to the formation of martensite upon final cooling to
room temperature (RT). With increasing Al- and Mn-contents the tensile strength rose from 720 to 1050 MPa,
whereas the total elongation decreased from 39% to 17%. Both highest mechanical and chemical RA stability
were found for the steel grades containing 2.8 and 3.3 wt% Al, resulting in the superior combination of strength
and ductility, namely RmxA80 of almost 30,000 MPa% by a density reduction up to almost 5%.

1. Introduction
The challenging demands of the automotive industry concerning
crashworthiness, formability and reduction of CO2 emissions are
driving factors for the development of new steel grades [1,2]. In order
to meet these requirements “Advanced High Strength Steels” (AHSS)
are currently under development [3–5]. By making use of these new
steel grades the material’s strength can be enhanced without a dete-
rioration of ductility, allowing for the down-gauging, resulting in a
significant weight reduction [1,6–8].
The 1st generation AHSS includes the DP (Dual Phase), TRIP
(Transformation Induced Plasticity) and CP (Complex Phase) steels.
These steels mainly have a multiphase structure, which combines the
advantages of the individual microstructural constituents and thereby
tensile strengths up to 1200 MPa and total elongations up to 40% can be
achieved [9–11]. The microstructure of DP steels consists of a soft
ferritic matrix, including a second phase of lath-type cubic martensite.
Due to the large difference in hardness between the ferritic and mar-
tensitic phase, these steel grades tend to the micro-crack formation
during forming operations with localized deformation such as e.g.
bending, particularly with small bending radii [2]. On the contrary,
they are well suited for the applications using forming operations with
global deformation, i.e. for deep drawing [11]. TRIP steels typically
have a microstructure consisting of the soft ferritic matrix and hard
inclusions, representing bainitic ferrite and RA. In order to ensure a
sufficient strain-induced austenite to martensite transformation during
deformation (the TRIP effect), the stabilization of RA and therefore the
prevention of athermal martensite formation during final cooling is a
key factor to be kept in mind during production of this steel grade.
Both, mechanical and chemical stability have to be adjusted in order to
achieve a superior combination of strength and ductility [12–14]. In
particular, C dissolved in RA, as a pronounced austenite stabilizer, most
efficiently decreases the MS temperature and therefore large quantities
of RA can be stabilized at RT [15]. Furthermore, since smaller RA grains

⁎
Corresponding author.
E-mail addresses: simone.kaar@fh-wels.at (S. Kaar), daniel.krizan@voestalpine.com (D. Krizan), jonas.schwabe@thyssenkrupp.com (J. Schwabe),
harald.hofmann@thyssenkrupp.com (H. Hofmann), thomas.hebesberger@voestalpine.com (T. Hebesberger), christian.commenda@voestalpine.com (C. Commenda),
ludovic.samek@fh-wels.at (L. Samek).

https://doi.org/10.1016/j.msea.2018.08.066
Received 14 May 2018; Received in revised form 17 August 2018; Accepted 20 August 2018
Available online 22 August 2018
0921-5093/ © 2018 Elsevier B.V. All rights reserved.
S. Kaar et al.
have a lower number of potential nucleation sites for martensitic
transformation, a larger driving force for nucleation of martensite must
be taken into consideration. Thus, at smaller grain sizes the transfor-
mation of remaining austenite to athermal martensite can be effectively
suppressed, since an increase in the transformation driving force leads
to further decrease in the MS temperature [13,15]. In addition, the
stress state, the distribution of RA within microstructure, its volume
fraction, morphology and the stacking fault energy have an impact on
the RA stability, as well [14]. Due to the hardness differences of in-
dividual microstructural constituents, TRIP steels are less suitable for
the forming operations with localized deformation. In opposite, they
have an excellent performance during the forming operations with
global deformation [9]. Finally, CP steels possess a homogeneous mi-
crostructure consisting of ferrite, bainite, martensite and tempered
martensite, respectively. Due to the lower difference in hardness be-
tween the individual microstructural compounds, CP steels are char-
acterized by a higher resistance to stress concentrations in the micro-
structure, resulting in an excellent suitability for manufacturing
processes such as bending and roll forming [10].
The 2nd generation AHSS includes TWIP (Twinning Induced
Plasticity), Nano-TWIP, Duplex and Triplex steels, having an out-
standing combination of strength and ductility with Rm × A80 of ap-
proximately 50,000 MPa%. However, due to the high alloying costs and
challenging processing, they have been scarcely used in some industrial
applications [11,16,17].
The development of steel grades regarding as the 3rd generation
AHSS is currently ongoing. The mechanical properties of Medium-Mn,
TBF (TRIP-aided Bainitic Ferrite) and Q&P (Quenching and
Partitioning) steels close the gap between the 1st and 2nd generation
AHSS [11,18–21].
Apart from the increase in strength, the reduction in density, e.g.
due to the significant Al addition, is a further opportunity for remark-
able weight savings in modern automotive platforms [21,22]. Both, the
lower atomic mass of Al and the resulting lattice expansion due to the
larger atomic radii of Al compared to pure Fe, contribute to the re-
sulting density reduction. Thus, the addition of 1 wt% Al leads to a
density reduction of approximately 1.3% compared to pure Fe. Drewes
et al. [23,24] have derived a linear relation between the Al-content in
steel and its density (in g/cm³), described by the following formula:
ρ = −0.102*Al[wt%]+7.86 (1)
New steel grades, which unite both TRIP-effect and density-reduc-
tion, are currently the subject of intense development [25–27]. This
includes δ-TRIP steels and Al containing medium Mn lightweight steels
[6,7,28,29].
δ-TRIP steels have a multiphase microstructure consisting of δ-fer-
rite, bainitic ferrite and RA, which transforms to martensite during
plastic deformation [30,31]. Their typical chemical composition is
0.3–0.4 wt% C, 2.0–6.0 wt% Al, 0.2–0.8 wt% Si and 0.5–1.6 wt% Mn
[6,32]. Since δ-TRIP steels undergo the TRIP-effect, they achieve ex-
cellent mechanical properties with tensile strengths between 600 and
800 MPa by total elongations exceeding 30% [6,33,34]. The addition of
Al also enables the existence of δ-ferrite over the entire temperature
range during spot welding, resulting in a microstructure consisting of
both ferrite and martensite. As a result, a fully martensitic micro-
structure in the regions affected by spot welding can be avoided, pre-
venting the occurrence of hardness peaks in both heat affected and
fusion zone [35,36].
Medium Mn steels with a Mn content from 3.5 wt% to 10 wt% al-
loyed with relatively high Al contents have been proposed as a novel
approach for lightweight steels with an excellent combination of
strength and ductility. In these steel grades, the total Al and Si content
typically exceeds 4 wt%, resulting in the desired density reduction [37].
By the addition of Al and Si, the cementite precipitation can be sup-
pressed and furthermore the stacking fault energy (SFE) of the austenite
can be tailored to promote both TRIP and TWIP effects [38]. However,
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Materials Science & Engineering A 735 (2018) 475–486
Al and Si stabilize ferrite and expand the two-phase (α + γ) region
[21], thus increasing the complexity in thermomechanical processing if
hot working in the two-phase range cannot be avoided [39].
As already mentioned in the previous paragraph, there exists a
number of publications related to the development of lightweight steels
containing RA. The present paper however focusses on the development
and in depth characterization of the structure-property relation in
0.4 wt% C, 0.25 wt% Si, 1.1–2.5 wt% Mn and 2.8–5.2 wt% Al steels,
which closes the gap in the state-of-the-knowledge between common δ-
TRIP and lightweight medium Mn steels. Moreover, the main aim of this
work is to study the influence of the Al and Mn additions on the mi-
crostructure, especially the evolution of its individual microstructural
constituents, their grain size and morphology. The resulting mechanical
properties of the present lightweight steels were linked with the find-
ings of the RA stability examinations in order to evaluate their potential
for body-parts applications in the automotive industry.
2. Experimental procedure
The chemical compositions of the investigated δ-TRIP steels and the
resulting relative density reductions Δρ/ρ due to the Al-addition mea-
sured according to DIN EN ISO 1183-1 are listed in Table 1. The four
60 kg steel ingots were cast under laboratory conditions by induction
furnace melting. First, the ingots were heated to a temperature of
1200 °C for 90 min and hot rolled to pre-strips of a thickness of 35 mm.
After reheating, the material was hot rolled to a thickness of 4 mm at a
finishing temperature of 950 °C. In order to simulate a coiling proce-
dure, the strips were cooled from 700 °C at a cooling rate of 0.007 K/s to
300 °C, followed by final air cooling to RT. In order to avoid cracking
during cold rolling, after a dwell time of 1 week, the hot rolled strips
were tempered in a batch-annealing-like furnace at a temperature of
650 °C for 8 h. Finally, the material was cold rolled to a thickness of
1.5 mm.
Thermodynamic simulations were conducted to investigate evolu-
tion of the equilibrium phase fractions of the respective microstructural
constituents as a function of temperature using a ThermoCalc software
(TCFE 6 database).
The cold rolled sheets were heat treated with regard to the
achievement of the desired microstructure and mechanical properties.
To accomplish this, a multipurpose annealing simulator (MULTIPAS)
was employed to simulate industrial continuous annealing. The cold
rolled samples were heated using a rate of 25 K/s to an intercritical
temperature of 850 °C and held for 180 s, followed by quenching with a
cooling rate of 70 K/s to an isothermal over-aging temperature of
400 °C and held at this temperature for 540 s. Finally, the specimens
were quenched to room temperature at a rate of 70 K/s. The material
was cut into strips of 450 × 20 mm2. Three thermocouples were welded
onto the cold rolled sheet surface to monitor the material’s temperature
during annealing. The samples were heated conductively by alternating
current in air atmosphere and cooled by compressed air. Due to the
contact with air and the resulting oxide formation, the samples had to
be pickled in sulphuric acid after annealing.
The microstructure was examined using an imaging SEM (Zeiss
Ultra 55), EBSD (Zeiss Supra 35) with Oxford Instruments NanoAnalysis
and XRD (PANalytical XPert Pro, Co-source, λKα1 = 0.179 nm). For the
Table 1
Chemical composition of the investigated steels in wt% and resulting density
reduction in % measured according to DIN EN ISO 1183-1.
Steel grade C Si Mn Al Δρ/ρ
A: Fe-0.4C-1.1Mn-2.8Al 0.4 0.3 1.1 2.8 4.24
B: Fe-0.4C-1.6Mn-3.3Al 0.4 0.3 1.6 3.3 4.80
C: Fe-0.4C-1.5Mn-5.2Al 0.4 0.3 1.5 5.2 7.38
D: Fe-0.4C-2.5Mn-5.2Al 0.4 0.3 2.5 5.2 7.52
S. Kaar et al.
Fig. 1. Fractions of the equilibrium phases (ferrite, austenite, cementite and κ-carbide) calculated by ThermoCalc.
SEM investigations, the specimens were electrochemically polished and
for EBSD they were mechanically polished with an alkaline dispersion
with nano silica. Using SEM with BSE mode (= Z-contrast) the different
types of carbides could be distinguished with confidence. The quanti-
tative determination of the phase fractions was realized by means of
XRD using the Rietveld-method (HighScore Plus 3.0e, Malvern
PANalytical).
The tensile tests of the heat-treated samples were performed ac-
cording to DIN EN ISO 6892-1, using a Roell-Korthaus RKM 400/100
universal testing machine. For these experiments, flat tensile specimens
with 25 mm gauge length and 12.5 mm width were selected. The tests
were performed at RT using a strain rate of 0.00417 s−1. For each steel
grade, 5 specimens were tested and the average values for the re-
spective mechanical properties were determined.
In addition, the interrupted tensile tests were carried out at different
strain levels for the detailed investigation of the strain-induced auste-
nite to martensite transformation. The saturation magnetization
method (SMM) [40] was used to determine the amount of RA at gra-
dually increased strain. For this purpose, the specimens with the di-
mensions of 3.5 × 10 × 1.5 mm3 were manufactured from the centre of
the tensile samples. In order to ensure comparability between the RA
stability of the investigated steel grades, the kp-value was calculated
according to the Ludwigson-Berger relation [41]:
1 1 kp p
− = *ε
Vγ Vγ0 p (2)
Here, Vγ is the volume fraction of RA, Vγ0 is the initial fraction of
RA, kp is the stability constant, ε is the logarithmic strain and p is a
strain exponent related to the auto-catalytic effect of martensitic for-
mation. According to Matsumura et al. [42] p can be considered as 1 for
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Materials Science & Engineering A 735 (2018) 475–486
TRIP-steels as the autocatalytic effect can be neglected close to RT. The
lower kp, the higher the stability of RA.
Both morphology and grain size of the RA islands were examined by
analyzing SEM images using the software ImageJ. The equivalent circle
diameter (ECD) was determined as a representative value for the grain
size of RA, according to the following equation:
4*Aγ
ECD =
π (3)
Here Aγ is the area of the RA grains. The equivalent circle diameter
represents the diameter of the RA grain, if it was circular.
Since the morphology of RA significantly influences the RA stability,
a form factor was introduced:
Aγ
circularity = 4*π*
Pγ2 (4)
Here, Aγ is the area and Pγ is the perimeter of the RA grains. The
circularity can vary between 0 and 1, whereby a factor of 1 means that
the grain is circular, whereas a factor of 0 means that the grain is
stretched infinitely.
The carbon content in RA was calculated using the equation pro-
posed by Dyson and Holmes [43]:
a γ −3.578 − 0.0056*XAl −0.00095*XMn
XC =
0.0033 (5)
Here, aγ represents the austenite lattice parameter in nm and XC, XAl
and XMn are the contents of carbon, manganese and aluminum in wt%,
respectively. The lattice parameter aγ was measured by XRD at an ac-
celeration voltage of 35 kV and a filament current of 45 mA using a
PANalytical XPert Pro diffractometer. The Al and Mn contents in RA
S. Kaar et al.
were measured by the use of energy dispersive X-ray (EDX) analysis
during the EBSD data acquisition.
The MS-temperature in °C was determined taking into account the C,
Mn, Si and Al content in RA using the equation according to Mahieu
[44]:
MS = 539 − 423C − 30.4Mn − 7.5Si+30Al (6)
3. Results
3.1. Thermodynamic simulation
Fig. 1 represents the fractions of the equilibrium phases ferrite,
austenite, cementite and κ-carbides for the four investigated steels,
calculated by ThermoCalc. When reaching the solidus temperature, δ-
ferrite started to transform from the liquid state. During cooling the
amount of δ-ferrite increased, until the Ac3-temperature of approxi-
mately 1400 °C was reached, whereby the formation of austenite started
from this point onward. For the steels with 2.8 and 3.3 wt% Al a full
austenitization could be reached, whereas for the steel grades con-
taining 5.2 wt% the presence of δ-ferrite in the microstructure in the
entire temperature range, i.e. from liquidus-temperature to RT, could
be predicted by thermodynamic calculations. In this respect, the
minimum value of approximately 25 vol% could be forecast at a tem-
perature close to 1250 °C. During further cooling, the austenite content
decreased, while the amount of α-ferrite increased. For all investigated
compositions, at a temperature of 850 °C, the phase fractions of ferrite
and austenite were approximately 55 and 45 vol%, respectively. At a
temperature of approximately 750 °C the carbide formation took place,
namely cementite for the steels with the lower Al-content and κ-
Fig. 2. SEM micrographs of the (a) A: Fe-0.4C-1.1Mn-2.8Al, (b) B: Fe-0.4C-1.6Mn-3.3Al, (c) C: Fe-0.4C-1.5Mn-5.2Al, and (d) D: Fe-0.4C-2.5Mn-5.2Al hot rolled
sheets.
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Materials Science & Engineering A 735 (2018) 475–486
carbides for those with the higher Al-content. After reaching the Ac1
temperature, which was approximately alike for all investigated com-
positions, no austenite should be present in the microstructure.
Therefore, the final predicted microstructure after hot rolling and
coiling should consist of α-ferrite and cementite for the steels A and B,
while α- and δ-ferrite along with κ-carbides can be expected for the
steels C and D, respectively.
3.2. Microstructure
Fig. 2 shows the SEM images of the batch-annealed hot rolled strips
for the steels A–D. As already predicted by the equilibrium calculations,
for the steels A and B the microstructure consisted of α-ferrite and
pearlite, whereas with increasing Al- and Mn-content (steel C and D) κ-
carbides were present in the matrix consisting of α- and δ-ferrite. The
batch-annealing treatment at 650 °C for 8 h led to a spheroidization of
the carbides. In particular, the commonly lamellar pearlite altered its
morphology to more spheroidal one. However, regardless of the che-
mical composition, the secondary phases were present in the form of
bands aligned parallel to the rolling direction.
The XRD patterns of the batch-annealed hot rolled steels are illu-
strated in Fig. 3. For the steels A and B, the intensity peaks of ferrite and
cementite were detected, the presence of κ-carbides was not observed.
At the higher Al-contents (steel C and D), the intensity peaks related to
cementite decreased, while characteristic κ-carbide Bragg peaks started
to appear.
Table 2 gives an overview of the individual constituents in the mi-
crostructure of the batch-annealed hot rolled steels calculated from the
XRD data by means of the Rietveld-method. At low Al-contents, namely
2.8 and 3.3 wt% (steel A and B), 5.7 and 5.4 wt% cementite were
S. Kaar et al.
Fig. 3. XRD pattern of the batch-annealed hot rolled steels A–D.
Table 2
Fraction of the individual constituents present in the structure of the batch-
annealed hot rolled steels A–D in wt%.
Steel Ferrite Cementite Kappa
A: Fe-0.4C-1.1Mn-2.8Al 94.3 ± 0.83 5.7 ± 0.32 < 0.1
B: Fe-0.4C-1.6Mn-3.3Al 94.6 ± 0.85 5.4 ± 0.28 < 0.1
C: Fe-0.4C-1.5Mn-5.2Al 90.1 ± 0.77 < 0.3 9.9 ± 0.41
D: Fe-0.4C-2.5Mn-5.2Al 91.5 ± 0.78 < 0.3 8.5 ± 0.39
present in the microstructure, whereas the increase of Al to 5.2 wt%
(steel C and D) led to the formation of 9.9 and 8.5 wt% κ-carbides in-
stead of cementite. For the steels C and D the volume fraction of ce-
mentite was below the detection limit.
The SEM micrographs of the cold rolled sheets intercritically heat-
treated using the MULTIPAS simulator are shown in Fig. 4. On the one
hand, it can be seen that the microstructure of the steels A and B
consisted of ferrite, RA and bainite. On the other hand, with increasing
Al-content martensite was formed during cooling, resulting in a final
microstructure of ferrite, RA, martensite and only small amounts of
bainite for the steels C and D, respectively. The morphology of RA in
case of the steel A and B with a lower Al content can be characterized as
a mixture of grains with lamellar and globular morphology. However,
for the steel C and D with a higher Al content, the islands of RA em-
bedded in the ferritic matrix were predominantly globular-shaped.
Fig. 5 depicts the EBSD phase maps of the investigated cold rolled
steels, enabling the distinction of the ferritic matrix (blue), the RA is-
lands (red) and the bct-martensite (green) adjacent to the RA, respec-
tively. It is evident that the present phase maps manifest the differences
in microstructure between the steel grades with the lower and higher
Al-content. For the steels containing the lower Al-contents (steel A and
B), the microstructure consisted of ferrite and RA (18.7 and 23.4 vol%),
whereas for the steel grades C and D with the higher Al-content, besides
ferrite and RA (22.9 and 22.6 vol%), bct-martensite could be observed
in the microstructure.
3.3. Mechanical properties
Fig. 6 represents the stress-strain curves for the cold rolled and in-
tercritically heat-treated steels A to D. It is obvious (Fig. 6(a)) that both
increasing Al- and Mn-contents led to a significant decrease of the yield
strength (Rp0.2), the increase of the tensile strength (Rm), while both
uniform and total elongation (A80) declined. Due to the absence of
skinpassing, a pronounced discontinuous yielding could be observed for
all investigated steel grades due to the segregation of C atoms in the
form of well-known Cottrell atmospheres in vicinity of dislocations
during annealing and thus, the impediment of their movement took
place. By the effect of stresses, the dislocations were unpinned, re-
sulting in the formation of Lüders bands [45]. However, this effect
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Materials Science & Engineering A 735 (2018) 475–486
could be reduced for the steels with higher alloying contents (steel C
and D) as a consequence of the presence of athermal martensite in the
initial microstructure. This allows for the formation of fresh unpinned
mobile dislocations at the interfaces between ferrite and martensite
starting from the onset of straining. The pronounced work hardening at
the beginning of straining can therefore be enabled and the localization
of plastic deformation in the form of Lüders bands can be significantly
diminished [2].
Fig. 6(b) displays the average values of the mechanical properties
for all investigated density reduced TRIP steels. The tensile strength
increased by the addition of Al and Mn from 725 to 1050 MPa with a
decrease of the total elongation from 39% to 17%. Henceforth, a pro-
duct of the tensile strength and total elongation of 28,240, 29,520,
20,750 and 18,040 MPa% from the steel A to D could be reached. Fi-
nally, the yield strength declined from 555 to 385 MPa with an increase
of both Al and Mn content.
4. Discussion
4.1. Effects of Al and Mn on the microstructural evolution
The microstructure of the hot rolled steels A-D was investigated by
means of SEM and XRD. For the steels A and B with 2.8 and 3.3 wt% Al,
respectively, the microstructure consisted of ferrite and cementite. On
the contrary, the increase of the Al-content to 5.2 wt% led to the for-
mation of κ-carbides on the expense of cementite, wherein the κ-car-
bides were located in the form of bands and partially located along the
ferrite grain boundaries. Using SEM operated in the SE-mode, the dis-
tinction of individual types of carbides, i.e. cementite vs. κ-carbides,
was impossible. Since both carbide species have the different crystal-
lographic structure, this issue can be solved for example by the em-
ployment of the XRD technique. In this respect, it is well known that
cementite has an orthorhombic structure whereas κ-carbides crystallize
in an anti-perovskite one. It is however apparent that the sample pre-
paration and data treatment of the XRD analysis is a rather time con-
suming process. Furthermore, the XRD analysis only allows for the
identification of individual microstructural compounds in a material,
but the detection of their exact location within the microstructure
cannot be realized using this technique. Taking these difficulties of XRD
into consideration, another observation method was proposed in the
present study. In this context, SEM using the BSE-imaging mode can be
employed for the fast and reliable identification of carbides and ex-
amination of their location in the microstructure. The intensity of the
BSE mode is primarily dependent on the average atomic number of the
given microstructural compound, known as the Z-contrast [46]. At
primary electron energies exceeding 5 keV heavy elements reflect a
larger quantity of back-scattered electrons, appearing brighter than
light elements in the BSE image. Thus, cementite and κ-carbides can
easily be distinguished using this method.
S. Kaar et al.
Fig. 4. SEM micrographs of the (a) A: Fe-0.4C-1.1Mn-2.8Al, (b) B: Fe-0.4C-1.6Mn-3.3Al, (c) C: Fe-0.4C-1.5Mn-5.2Al, and (d) D: Fe-0.4C-2.5Mn-5.2Al cold rolled
sheets.
Fig. 7 depicts the SEM images with the BSE contrast of the hot rolled
steels A–D, wherein the clear distinction between cementite (bright)
and κ-carbides (dark) based on the Z-contras t in the BSE-mode can be
stated. Given that, the present method can detect the presence of κ-
carbides in a simple and fast way.
It is evident from the difference in backscatter coefficients that ce-
mentite and κ-carbides must differ in their chemical composition, which
was additionally proven by means of WDX. Table 3 presents the results
of the WDX analysis of ferrite, cementite and κ-carbides. Both cementite
and κ-carbides contained lower amounts of Fe and Si than the ferritic
matrix. but they were distinctively enriched in C and Mn. It can also be
seen in Table 3 that κ-carbides had the largest amount of Al, whereas
cementite contained the highest amounts of Mn and C.
After annealing of the cold rolled material, the final microstructure
consisted of ferrite, RA, bainite or martensite (Fig. 4). During the
heating stage to the intercritical annealing temperature of 850 °C, be-
sides the recrystallization of the cold deformed microstructure, both κ-
carbides and cementite could be successfully dissolved. This could be
accomplished due to the fact that the temperature of the complete
carbide dissolution of approximately 750 °C, as predicted by Thermo-
Calc calculation (Fig. 1), was significantly exceeded. During inter-
critical annealing, the ferrite to austenite formation took place. It is also
evident from the ThermoCalc calculations (Fig. 1) that for the steels A
and B with a lower Al content a higher amount of intercritical austenite
was formed compared to the steels C and D with a higher Al-content.
This means in the latter case a higher enrichment of intercritical aus-
tenite in C and Mn compared to the former one. This phenomenon was
reflected during the holding of the investigated steels in the region of
the isothermal bainitic transformation (IBT), so-called over-aging. For
the steel grades containing lower amounts of Al, a certain amount of
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Materials Science & Engineering A 735 (2018) 475–486
bainite was formed during isothermal holding at 400 °C. It is generally
known that Al accelerates the bainitic reaction [47,48] and high
amounts of bainite can be formed during over-aging, since due to its
strong ferrite stabilization effect the T0-line is shifted to the larger C-
contents in remaining austenite [49,50]. This is however in contrast
with the results obtained in the present study, while the increase of the
Al-content to 5.2 wt% led indirectly via above mentioned pronounced C
and Mn enrichment of remaining austenite prior to over-aging to the
postponed formation of bainite. As a result rather low amount of bainite
could form during the over-aging stage for the density-reduced TRIP
steels with the higher Al content. Both SEM (Fig. 4) and EBSD (Fig. 5)
images confirmed this statement, where the final microstructure of the
steels C and D included bct-martensite instead of bainite.
In addition, dilatometry was applied for the detailed investigation of
the IBT in the over-aging section using the parameters in analogy with
the laboratory annealing simulations. In general, for all investigated
steel grades rather minor IBT could be detected at 400 °C (Fig. 8). The
largest IBT was observed for the steel B followed by the steel A. How-
ever, for both steels C and D, the IBT was evidently suppressed, as re-
flected by the small length variations measured by dilatometry. Due to
the postponed IBT, the remaining austenite could not sufficiently be
enriched in C and transformed to athermal martensite upon final
cooling. This is an additional confirmation of the presence of fresh bct-
martensite in the microstructure, as already stated by the SEM (Fig. 4)
and EBSD (Fig. 5) examination.
4.2. Correlation between microstructure and tensile properties
Both type and morphology of the microstructural constituents can
affect the tensile properties of the annealed cold rolled sheet steels.
S. Kaar et al. Materials Science & Engineering A 735 (2018) 475–486

Fig. 5. EBSD phase maps of the (a) A: Fe-0.4C-1.1Mn-2.8Al, (b) B: Fe-0.4C-1.6Mn-3.3Al, (c) C: Fe-0.4C-1.5Mn-5.2Al, and (d) D: Fe-0.4C-2.5Mn-5.2Al cold rolled
sheets.

With increasing Al- and Mn-contents, the tensile strength increased,
while the total elongation was reduced. The presence of fresh marten-
site in the microstructure of the steels C and D led to a declination of
yield strength. Since the microstructure of the steels A and B was
comparable, consisting of RA and bainitic islands embedded in the
ferritic matrix, they also had similar mechanical properties. When the
Mn-content was increased from 1.1 to 1.6 wt% (from the steel A to B),
the yield strength slightly increased as a consequence of an enhanced
solid solution hardening. Furthermore, the tensile strength rose from
725 to 834 MPa, while the total elongation decreased from 39% to 35%.
Further increase of the Al-content from 3.3 to 5.2 wt% led to a sharp
decrease of the yield strength to 434 MPa, caused by the presence of
athermal martensite in the final microstructure. For this reason the
tensile strength rose up to 943 MPa, accompanied with a decrease in
total elongation to 22%. When the Mn-content was further increased to
2.5 wt%, a larger amount of athermal martensite was formed in the
microstructure, resulting in a further decrease in yield strength to
384 MPa due to internal stresses, occurring at the interface between
ferrite and martensite. This stemmed from the volume expansion re-
lated to the austenite to martensite transformation. Therefore, yielding
started in the vicinity of these areas, even under a very low applied
stress [51]. In addition, the presence of larger quantities of athermal
martensite caused a further increase in tensile strength to 1055 MPa
and a reduction in total elongation to 17%.

Fig. 6. (a) Stress-strain curves for the cold rolled steels A–D without skin-pass, (b) mechanical properties for the cold rolled steels A–D without skin-pass.

481
S. Kaar et al. Materials Science & Engineering A 735 (2018) 475–486

Fig. 7. SEM micrographs of the (a) A: Fe-0.4C-1.1Mn-2.8Al, (b) B: Fe-0.4C-1.6Mn-3.3Al, (c) C: Fe-0.4C-1.5Mn-5.2Al, and (d) D: Fe-0.4C-2.5Mn-5.2Al hot rolled
sheets, showing the clear distinction between cementite (bright) and κ-carbides (dark) based on the Z-contrast in the BSE-mode.

Since all investigated steel grades contain metastable RA, which can
transform to strain-induced martensite prior to necking, their strain
hardening response characterized by strain hardening rate as a function
of logarithmic strain was investigated in detail (Fig. 9). It can be seen
that the strain hardening rate of both steel A and B decreased at the
onset of straining, followed by a plateau during further deformation.
For the steel C with higher Al-content, the strain rate was higher at the
beginning of straining and declined slower with increasing strain
compared to the steels A and B. Finally, the steel D with both increased
Al- and Mn-content, extensively hardened in the initial stage of
straining followed by an abrupt decrease of strain hardening rate with
further deformation. Such a strain hardening behavior can indicate a
lower RA stability and thus a faster and earlier strain-induced austenite
to martensite transformation of the steel D compared to the steels A-C.
The present results are in analogy with the investigation of Sohn et al.
[52], i.e. for the steels with microstructures consisting of ferrite, RA and
bainite, where a similar strain hardening behavior was found to that of
the steels A and B. Moreover, the investigated steels containing mar-
tensite also displayed a comparable evolution of strain hardening rate
to that of the present steels C and D.
It can be deduced from the reduced elongation of the steels C and D,
stemming from the high strain hardening at the beginning of straining
that the mechanical properties can be significantly influenced by the
strain-induced martensitic transformation. In order to determine the
stability of RA against strain-induced martensitic transformation, in-
terrupted tensile tests were carried out, followed by the magnetic
measurement of the RA fraction at gradually increased strains.
Fig. 10(a) displays the RA content as a function of engineering strain for
the investigated steels A–D. For the steels A and B, the amount of RA
decreased less pronouncedly compared to the steel grades with higher

Table 3
Distribution of the alloying elements in ferrite, cementite and κ -carbides for the batch-annealed hot rolled steel D: Fe-0.4C-2.5Mn-5.2Al (SEM-BSE image and WDX-
analysis).

482
S. Kaar et al.
Fig. 8. Dilatometry curves of the annealed cold rolled steels A–D showing the
IBT.
Fig. 9. Strain hardening rate as a function of logarithmic strain for the annealed
cold rolled steels A–D.
Al-content. Obviously, the volume fraction of RA declined almost lin-
early for the steels A and B, whereas in case of the steels C and D with
an increased Al-content, the decrease was sharply regressive. In
Fig. 10(b), the amount of transformed austenite is plotted as a function
of logarithmic stain according to the Eq. (2). This relation enables the
linearization of the results and therefore more straightforward
Fig. 10. (a) RA content as a function of engineering strain, (b) transformed RA content as a function of logarithmic strain determined by the Eq. (2).
483
Materials Science & Engineering A 735 (2018) 475–486
comparison of their RA stability among the investigated steel grades.
For the steels A and B, the kP-value was 20.9 and 34.5, whereas for the
steels C and D, it was 154.9 and 152.1, respectively. Therefore, the
higher RA stability could be stated for the steels containing 2.8 and
3.3 wt% Al compared to the ones with the higher Al content. Hence-
forth, apart from the presence of the fresh martensite in the micro-
structure of the steels C and D, the more rapid strain-induced marten-
sitic transformation (SIMT), as an aftermath of lower RA stability, is an
additional explanation of the increased tensile strength and decreased
elongation compared to the steels A and B (Fig. 6).
The main factors, influencing the RA stability, were also thoroughly
investigated in the present study. Since both grain size and morphology
of RA have impact on its mechanical stability, these two parameters
were analyzed in detail by means of optical methods. The minimum,
maximum, median and mean ECD and circularity of the RA grains were
determined for all investigated density-reduced TRIP steels and they are
illustrated in Fig. 11 in the form of boxplots. The present boxplots
consist of a box including 50% of the averaged data. The two horizontal
lines situated outside the box, represent the minimum and maximum
values of the evaluated data. Furthermore, the horizontal line, located
inside the box, marks the median and the square represents the mean
value. Due to a variety of grain sizes within the microstructure of each
investigated steel grade, the median was determined to be the most
important value, representing the final grain size. It is evident from
Fig. 11(a) that the smallest grains could be measured for the compo-
sitions containing less Al, whereas with increasing Al-content the grain
size of RA became evidently larger. The equivalent circle diameter for
the steels A and B was 573.5 and 488.3 nm, while for the steels C and D
it was 1005.0 and 1117.3 nm, respectively.
The circularity was also calculated as a measure representing the RA
morphology (Fig. 11(b)). The closer the circularity to 1, the more
globular the grains. Since the circularity for the steels A and B was
approximately 0.29, the RA grains were more lamellar. In opposite, for
the steels C and D, the circularity was between 0.64 and 0.56, in-
dicating a noticeable globular RA morphology. Given that, the highest
mechanical stability of RA could be found for the steels containing 2.8
and 3.3 wt% Al, since their microstructure contained the smaller and
more lamellar grains compared to the steel grades with the higher Al
content (the steel C and D). This in turn contributed to the enhanced
combination of strength and ductility for the steels A and B compared to
the steels C and D.
The chemical stability of RA, represented by the chemistry of this
microstructural compound, is another factor, influencing the overall RA
stability and therefore it was thoroughly investigated in the present
contribution as well. The Mn-, Al- and C-contents in RA and its lattice
parameters are listed in Table 4. The Mn-content of RA was measured
by means of EDX, whereas the C-content was calculated from the XRD
S. Kaar et al.
Fig. 11. (a) ECD and (b) circularity of RA in the final annealed steels A–D.
data according to Eq. (5). Based on these two methods, an evident Mn-
and C-enrichment of RA compared to the bulk composition could be
detected. The lowest amount of Mn in RA was measured for the steel A
(1.6 wt%), while the largest Mn-content in RA had the steel grade D
(3.4 wt%) as the consequence of the highest overall Mn-content in the
steel composition. The calculation of the C-content in RA revealed its
largest enrichment for the steel A (1.5 wt%), followed by the steel B
(1.2 wt%) and the steel C (1.2 wt%). On the contrary, for the steel grade
D, the lowest C-content in RA was calculated (0.9 wt%). In order to
describe the effect of both C- and Mn-content in RA on its chemical
stability, the MS-temperature of RA was calculated according to the Eq.
(6): The lower the MS-temperature the higher necessary chemical
driving force for the austenite to martensite transformation. On that
account, the highest chemical RA stability could be inferred for the steel
A, followed by B, C and finally the steel D. In this context, it can be
stated that both lowest chemical and mechanical RA stability of the
steel D were responsible for the very high strain rate at the onset of
straining (Fig. 9), compared to steel C, leading to the highest tensile
strength and lowest elongation (Fig. 6).
Apart from the above-mentioned factors, SFE of RA also contributes
to the overall RA stability of a steel [14]. It is well known from the
literature [53,54] that Al increases SFE of RA, resulting in its higher
stability. Taking into account the chemistry of steel B and C with the
equivalent C, Mn and Si content in both steel chemical composition
(Table 1) and in RA (Table 4), an increased Al content in the steel C
should stabilize RA more effectively compared to the steel B. Never-
theless, the RA stability for the steel B and C, analyzed in Fig. 10, be-
haved exactly in the opposite way. In that sense, it can be concluded
that the factors, investigated in the preceded paragraphs, play a major
role in the overall RA stability of the present density- reduced TRIP
steels, largely overweighting the impact of the SFE in the RA.
5. Conclusion
In the present contribution, the structure-property relationships of
the four different density-reduced TRIP steels with Al-contents between
2.8 and 5.2 wt% and Mn-contents ranging from 1.1 to 2.5 wt% were
Table 4
Results for the C-, Al- and Mn-content in RA and the corresponding MS-temperature.
Steel A: Steel B:
XMn [wt%] 1.6 ± 0.2 2.2 ± 0.2
XAl [wt%] 2.61 ± 0.2 3.11 ± 0.3
aγ [nm] 0.3644 ± 0.0012 0.36385 ± 0.0011
XC [wt%] 1.5 1.2
MS [°C] −71 38
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Materials Science & Engineering A 735 (2018) 475–486
investigated in detail. The study concentrated on the influence of the
Al- and Mn-addition on the microstructure, mechanical properties and
RA stability of these steel grades. The main findings of the present paper
can be summarized as follows:
• Significant influence of the steel chemistry, especially the Al-con-
tent, on the microstructural evolution could be observed in the as
hot rolled state. For the steels containing lower Al-contents, the
microstructure consisted of ferrite and cementite, whereas for those
with an increasing Al-content, predominantly κ-carbides were pre-
sent in the ferritic microstructure instead of cementite.
• By means of SEM using the Z-contrast a fast and reliable distinction
between cementite and κ-carbides became possible even without the
application of more complex XRD method.
• Concerning the steel density, the addition of Al led to its reduction
as a consequence of lower atomic mass and the lattice expansion due
to larger atomic radii compared to Fe. For the steels A to D, a density
reduction of 4.2%, 4.8%, 7.4% and 7.5% could therefore be ob-
tained.
• The heat treatment of the cold rolled sheets led to the dissolution of
cementite and κ-carbides, resulting in a final microstructure of fer-
rite, RA and bainite or martensite, depending on steel chemistry.
The amounts of RA, measured by saturation magnetization, ranged
from 19 to 23 vol%. With increasing Al-content, the bainite forma-
tion was indirectly suppressed due to the presence of larger amount
of intercritical ferrite, which increased the C content in the austenite
prior to IBT. This in turn resulted in the formation of martensite
upon final cooling.
• Tensile testing revealed a substantial impact of the overall chemical
composition on the mechanical properties of the investigated steels.
The increase of the Al- and Mn-contents led to the decrease of the
yield strength from 560 to 380 MPa due to the presence of fresh
martensite in the steel microstructure. Furthermore, with increasing
alloying content, the tensile strength increased from 724 to
1055 MPa due to the lower RA stability, resulting in a faster strain-
induced austenite to martensite transformation. As a result, the total
elongation of the investigated steels also declined from 39% to 17%.
Steel C: Steel D:
2.3 ± 0.2 3.4 ± 0.3
4.63 ± 0.3 4.75 ± 0.3
0.36448 ± 0.0009 0.36376 ± 0.0006
1.2 0.90
113 195
S. Kaar et al.
The best combination of strength and ductility was achieved for the
steel containing 3.3 wt% Al and 1.6 wt% Mn, whereby the product
of tensile strength and total elongation reached 29,520 MPa%.
• For the steels containing 2.8 or 3.3 wt% Al, both the highest me-
chanical and chemical stability of RA could be established due to the
smaller and more lamellar grains. Furthermore, the C-content in RA
was higher for these steel grades, which additionally contributed to
the RA stabilization. The resulting TRIP effect remarkably enhanced
the product of tensile strength and total elongation of these parti-
cular steel grades.
In comparison to the first generation AHSS, the investigated steels
had comparable or even significantly improved mechanical properties
in the range from 18,040 MPa% to 29,520 MPa% by an advantageous
density reduction as an aftermath of the Al additions. Therefore, the
present density reduced steels can be considered as a suitable candidate
for safety related lightweight applications in the automotive industry.
However, in order to ease their manufacturing, the evaluation of im-
portant processing characteristics such as joining and forming should be
the scope of future research.
Acknowledgement
The authors sincerely acknowledge the R&D collaboration platform
between voestalpine Stahl GmbH and ThyssenKrupp Steel Europe,
which allowed for the realization of the common project, related to the
development of density-reduced TRIP steels.
Appendix A. Supplementary material
Supplementary data associated with this article can be found in the
online version at doi:10.1016/j.msea.2018.08.066.
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