Journal of Materials Processing Technology 177 (2006) 390–395

Formability of Nb bearing ultra high-strength TRIP-aided sheet steels

Koh-Ichi Sugimoto a,∗ , Toshiki Muramatsu b , Shun-Ichi Hashimoto c , Yoichi Mukai d
aDepartment of Mechanical Systems Engineering, Shinshu University, 4-17-1, Wakasato, Nagano 380-8553, Japan
b Shinshu University, 4-17-1, Wakasato, Nagano 380-8553, Japan
c Ferrous Department, CBMM Asia Co., Ltd., Akasaka Nakanishi Bldg. Bekkan 1F, 4-1-4, Akasaka, Minato-ku, Tokyo 107-0052, Japan
d Research & Development Labs., Kobe Steel Ltd., 2222-1, Ikeda, Onoe-cho, Kakogawa, Hyogo 675-0023, Japan

Abstract
Microstructure, tensile property and formability of formable ultra high-strength 0.2% C–1.5% Si–1.5% Mn–0.02–0.11% Nb TRIP-aided sheet
steels with bainitic ferrite matrix (TBF steels) were investigated for automotive applications such as impact member reinforcements, seat frames etc.
Nb addition of 0.08% achieved the best combination of total elongation and stretch-flangeability, accompanied with an increase in peak austempering
temperature for total elongation. The excellent total elongation and stretch-flangeability were primarily associated with microstructure of the matrix,
retained austenite characteristics, morphology of matrix and retained austenite, etc. It was expected that hot-dip galvanizing just after continuous
annealing can be realized in the 0.08% Nb TBF steels.
© 2006 Elsevier B.V. All rights reserved.

Keywords: Ultra high-strength steel; TRIP-aided steel; Retained austenite; Banitic ferrite; Morphology; Cold formability; Stretch-flangeability; Niobium; Microal-
loying

1. Introduction attained by complex additions of niobium and molybdenum

In order to attain a drastic weight reduction and crash worthi-
ness performance of vehicles, formable ultra high-strength steels
with tensile strength of 980–1470 MPa are required for automo-
tive applications such as center pillar reinforcement, seat frame
and so on. The transformation-induced plasticity (TRIP) [1] of
retained austenite is very useful for improving the formability
of these steels. In addition, bainitic ferrite lath structure is favor-
able for improving the stretch-flangeability of ultra high-strength
steel because it has uniform fine structure without microscopic
stress concentration sites. On the basis of such an idea, a new type
of 980–1470 MPa grade 0.2% C–1.5% Si–1.5% Mn TRIP-aided
steel with bainitic ferrite lath structure matrix or TRIP-aided
bainitic ferrite steels (TBF steels) was developed [2].
According to a previous study on a conventional type of
C–Si–Mn TRIP-aided steel with polygonal ferrite matrix, nio-
bium addition increased tensile strength due to grain refining
[3–5] and fine precipitates [5–7]. In addition, it improved the
strength – elongation balance (a product of tensile strength and
total elongation) due to increased volume fraction of retained
austenite [4,6,8,9]. Further strengthening of the steel was also
∗ Corresponding author.
E-mail address: sugimot@gipwc.shinshu-u.ac.jp (K.-i. Sugimoto).
primarily due to fine NbMoC precipitation [10]. However, no
research is reported about effects of niobium addition on some
properties of the TBF steel. So, in this study the effects of
niobium content on the microstructure, tensile property and
formability of 0.2% C–1.5% Si–1.5% Mn TBF steels are
examined.
2. Experimental procedure
In this study, five steels with different niobium content were prepared as
air-melted 50 kg ingots, followed by hot forging to produce 30 mm thick slabs.
Chemical compositions of these steels are shown in Table 1, in which martensite
start temperature (MS ) was calculated using the experimental relation in [11].
The slabs were reheated to 1200 ◦ C and hot-rolled to a thickness of 3.2 mm,
finishing at 850 ◦ C and then coiled at 600 ◦ C, as shown in Fig. 1. After cold
rolling to a thickness of 1.2 mm, the sheets were first annealed at 900 ◦ C and
then austempered at TA = 300–525 ◦ C for tA = 200 s in salt baths.
Volume fraction of retained austenite was quantified from integrated intensity
of (2 0 0)␣ , (2 1 1)␣ , (2 0 0)␥ , (2 2 0)␥ and (3 1 1)␥ peaks of Mo-K␣ radiation [12].
The carbon concentration (C␥ , mass%) was estimated by substituting the lattice
constant (a␥ , 10−1 nm) measured from (2 0 0)␥ , (2 2 0)␥ and (3 1 1)␥ peaks of
Cu-K␣ radiation into the equation proposed by Dyson and Holmes [13].
Tensile tests were carried out on a hard type of testing machine at 20 ◦ C,
using JIS-13B specimens of gage length of 50 mm, gage width of 12.5 mm and
thickness of 1.2 mm. Hole-expanding tests were conducted using disk specimens
of 50 mm diameter. First, a hole of 4.76 mm diameter was punched on the disk
specimen using a graphite type of lubricant, at a cross head speed of 10 mm/min,
at a clearance of 10% and at 20 ◦ C. Subsequently, hole-expanding tests were

0924-0136/$ – see front matter © 2006 Elsevier B.V. All rights reserved.
doi:10.1016/j.jmatprotec.2006.03.186
 K.-I. Sugimoto et al. / Journal of Materials Processing Technology 177 (2006) 390–395 391

Table 1
Chemical composition (mass%) and estimated martensite-start temperature (Ms , ◦ C) of steels used.
Steel C Si Mn P S Al Nb N MS

0 Nb 0.20 1.50 1.50 <0.02 0.005 0.040 – 0.0060 421

2 Nb 0.20 1.50 1.50 <0.02 0.005 0.040 0.020 0.0060 421
5 Nb 0.20 1.54 1.52 0.005 0.002 0.030 0.048 0.0074 420
8 Nb 0.20 1.48 1.51 0.005 0.003 0.024 0.078 0.0068 420
11 Nb 0.20 1.48 1.44 0.004 0.003 0.040 0.109 0.0113 423

where d0 and df are initial hole diameter (4.76 mm) and hole diameter on crack-
ing, respectively.

3. Results and discussion

3.1. Microstructure and retained austenite characteristics

Fig. 2 shows typical scanning electron micrographs of 0

Nb and 5 Nb steels. When 0 Nb steel is austempered at tem-
peratures far below MS after annealing, martensite structure
coexists with bainitic ferrite in the matrix (Fig. 2a). However,
when austempered at temperatures above MS , the microstructure
Fig. 1. Schematic diagram of hot and cold rolling process of 0 Nb–11 Nb steels, mainly consists of bainitic ferrite matrix and interlath retained
in which “AC” and “OQ” represent air cooling and quenching in oil, respectively. austenite films (Fig. 2c). The similar microstructure is obtained
even when the sample are austempered at temperatures a little
carried out at a punch rate of 1 mm/min and at 20 ◦ C, using a flat punch of 1 mm lower than MS (Fig. 2b).
radius. The hole-expanding ratio (λ) was determined by the following equation. Niobium addition of more than 0.05 mass% refines the prior

(d − d ) 
λ=
f 0
× 100% (1)
austenite grain size and the resultant retained austenite film size,
d0 as shown in Fig. 2d. However, the amount of pro-eutectoid fer-

Fig. 2. Typical scanning electron micrographs of 0 Nb and 8 Nb steels austempered at TA = 325 ◦ C, 400 ◦ C or 475 ◦ C. Arrows in (d) represent pro-eutectoid ferrite.
392 K.-I. Sugimoto et al. / Journal of Materials Processing Technology 177 (2006) 390–395

Fig. 3. Variations in (a) volume fraction (f␥0 ) and (b) carbon concentration (C␥0 ) of retained austenite as a function of austempering temperature (TA ) in 0 Nb–11
Nb steels.

rite along prior austenite grain boundary (see arrows in Fig. 2d,
hereafter call soft phase) increases. It is noteworthy that matrix
structure changes from lath structure to granular structure, and
consequently retained austenite morphology tends to change
from plate like to blocky (Fig. 2e,f), when 5 Nb–11 Nb steels are
austempered at temeperatures higher than 400 ◦ C. Any cemen-
tites did not appear in these steels, in contrast to conventional
TRIP-aided steel with polygonal ferrite matrix.
Fig. 3 shows the variations in volume fraction (f␥0 ) and car-
bon concentration (C␥0 ) of retained austenite as a function of
austempering temperature (TA ) for 0 Nb–11 Nb steels. Niobium
addition of 0.02–0.11 mass% decreases carbon concentration of
the retained austenite, except at high austempering temperatures.
On the other hand niobium addition of 0.05–0.08 mass% brings
on a little increase in volume fraction of retained austenite at
low austempering temperatures, although its volume fraction
decreases at high austempering temperatures.
According to Drewes and Walker [5], niobium plays the fol-
lowing roles in conventional TRIP-aided steels.
(2) In precipitated form as carbides, nitrides or carbonitrides,
niobium has a grain refining effect, increasing the ten-
sile strength. Further more, niobium suppresses undesired
pearlite formation in the TRIP-aided steels.
So, it is expected that high retained austenite volume fraction
at low austempering temperatures of the present 5 Nb and 8 Nb
steels may be caused by the niobium in dissolved form which
suppresses cementite precipitation in the temperature range of
bainite formation. Also, soft phase seen in Fig. 2d may assist
such a high volume fraction. When austemperd at high tem-
peratures of 400–500 ◦ C, niobium addition of 0.05–0.11 mass%
changed morphology of matrix structure and retained austen-
ite (Fig. 2e,f). These morphology changes, due to niobium in
solid solute as ferrite former element, may suppress a decrease
in carbon concentration of retained austenite. On the other hand,
refinement of retained austenite phase and matrix through prior
austenite grain refining is considered to be caused by niobium
in precipitated form as NbC.

(1) Niobium in solid solution lowers the martensite start temper-
ature. Furthermore, in dissolved form it suppresses carbide
precipitation in the temperature range of bainite formation,
with consequent increase in the residual austenite content
and its carbon content.
3.2. Strength
Fig. 4 shows variations in yield stress or 0.2% offset proof
stress (YS) and tensile strength (TS) with austempering tem-
perature (TA ). Niobium addition of 0.05–0.11 mass% increases

Fig. 4. Variations in (a) yield stress (YS) and (b) tensile strength (TS) as a function of austempering temperature (TA ) in 0 Nb–11 Nb TBF steels.
 K.-I. Sugimoto et al. / Journal of Materials Processing Technology 177 (2006) 390–395
Fig. 5. The amount of NbC precipitates of 0.2% C–1.5% Si–1.5% Mn–Nb sys-
tems computed by Thermo-Calc.
yield stress of the steels with appearance of yield point, except
at low austempering temperatures of 300–350 ◦ C. An increment
of the yield stress is about 50 MPa. On the other hand, the ten-
sile strength is not influenced by niobium addition, although a
decrease in tensile strength appears at low austempering tem-
peratures in the same way as yield stress. Yield ratios (YS/TS)
of 2 Nb–11 Nb steels are between 0.70 and 0.85 and increases
with austempering temperature. These yield ratios are higher
than that of 0 Nb steel.
According to Hashimoto et al. [10], niobium addition of
0.02–0.05 mass% to 0.2% C–1.5% Si–1.5% Mn TRIP-aided
Fig. 6. Variations in (a) total elongation (TEl) and (b) hole-expanding ratio (λ) as a function of austempering temperature (TA ) in 0 Nb–11 Nb steels.
Fig. 7. Nb content dependence of (a) strength - elongation balance (TS×TEl) and (b) strength – stretch-flangeability balance (TS×λ) of 0 Nb–11 Nb steels.
393
steel with polygonal ferrite matrix increases tensile strength
by 50–100 MPa due to fine NbC precipitates. In the present
2 Nb–11 Nb steels, volume fraction of NbC precipitates con-
siderably increases with niobium content, as shown in Fig. 5.
However, a large amount of pro-eutectoid ferrite was observed
in these steels (Fig. 2d). So, it is supposed that this soft phase sets
off both precipitation strengthening of NbC and microstructure
refining strengthening.
Increasing niobium content increased yield point elongation
of steels. Such a remarkable yield point behavior may contribute
to increase in yield stress at high austempering temperatures,
despite setoff of precipitation hardening and softening by pro-
eutectoid ferrite.
3.3. Ductility and formability
Fig. 6 shows austempering temperature dependences of total
elongation (TEl) and hole-expanding ratio (λ) of 0 Nb–11
Nb steels. Fig. 7 shows niobium content dependences of
strength – elongation balance (TS×TEl) and strength – stretch-
flangeability balance (TS×λ) of these steels. It is found that
niobium addition of 0.05–0.08 mass% increases total elonga-
tion of the steels at austempering temperatures higher than
TA = 450 ◦ C, corresponding to hot-dip galvanizing (GI) temper-
ature. On the other hand, hole-expanding ratio is enhanced by
niobium addition of 0.08–0.11 mass%. It is very important that a
large hole-expanding ratio is achieved in a tensile strength range
of 1000–1400 MPa (at TA = 300–350 ◦ C).
394 K.-I. Sugimoto et al. / Journal of Materials Processing Technology 177 (2006) 390–395
In generally, total elongation of TRIP-aided steel is prin-
cipally controlled by retained austenite characteristics and a
difference in strength between matrix and second phase [14].
As shown in Fig. 3, retained austenite characteristics were not
improved by niobium addition. On the other hand, niobium addi-
tion changed the matrix structure from bainitic ferrite lath struc-
ture to granular beinitic ferrite and resultantly retained austenite
phase from plate like type to blocky type when austempered at
temperatures higher than 400 ◦ C. According to Sugimoto et al.
[15,16], a combination of polygonal ferrite matrix and blocky
second phase, similar to conventional TRIP-aided steel, tends to
considerably raise a long range internal stress. Also, this internal
stress enhances total elongation by increasing strain-hardening
rate. So, the large total elongations of 5 Nb and 8 Nb steels
austempered at TA = 450–500 ◦ C are considered to be owing to
morphology change of matrix and retained austenite phase.
Figs. 6 and 7 showed that stretch-flangeabilities of the steels
were enhanced by niobium addition of 0.08–0.11%, especially
at low austempering temperatures. According to our previous
study [17], the stretch-flangeability of the TRIP-aided steels
is principally controlled by (i) metallurgical factors such as
matrix structure and retained austenite characteristics and (ii)
hole-surface damage on hole-punching such as voids at the
matrix/second phase interface.
It was found from measurement of the hole-surface damage
that the shear section length of 8 Nb steel increases in the same
way as 2 Nb–5 Nb steels when austempered at 300–325 ◦ C,
which means a low damage at break section. From SEM obser-
vation of the shear and break sections, void formation and its
linkage were suppressed in these steels. From Figs. 2 and 3,
microstructure of 8 Nb steel austempered at 300–350 ◦ C was
characterized by a large amount of retained austenite, fine prior
austenite grain size (fine lath structure and retained austenite
films) and much pro-eutectoid ferrite. So, it is considered that
high strength – stretch-flangeability balance of the 8 Nb–11 Nb
steels is principally associated with these microstructural prop-
erties. Even when austempered at 450–500 ◦ C, the 8 Nb and
11 Nb steels exhibited high strength – stretch-flangeability bal-
ance, although bainitic ferrite lath structure changed to granular
bainitic ferrite phase. As the retained austenite characteristics
were not improved by niobium addition, this improvement may
be caused by refinement of microstructure by niobium addition.
4. Conclusions
(1) Niobium addition of 0.05–0.8 mass% decreased carbon con-
centration of retained austenite (except at high austempering
temperatures) and brought on a little increase in its volume
fraction at low austempering temperatures.
(2) Niobium additions of 0.05–0.11 mass% increased non
martensite structure at low austempering temperatures. Also
they changed matrix structure and retained austenite mor-
phology when austempered at 400–500 ◦ C. It was expected
that NbC precipitates refined prior austenite grain size, and
niobium in solid solution promoted granular bainitic ferrite.
(3) Yield stresses of 5 Nb–11 Nb steels increased by about
50 MPa, when austempered at temperatures higher than
400 ◦ C. However, tensile strength was not influenced by
niobium addition.
(4) Total elongation was improved by niobium additions of
0.05–0.08 mass% when austempered at 450–500 ◦ C, equiv-
alent to hot-dip galvanizing temperature. It is considered
that the large elongation is caused by (i) a high long range
internal stress in matrix due to morphology change of matrix
and second phase and (ii) relatively high volume fraction and
stability of retained austenite.
(5) Stretch-flangeability was significantly improved by niobium
addition of 0.08–0.11 mass%, especially when austempered
at low temperatures of 300–350 ◦ C. It was considered that
this is associated with refined microstructure and an increase
in pro-eutectoid ferrite volume fraction.
Acknowledgements
The authors gratefully acknowledge financial support by
grants from The Iron and Steel Institute of Japan (2004). A part
of this study was supported by the Grant-in-Aid for Scientific
Research (C), The Ministry of Education, Science, Sports and
Culture, Japan (No.2004-15560624).
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