Materials Science & Engineering A 588 (2013) 142–150

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Materials Science & Engineering A

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

The influence of Nb on transformation behavior and mechanical

properties of TRIP-assisted bainitic–ferritic sheet steels
K. Hausmann a,n, D. Krizan a,1, K. Spiradek-Hahn b,2, A. Pichler a,3, E. Werner c,4
a
voestalpine Stahl GmbH, voestalpine-Straße 3, A-4020 Linz, Austria
b
Alloy Development Group, Forschungszentrum Seibersdorf, Montanuniversität Leoben, A-2444 Seibersdorf, Austria
c
Lehrstuhl für Werkstoffkunde und Werkstoffmechanik, Technische Universität München, D-85748 Garching b. München, Germany

art ic l e i nf o a b s t r a c t

Article history: In this study the concept of microalloying was applied to TRIP-aided bainitic–ferritic (TBF) sheet steel.
Received 19 June 2013 A newly designed chemical composition was introduced including significantly reduced Si content. The
Received in revised form impact of Nb on phase transformation, microstructure and mechanical properties was investigated. Nb
25 July 2013
addition was found to indirectly accelerate transformation kinetics through grain refinement resulting in
Accepted 1 August 2013
pro-eutectoid ferrite and upper bainite formation. A change in morphology of the bainitic matrix from
Available online 17 August 2013
lath-like to globular was observed as a result of grain refinement. The amount of cementite was reduced
Keywords: and the amount of retained austenite increased through the addition of Nb. The changes in phase
Nb microalloying transformation and microstructure resulted in significantly improved mechanical properties comprising
TRIP-aided steel
both elevated stretch formability and edge crack resistance.
Microstructure
& 2013 Elsevier B.V. All rights reserved.
Mechanical properties

1. Introduction [2]. However, these steels lack sufficient performance in bendability,

Limited access to natural energy resources, global competition
and discussions about climate change resulted in the worldwide
growing interest in fuel savings and emission reduction. The
automotive industry holds great potential to cut fuel consumption
along with CO2 emissions and simultaneously improve passenger
safety [1]. Vast developments in advanced high strength steels
(AHSSs) enable lightweight steel technology through vehicle mass
reduction via significantly reduced material requirements and
increased component complexity.
Intensive recent efforts in steel research have brought about the
“Third Generation” AHSS comprising quench and partitioning (Q&P)
and TRIP-aided bainitic–ferritic (TBF) steels, both defined by their
characteristic microstructure and heat treatment. TRIP steels with
polygonal ferrite (termed conventional TRIP steels in the following) are
well known for their outstanding combinations of strength and stretch
formability comprising both high tensile strength and high elongations
n Since Si is the most suitable for preventing cementite formation
Corresponding author. Tel.: þ 43 50304 15 74671; fax: þ 43 50304 55 4338.
E-mail addresses: katharina.hausmann@voestalpine.com (K. Hausmann).
daniel.krizan@voestalpine.com (D. Krizan), krystina.spiradek-hahn@unileoben.ac.at
(K. Spiradek-Hahn), andreas.pichler@voestalpine.com (A. Pichler).
jahn@wkm.mw.tum.de (E. Werner).
1
Tel.: þ43 50304 15 76021; fax: þ43 50304 55 76021.
2
Tel.: þ43 664 826 7853; fax: þ 43 50550 3330.
3
Tel.: þ43 50304 15 75092; fax: þ 43 50304 55 75092.
4
Tel.: þ49 89 289 15247; fax: þ 49 89 289 15248.
stretch flangeability and edge formability for applications that require
high localized strain realizations [3,4]. Quench and partitioning (Q&P)
steels [5–7] are quenched well below martensite start temperature
and are either isothermally held at quenching temperature or reheated
and held above martensite start temperature. Isothermal transforma-
tion of TBF-steels is conducted above martensite start temperature
so avoiding the formation of (annealed) martensite before the final
cooling. Full austenitization and a critical cooling rate to avoid the
presence of polygonal ferrite in the microstructure are required
for both TBF and Q&P microstructures. The replacement of the poly-
gonal ferritic matrix, as present in conventional TRIP steels, by bainite
and/or tempered martensite diminishes hardness differences between
the phases [8–10] resulting in outstanding edge formability and
stretch flangeability. Therefore, Q&P and TBF steels are characterized
by their excellent balance between low edge crack susceptibility and
high uniform and total elongations. While hole expansion and
bendability of TBF steels is slightly inferior to Q&P steels, they possess
outstanding elongations by an extended exploitation of the TRIP-
effect.
during cooling and holding at the overaging temperature, rather
high Si contents of 1.5 mass-% Si are commonly added to TBF steels
[11]. However, Si-additions result in silicon-oxides that are picked
up by the rolls of the production line causing detrimental
indentations on the sheet surface. For conventional TRIP steels
great efforts have been put into finding alternative alloying
concepts to suppress cementite formation. Even though Al fulfills

0921-5093/$ - see front matter & 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.msea.2013.08.023
 K. Hausmann et al. / Materials Science & Engineering A 588 (2013) 142–150
this purpose for conventional TRIP steels, the amount of Al
required to prevent cementite formation in TBF steels causes
unfeasibly high annealing temperatures to fully austenitize the
material [12]. The chemical composition of the steel used as
reference material in the present contribution has been proven
to enable a tremendous reduction of the silicon content. The
microalloying element Nb is known to improve manufacturability
and final properties of AHSS by precipitation strengthening and
grain refinement [13–19]. The influence of Nb on transformation
behavior of conventional TRIP steels has been studied by Pereloma
et al. [20] for the composition of 0.2 mass-% C–1.55 mass-%
Mn–1.5 mass-%Si. The present work fills the gap of combining
third generation AHS-TBF steels of Si o 1:5% with the concept of
microalloying. Detailed insight will be provided into the effect of
Nb addition on transformation behavior, microstructure and
mechanical properties of TBF steels with a minimum tensile
strength of 980 MPa.
2. Experimental procedures
To investigate the influence of Nb on transformation behavior,
microstructure and mechanical properties of TBF sheet steel, a
Nb-free reference material and three Nb containing variants are
considered. The chemical composition of these steels is listed in
Table 1. The steel grades were air cast in a laboratory medium
frequency furnace. The ingots were hot rolled in a laboratory hot
rolling simulator to a thickness of 4 mm. An initial reheating
temperature of 1180 1C, a finishing temperature of 900 1C, and a
coiling temperature of 650 1C were chosen. The hot rolled material
was then cold rolled to a final sheet thickness of 1 mm using a cold
rolling simulator.
The proper adjustment of the heat treatment is crucial for
gaining detailed insight into the correlation between microstruc-
ture and mechanical properties. Therefore, annealing simulations
were performed on as-cold rolled samples with a laboratory
annealing simulator [21]. The samples were heated with 25 K/s,
fully austenitized at 900 1C for 60 s, cooled with 50 K/s to over-
aging temperature ðT oa Þ as shown in Fig. 1. The samples were held
at temperatures ranging from 350 1C to 475 1C applying overaging
times ðt oa Þ between 30 and 600 s and finally cooled to room
temperature at a cooling rate of 50 K/s.
The transformation behavior of the austenitized steels was
characterized by means of dilatometric experiments using a Bähr
dilatometer DIL 805 A/D. Continuous and isothermal dilatometric
measurements were conducted on as-cold rolled material. All
samples (1  3.5  10 mm3) were heated with 25 K/s and fully
austenitized at 900 1C for 60 s. In the continuous cooling experi-
ments the cooling rate was 50 K/s (Fig. 2a). Isothermal heat treat-
ment (overaging) was conducted at 400 1C for 1200 s (Fig. 2b). From
annealing to overaging and for the final cooling to room temperature
a cooling rate of 50 K/s was selected. In subsequent trials for
observations on bainite morphology, the same annealing cycle was
performed at a cooling rate of 30 K/s for the Nb-free reference
material and a cooling rate of 80 K/s for the grade 25Nb between
Table 1
Chemical composition of the investigated TBF steels in mass-%.
Steel C Si Mnþ Crþ Mo Nb
0Nb 0.17 0.79 2.6 0.000
25Nb 0.17 0.78 2.6 0.025
45Nb 0.17 0.78 2.6 0.045
90Nb 0.17 0.78 2.6 0.090
143
Fig. 1. (a) Annealing cycles (time–temperature schedules) indicating heating and
cooling rates, annealing temperatures, and holding times.
Fig. 2. (a) Continuous and (b) isothermal dilatometry annealing cycles, CR: cooling rate.
austenitization and overaging. As a measure of transformation and
precipitation during overaging, the normalized length of the dilat-
ometer sample was determined according to Δlnorm ¼ ðll0 Þ=
lmax  100%, where l is the current length, l0 the length at the
beginning of the overaging step and lmax the total length after
quenching to room temperature.
To reveal the primary austenite grain, samples were annealed
at 900 1C, continuously quenched at cooling rates of at least 120 K/
s and then etched with Bechet–Beaujard etchant. The final micro-
structure obtained from the annealing cycles was analyzed with
light optical microscopy (LOM) using LePera color etchant [22].
Bainite and ferrite appear blue and brown, whereas austenite and
carbon rich martensite appear white and are therefore sometimes
difficult to distinguish. Martensite with less carbon is colored
brownish and can be mainly found within large retained austenite
islands of low stability against martensite transformation. This
combination is known as martensite/austenite constituent.
For scanning electron microscopy (SEM) the samples were
mechanically polished using first silicon carbide paper followed by
diamond spray and were then electropolished with perchloric acid.
Energy dispersive X-ray spectroscopy (EDX) was used to identify the
composition of selected precipitates during SEM observations. Thin
foils were produced for transmission electron microscopy (TEM)
observations by mechanical grinding of disks of 3 mm diameter
followed by electropolishing in acetic acid containing 5–10% per-
chloric acid. A Philips CM20 with an acceleration voltage of 200 kV
was used for TEM analysis. In addition, the equivalent circle
diameter (ECD) of about 500 particles of bainite and austenite was
determined separately using high resolution (HR) TEM.
Inductively coupled plasma mass spectroscopy (ICP-MS) was
N used to reveal the amount of Nb precipitated. The amount of
precipitated NbC as a function of temperature was calculated using
0.005 ThermoCalc in conjunction with the database TCFE6. All fcc and
0.004 bcc phases and cementite were considered in these calculations.
0.005
0.006
The strain induced transformation behavior of retained austenite
was investigated by means of interrupted tensile tests. For this,
144 K. Hausmann et al. / Materials Science & Engineering A 588 (2013) 142–150

tensile tests were interrupted at different tensile strains between

1% and 10% in steps of 1%. An additional sample was strained to
0.5% tensile strain. The amount of untransformed retained auste-
nite of these samples and of all other microstructures was
determined by magnetic measurements using the saturation
magnetization method (SMM) [23]. The carbon content of the
retained austenite was calculated with the formula of Dyson and
Holmes [24] from austenite lattice constants obtained by XRD
peak evaluation with the Rietveld method [25].
To obtain the mechanical properties tensile testing was per-
formed according to the international standard ISO 6892-1 on a
ZWICK-Roell BTC-FR020TN tensile testing machine. To quantify
the differences in work-hardening behavior, the work-hardening
rate and the differential n-value n′ are calculated according to
standard E 646. The work-hardening rate θ ¼ dst =dφl is deter-
mined by the true stress st and the logarithmic strain φl in the
tensile direction. The differential n-value is defined as follows:
dðln st Þ
n′ ¼ : ð1Þ
dðln φl Þ
Hole expansion tests were performed on samples with a
punched hole corresponding to the testing procedure ISO/WD
16630 applying a conical expansion tool with a top angle of
601 711. The hole expansion strain λ ¼ ðdd0 Þ=d0  100% was
calculated from the initial diameter d0 and the final diameter d
of the expanded hole.

3. Results

Nb plays a crucial role for the grain refinement of many steel

grades [13–19]. Bechet–Beaujard etching is used to reveal the prior
austenite grain size of the investigated TBF steels (Table 2) [26].
The primary austenite grain size of the Nb-free reference material
is significantly larger than the grain size of the niobium containing Fig. 3. (a) LePera etched LOM micrograph and (b) SEM micrograph of TBF steel
steels. 25Nb for a fixed overaging temperature and time of T oa ¼ 400 1C and t oa ¼ 600 s,
Fig. 3 shows a typical example of a TBF steel microstructure as respectively.
observed in the light optical microscope (Fig. 3a) and in the
scanning electron microscope (Fig. 3b) after isothermal holding
the black round dots appearing in the grade 45Nb (Fig. 5c) and even
at T oa ¼ 400 1C for t oa ¼ 600 s. Due to LePera's etchant, the bainitic
larger in the grade 90Nb (Fig. 5d) were identified as Nb carbides.
matrix appears brown/blue (Fig. 3a). The numerous small white
The composition of the carbides was identified by selected area
areas indicate retained austenite. The large white areas in the
diffraction (SAD) in the transmission electron microscope. Fig. 6
micrograph of Fig. 3a potentially contain martensite, which
gives an example for the identification of a large precipitate. The
appears as a white pattern in the SEM image (Fig. 3b) as opposed
Laue-/Bragg-indices Fig. 6b were deduced from selected area
to the dark and even elevated retained austenite inclusions.
diffraction patterns (SADPs) (Fig. 6a).
The SEM-microstructures of all Nb-variants and the Nb-free
Two populations of NbC particles are present in the Nb-
reference material are shown in Fig. 4. The bainite of the Nb-
containing steels. Quantitative analysis (Table 3) reveals that all
variants appears more globular as compared to the mainly lath-
Nb-variants contain both NbC particle populations. While the
like bainite of the reference material. Also, the reference material
density of coarse NbC particles remarkably increases with the Nb
contains large amounts of lath like retained austenite, while the
content, no significant trend was found regarding the density of
retained austenite of the grades with Nb addition appears more
fine NbC particles.
blocky-like.
To investigate the potential to dissolve the NbC particles during
Transmission electron microscopy (TEM) is a valuable tool to
annealing the amount of undissolved Nb was measured before and
confirm the SEM observations with respect to the change in bainite
after annealing. The greater the Nb content the more Nb pre-
and retained austenite morphology as well as to gain quantitative
cipitates were observed (Fig. 7). Since the results for the as-cold
information on carbide precipitation. The TEM analysis performed on
rolled and annealed samples mutually fall into their scatter bands,
all investigated steel grades (Fig. 5) confirms the SEM results in terms
a significant dissolution or further precipitation of NbC during the
of these morphology changes. Moreover, considerably less cementite
austenitization step can be excluded. Due to the filtering technique
is found in the bainite of the Nb microalloyed TBF steels. Using EDX
employed in this analysis, fine particles are hardly detected. The
amounts shown are therefore minimum amounts of Nb carbides.
Table 2
Prior austenite grain size after quenching from annealing temperature T an ¼ 900 1C The transformed austenite fraction of continuously cooled
for the niobium free steel and the three steels alloyed with Nb. samples (cooling rate 50 K/s) is shown in Fig. 8a as a function of
temperature. Down to a temperature of 400 1C the reference
Steel 0Nb 25Nb 45Nb 90Nb material does not begin to transform, whereas the austenite of
ECD ½μm 12.1 77.3 6.0 7 3.4 5.3 7 2.9 5.5 7 3.1
the Nb alloyed steels transforms starting at 640 1C until the
overaging temperature is reached where roughly 20% ferrite and
 K. Hausmann et al. / Materials Science & Engineering A 588 (2013) 142–150 145

Fig. 4. SEM micrographs of (a) 0Nb (b) 25Nb (c) 45Nb (d) 90Nb heat treated TBF steels (T oa ¼ 400 1C and t oa ¼ 600 s).

Fig. 5. TEM micrographs of (a) 0Nb (b) 25Nb (c) 45Nb (d) 90Nb heat treated TBF steels (T oa ¼ 400 1C and t oa ¼ 600 s).

upper bainite are formed. The same transformation behavior is
observed for all Nb-variants.
Fig. 8b illustrates the effect of Nb on the isothermal bainitic
transformation (IBT) at 400 1C. All steel grades transform approxi-
mately with the same velocity and transformation is completed
after about 120 s. The amount of isothermal bainite as shown in
Fig. 8b is less for Nb microalloyed steels. The fractions of both the
isothermal bainite and the transformation product of cooling to
overaging (Fig. 8a) add up to approximately the same amount.
The amount of retained austenite as a function of overaging time
is given in Fig. 9a. In all steel grades it initially increases followed by a
saturation after about 200 s. The most significant increase of retained
austenite as compared to the reference material was observed for the
25Nb steel. A further increase of the Nb content does not result in a
further increase of the amount of retained austenite.
The stability of retained austenite against strain induced
martensitic transformation was studied by measuring the amount
of retained austenite as a function of tensile strain (Fig. 9b) by
means of interrupted tensile tests. The amount of retained auste-
nite decreases with increasing plastic deformation. Transformation
slows down a few percent before fracture strain is reached. All
steel grades show almost the same stability behavior.
146 K. Hausmann et al. / Materials Science & Engineering A 588 (2013) 142–150
Fig. 6. (a) Selected Area Diffraction Pattern (SADP) and (b) Laue-/Bragg-indices of a NbC particle shown in Fig. 5d.
Table 3
Two NbC particle populations, fine and coarse, characterized by ECD and density of these precipitates in the steels 25Nb, 45Nb and 90Nb.
Fine NbC particles
Steel 25Nb 55Nb
ECD [nm] 5.7 7 1.9 6.4 7 2.8
Particle density [1/m2 ] 767 13 657 21
Fig. 7. Amount of undissolved Nb as a function of the overall niobium content for
steel grades 25Nb, 45Nb and 90Nb measured by ICP-MS.
The carbon content of retained austenite for the entire steel
series is given in Table 4. All steels, the reference material as well
as the Nb microalloyed variants, contain the same amount of
carbon in the retained austenite after an isothermal heat treat-
ment at T oa ¼ 400 1C and t oa ¼ 600 s.
Yield and tensile strength as a function of overaging time are
given in Fig. 10a for all steel grades after overaging at 400 1C. Tensile
strength drops by about 200 MPa with increasing holding time and
remains the same after about 200 s in the overaging zone. Yield
strength first decreases slightly then increases again and stabilizes
after about 300 s of overaging. Fig. 10b shows the uniform and total
elongation as a function of holding time. Apart from small deviations
for the Nb alloys the two elongation measures increase with
increasing holding time with a logarithmic-type behavior. The Nb
steels exhibit outstanding improvements in both uniform and total
elongation compared to the reference material. However, the
difference in uniform and total elongation between the different
Nb variants is nearly negligible.
Coarse NbC particles
95Nb 25Nb 45Nb 90Nb
6.7 7 3.0 827 18 737 52 897 51
827 28 0.107 0.06 0.217 0.10 0.417 0.18
Fig. 11 shows the true stress–logarithmic strain ðst –φl Þ flow
curves, the work-hardening rate θ, and the differential n-value n′
as a function of logarithmic strain of the alloys that were
isothermally held at 400 1C for 600 s. The flow curve of the
Nb-free reference material is steeper and its work-hardening rate
and differential n-value are distinctly higher than those of the Nb
containing variants especially up to around 2% of logarithmic
strain. This results in higher elongations via elevated strain hard-
ening with increasing strain.
Mechanical properties and the amount of retained austenite of
the grade 25Nb as a function of overaging temperature are shown
in Fig. 12. Both yield and tensile strength decrease and elongations
increase accordingly with overaging temperature. The relation
between mechanical properties and overaging temperature can
be divided into three stages, namely into rather flat plateaus at
temperatures below martensite start temperature as well as above
450 1C and a linear range in between the plateaus. The amount of
retained austenite increases with overaging temperature,
decreases remarkably with overaging time at the highest overa-
ging temperature of 475 1C and reaches its highest values after
120 s of overaging at 450 1C.
Hole expansion strain as a function of overaging temperature is
shown in Fig. 13. The hole expansion strain decreases with
increasing holding temperature and the addition of Nb barely
affects the hole expansion strain.
4. Discussion
The two populations of NbC particles that have been found in
the Nb alloyed grades (Table 3) indicate two distinct formation
situations. The ThermoCalc based thermodynamic calculation
(Fig. 14) reveals that NbC particles are not completely dissolved
during reheating at 1180 1C in the grades 45Nb and 90Nb. There-
fore it can be concluded that the population of large particles in
these grades results from precipitates formed during casting
which undergo an additional Ostwald ripening during reheating
and further processing. This seems to be in contradiction to the
 K. Hausmann et al. / Materials Science & Engineering A 588 (2013) 142–150
Fig. 8. Transformation behavior for steel grades 0Nb, 25Nb, 45Nb and 90Nb: (a) transformed phase fraction of continuously cooled samples (50 K/s), (b) normalized length of
dilatometer samples during overaging at an overaging temperature of 400 1C.
Fig. 9. Amount of retained austenite for alloys 0Nb, 25Nb, 45Nb, 90Nb held at T oa ¼ 400 1C (a) as a function of overaging time and (b) as a function of tensile strain
ðt oa ¼ 600 sÞ.
Table 4
Carbon content C γ of retained austenite determined by XRD measurements based
on lattice constants according to Dyson and Holmes [24] for all TBF heat treated
samples (T oa ¼ 400 1C and t oa ¼ 600 s).
Steel 0Nb 25Nb 55Nb 95Nb
C γ [mass-%] 0.98 0.98 0.98 0.98
grade 25Nb for which a complete dissolution of NbC particles is
predicted. However, it is well known that during casting segrega-
tion takes place and conventional thermomechanical processing
does not reduce this segregation.
To prove segregation as a potential cause for the population of
large precipitates in the grade 25Nb, Scheil–Gulliver calculations
were carried out using the Scheil module of ThermoCalc. The mass
fraction of Nb in the liquid and solid phase as a function of the
mass fraction of solid is shown in Fig. 15. The Nb content in the
liquid and the solid phase grows exponentially with the mass
fraction of solid, and the liquid phase holds more than four times
as much Nb than the solid phase throughout solidification. Thus,
Nb strongly segregates with a tendency to remain in the liquid
phase. As segregation is not reduced significantly during reheating
it must be expected, that in the inter-dendritic regions with a high
Nb content even in the grade 25Nb NbC is not dissolved during
reheating.
The fine particles which are observed in all grades are a result
of precipitation during hot rolling and the slow cooling from the
coiling temperature. The almost unchanged fraction of precipitates
(Fig. 7) during the annealing of the cold rolled material is in
147
agreement with an expected minor Ostwald ripening due to the
low Nb content in solid solution and the low diffusivity of Nb at
the low annealing temperature and short time interval.
Niobium generally refines the overall microstructure (Table 2).
There is no significant further grain refinement for the steel grades
containing more than 0.025 mass-% Nb. As can be concluded from
Table 3, the addition of more than 0.025 mass-% Nb does not result
in the formation of a larger amount of finer precipitates, which
would contribute to a further grain refinement and possible
precipitation strengthening. Instead, a further increase in Nb
content leads to higher amounts of large precipitates, which does
not exert changes in microstructure.
As a result of grain refinement through Nb more nucleation
sites, preferably triple points of primary austenite grains, are
available that lead to the accelerated pro-eutectoid ferrite and
upper bainite formation of the Nb grades as opposed to the
reference material (Fig. 8a). This effect has been reported pre-
viously for microalloyed DP and conventional TRIP steels by
Pichler et al. [19]. A quite similar transformation behavior of Nb
variants during cooling (Fig. 8a) and isothermal holding (Fig. 8b) is
most likely related to their similar prior austenite grain size as
opposed to the Nb-free reference material.
Furthermore, the final bainitic matrix mainly comprises glob-
ular bainite as opposed to the lath-like bainite of the reference
material. A similar observation for an addition of 0.02–0.05 mass-%
Nb to a 0.2% C–1.5% Si–1.5% Mn TRIP-aided bainitic steel was
reported by Sugimoto et al. [9]. One possible explanation for the
observed change in bainite morphology due to Nb addition from
lath-like to globular bainite can be attributed to the pre-isothermal
transformation products. Formation of ferrite and upper bainite
upon cooling to IBT can cause differences in carbon distribution
148 K. Hausmann et al. / Materials Science & Engineering A 588 (2013) 142–150

Fig. 10. (a) Yield strength Rp0:2 and tensile strength Rm (b) uniform elongation Au and total elongation A25 as a function of overaging time at T oa ¼ 400 1C for steel grades 0Nb,
25Nb, 45Nb and 90Nb.

Fig. 11. Flow curves (st vs. φl ), work-hardening rate θ and differential n-value as a
function of logarithmic strain φl for all steel grades annealed at T oa ¼ 400 1C for
t oa ¼ 600 s.

within the remaining austenite grains. This locally increased

carbon content may influence both the bainite formation and
morphology during the IBT. To clarify the validity of this explana- Fig. 12. Tensile strength Rm , yield strength Rp0:2 , yield ratio Rp0:2 =Rm , total
tion, counterpart experiments with the reference material without elongation A25, uniform elongation Au , and the amount of retained austenite as a
function of overaging temperature T oa for the grade 25Nb.
ferrite and the Nb alloyed material with pro-eutectoid ferrite were
conducted. For this purpose, the reference material was cooled to
overaging temperature at a cooling rate of 30 K/s forcing the
formation of ferrite and the Nb alloyed grade was quenched to
overaging temperature at a cooling rate of 80 K/s preventing
ferrite formation. The bainite and retained austenite morphologies
are the same, regardless of ferrite formation. Therefore, the change
in bainite and retained austenite morphology is a consequence of
grain refinement, NbC precipitation or Nb in solid solution. In a
work reported by Bleck et al. [14], it is argued that NbC preferably
precipitates at the austenite grain boundaries influencing the
nucleation kinetics of bainite formation. In turn, bainite morpho-
logy can be affected by the change in nucleation kinetics.
The influence of Nb addition on bainite formation is accom-
panied by a markedly reduced cementite formation. This in turn
results in a remarkably increased retained austenite fraction
(Fig. 9). The exact reason for these morphology changes and the
decrease of the amount of precipitated cementite triggered by Nb
addition remains unclear at present and requires further Fig. 13. Hole expansion strain λ as a function of overaging temperature after
investigation. t oa ¼ 600 s for all investigated steel grades.
 K. Hausmann et al. / Materials Science & Engineering A 588 (2013) 142–150
Fig. 14. Calculated amount of NbC in thermodynamic equilibrium as a function of
temperature for the grades 25Nb, 45Nb and 90Nb predicted by ThermoCalc,
T rh : reheating temperature prior to hot rolling.
Fig. 15. Nb in the liquid and solid phase as a function of mass fraction of solid of the
grade 25 Nb according to the Scheil module of ThermoCalc allowing interstitial
back-diffusion, i.e. interstitial atoms are allowed to redistribute in the solid phase
according to thermodynamic equilibrium.
The tensile strength of multiphase steel grades can be esti-
mated applying the rule of mixture
Rm ¼ ∑ f vi si ; ð2Þ
i
where f vi is the volume fraction and si is the strength of the
respective phase i. Based on this relationship the decreasing
tensile strength with increasing overaging time (Fig. 10) can be
explained by the increasing fraction of bainite and the decreasing
amount of martensite formed during final cooling to room
temperature. Furthermore, the almost constant values for the
tensile strength for overaging times larger than 200 s are in
excellent agreement with the measurements (Fig. 8) which show
that the bainite formation saturates. The same argument holds
true for the decreasing yield strength at short overaging times. For
longer overaging times a distinctive increase of the yield strength
is observed. This behavior is typical for conventional TRIP steel
grades [27] and can be explained as follows: in particular for Dual-
Phase steel grades with hard martensite as an inclusion in a soft
ferritic matrix a low yield ratio as a result of high local stress at
ferrite/martensite phase boundaries is well known. For the mate-
rial in the present investigation short overaging times result in a
considerable amount of martensite formed during final cooling
and therefore the observation of low yield stress is reasonable.
Increasing overaging time increases the stability of the austenite
and decreases the amount of martensite formed during final
149
cooling. This in turn decreases the impact of the local stresses
and therefore an increase of the yield strength is observed.
The addition of Nb and the subsequent NbC precipitation are
well known for enhancing the tensile strength due to precipitation
strengthening and grain refinement [14–19]. This is in apparent
contradiction to the present results which clearly show a decrease
of strength due to the addition of Nb. For the present material an
increase of the strength due to precipitation hardening and a
lower grain size is expected, too. However, the replacement of
harder fine lath-like bainite by softer pro-eutectoid ferrite/upper
bainite and the more globular bainitic matrix as a consequence of
the Nb addition results in a decrease of strength.
Prolonged overaging times lead to an increase of the bainite
fraction and therefore to enhanced carbon partitioning and aus-
tenite stabilization (Fig. 9a). However, in particular at tempera-
tures of 450 1C and higher, carbon intended for partitioning begins
to precipitate after certain overaging times resulting in a strong
decrease of the amount of retained austenite. In this case time and
temperature are interchangeable resulting in accelerated parti-
tioning and precipitation at higher temperatures (Fig. 12). The
increase in uniform and total elongation with prolonged overaging
times (Fig. 10b) can likewise be attributed to the stabilization of
retained austenite due to carbon enrichment as the bainitic
transformation proceeds. The reduced strain induced martensite
formation at low strain levels results equivalently to conventional
TRIP steels in an increasing work hardening at high strain levels
(Fig. 11) and thereby in increasing elongation values (Fig. 10b).
Comparing the different grades investigated, the elongation of
the Nb-TBF steels is significantly improved compared to the
reference material as a result of a higher amount of retained
austenite with the same stability behavior (Fig. 9). This enables
more sources available for the overall TRIP-effect in the case of Nb
microalloyed steels. In addition, the soft phase transformation
product from cooling to overaging most likely contributes to
enhanced elongations. The similarity of the retained austenite
stability behavior indicated by the almost parallel graphs is in
good agreement with the XRD measurements revealing approxi-
mately identical lattice constants and thus carbon content of the
retained austenite of the four Nb containing grades (Table 4).
As the overaging temperature decreases, strength increases and
elongations decrease (Fig. 12) as expected due to lath thickness
decrease and microstructure change from a globular to a lath-like
bainite or even tempered martensite.
The yield ratio shown in Fig. 12 reveals two distinct regions
with low values above 450 1C and high values below 425 1C.
Disregarding their large scatter, the hole expansion strains
decrease more or less linearly with overaging temperature as
shown in Fig. 13. It is reasonable to study the relationship between
yield ratio and hole expansion strain multiplied by tensile strength
as given in Fig. 16 for the different overaging temperatures. In
general, the product of tensile strength and hole expansion strain
increases almost linearly with increasing yield ratio as well as with
decreasing overaging temperature within a deviation range of
about 5000 MPa%. However, the data density is high for the lower
and the upper ends of the yield ratio range, suggesting stagnation
of the yield ratio once the range of about 0.6–0.8 is exceeded to
either side. Considering overaging temperatures of 400 1C and
below the yield ratio is in the range of 0.8–0.85, whereas an
improvement in hole expansion strains can be achieved with
lower overaging temperatures.
Finally, the hole expansion strains of the Nb variants are at the
same level as those of the reference material (Fig. 13). The fact that
the edge formability is unaffected by the impressive influence of
Nb on mechanical properties is a key finding of the present work
and provides valuable information for further development of high
strength high ductility sheet steels.
150 K. Hausmann et al. / Materials Science & Engineering A 588 (2013) 142–150
Fig. 16. Tensile strength Rm times hole expansion strain λ as a function of the yield
ratio for all investigated grades; overaging temperatures range from 350 1C to
475 1C and overaging time is set to 600 s.
5. Conclusions
Two populations of NbC particles, coarse and fine precipitates,
were found in all Nb containing alloys. The size of both coarse and
fine NbC precipitates was consistent throughout the Nb variants,
whereas the density of coarse NbC particles increases with
increasing Nb content. While no further grain refinement occurs
for Nb contents above 0.025 mass-%, grain refinement by
0.025 mass-% in comparison to the Nb-free reference material is
very pronounced. Since the grain size of all Nb containing variants
is similar and the coarse NbC particles do not affect mechanical
properties, the final microstructure of the Nb variants and their
mechanical properties are quite similar as opposed to the refer-
ence material. Thus, the addition of 0.025 mass-% Nb to the
composition is sufficient to exploit its advantages with respect to
mechanical properties.
Grain refinement through Nb addition leads to a promotion of
transformation during cooling from austenitization to overaging
temperature which causes around 20% transformed phase fraction
prior to the overaging step. The Nb modified microstructure
containing ferrite and large amounts of granular bainite leads to
a significant drop in tensile strength. Moreover, the morphology of
bainite and hence the morphology of retained austenite are
strongly influenced by Nb addition. The lath-type bainite of the
Nb-free steel grade changes to globular bainite due to Nb addition.
This also alters the morphology of retained austenite morphology
from lath to blocky-like. Despite these massive changes in micro-
structure, the hole expansion strains are nearly unaffected by Nb
addition. The strongly reduced amount of cementite that is found
in the bainite of the Nb variants results in more carbon available
for the stabilization of retained austenite. This leads to higher
amounts of retained austenite with the same carbon content in the
Nb-bearing alloys compared to the reference material resulting in
significantly improved uniform and total elongations.
Therefore, adding Nb is beneficial for the production of sheet
steel with an excellent combination of tensile strength above
980 MPa, total elongation and low edge crack susceptibility.
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