Materials Science and Engineering A 528 (2011) 8299–8304

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Materials Science and Engineering A

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

Relation of ductile-to-brittle transition temperature to phosphorus grain

boundary segregation for a Ti-stabilized interstitial free steel
X.-M. Chen a , S.-H. Song a,∗ , L.-Q. Weng a , S.-J. Liu a , K. Wang b
a
Materials Science and Engineering, Shenzhen Graduate School, Harbin Institute of Technology, Xili, Shenzhen 518055, China
b
Department of Superalloys, Central Iron and Steel Institute, Bejing 100081, China

a r t i c l e i n f o a b s t r a c t

Article history: Equilibrium grain boundary segregation of phosphorus in a Ti-stabilized interstitial free (IF) steel is mea-
Received 17 July 2011 sured using Auger electron spectroscopy (AES) after the specimens are aged for adequate time at different
Received in revised form 1 August 2011 temperatures between 600 and 850 ◦ C. Based on the experimental data of equilibrium grain boundary
Accepted 1 August 2011
segregation along with the McLean equilibrium segregation theory, the free energy of segregation of
Available online 6 August 2011
phosphorus is evaluated to be ∼44.8 kJ/mol, being independent of temperature. With the AES results
being combined with the ductile-to-brittle transition temperatures (DBTTs) determined by impact tests,
Keywords:
a relationship between DBTT and phosphorus boundary concentration is established. Predictions with
Interstitial free steel
Grain boundary
the relationship indicate that cold work embrittlement may be severe if the steel is annealed at relatively
Segregation low temperatures after cold rolling.
DBTT © 2011 Elsevier B.V. All rights reserved.

1. Introduction the formation of {1 1 1} recrystallization texture, and therefore

As the automotive industry develops, high demands are placed
on the steel with high deep drawability, strength and surface qual-
ity. High strength interstitial free (IF) steel is one of the most widely
used steels in the automotive industry. It is well known that the low
carbon and nitrogen in IF steel, typically being less than 0.003 wt.%C
and 0.004 wt.%N, result in a high level of deep drawability [1], which
is extremely important in car skin applications. Elimination of these
solutes is achieved through careful control of the melt chemistry
during steel making and by the hyper-stoichiometric addition of
titanium and/or niobium to remove interstitial atoms from solid
solution through the formation of carbide, nitride and carbosul-
phide or carbonitride [1–4]. The application of IF steel without
addition of strengthening elements is limited for its low strength.
The most common solid solution strengthening elements added
in IF steel are P, Mn and Si, and P has the highest strengthen-
ing effect. Among these three strengthening elements, Mn and
Si may result in a considerable decrease in the steel formability,
while P may strengthen the steel without causing a considerable
loss of deep drawability [1,5–7]. However, P may precipitate as
FeTiP during batch annealing between 600 ◦ C and 850 ◦ C as long
as the process allows sufficient time for FeTiP precipitation [8,9].
The precipitation of FeTiP would reduce the concentration of P
in the matrix and lead to the deterioration of strength [7]. It is
demonstrated that the precipitation of FeTiP is deleterious for
causes deep drawability losses of IF steels [7,9,10]. With the help
of solubility product data of the precipitation in Ti-stabilized IF
steel, it is suggested that the equilibrium precipitation sequence
is TiN > TiS > Ti4 C2 S2 > TiC ∼ FeTiP [10,11]. Thus, the addition of Ti is
mainly used to stabilize N, S and C, and the precipitation of FeTiP
could be limited.
Also, the addition of Si would cause surface oxidation, and
then reduce the surface quality of IF steel and deteriorate coating
adhesion [2,12]. Therefore, P is a preferred strengthening element
in IF steels. However, the addition of phosphorus could cause
its grain boundary segregation which would shift the ductile to
ductile-to-brittle transition temperature (DBTT) to higher temper-
atures, leading to cold work embrittlement [13,14]. Particularly, the
embrittlement is more susceptible in IF steels since there is no grain
boundary segregation of carbon and nitrogen atoms, which could
increase the grain boundary cohesion [1,15].
In the present work, a relationship between DBTT and phos-
phorus grain boundary segregation for a Ti-stabilized IF steel
was established experimentally using Auger electron spectroscopy
(AES) in conjunction with impact tests. Based on this relationship,
predictions of DBTT as a function of aging temperature and phos-
phorus concentration in the matrix were made through predicting
the grain boundary concentration of phosphorus.
2. Experimental procedure

A Ti-stabilized IF steel doped with P was prepared by vacuum

∗ Corresponding author. Tel.: +86 755 26033465; fax: +86 755 26033504. induction melting. The chemical composition of the steel is listed
E-mail addresses: shsong@hitsz.edu.cn, shsonguk@yahoo.cn (S.-H. Song). in Table 1. The resulting ingot (50 kg) was hot rolled in the range

0921-5093/$ – see front matter © 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.msea.2011.08.002
8300 X.-M. Chen et al. / Materials Science and Engineering A 528 (2011) 8299–8304

Table 1
Chemical composition of the experimental steel.

C N Si Mn S Ti P

wt.% 0.0018 0.0020 0.058 0.32 0.011 0.066 0.037

at.% 0.0084 0.0080 0.12 0.32 0.019 0.077 0.067

910–1120 ◦ C into a plate 3 mm in thickness. A differential scanning

calorimetry (DSC) curve of the experimental steel is represented
in Fig. 1. As seen, the austenite/ferrite transition temperature is
∼920 ◦ C in the heating process and ∼897 ◦ C in the cooling pro-
cess at a rate of 1 K/min. Hence, in the present work all samples
were initially austenitized at 940 ◦ C for 15 min, then furnace cooled
to 850 ◦ C and held there for 30 min to obtain a uniform ferrite
microstructure. Finally, the samples were furnace cooled to differ-
ent temperatures and held there for adequate time (600 ◦ C for 25 h,
650 ◦ C for 120 min, 700 ◦ C for 90 min, 750 ◦ C for 60 min) to enable
grain boundary segregation to reach equilibrium [16], followed by
water quenching to suppress elemental segregation during cool-
ing. Fig. 2 shows the typical optical microstructures of the samples
after heat treated at different temperatures. As seen, there is no
visible difference in microstructure. The microstructure is ferrite
and has an average grain size of approximately 70 ␮m. Also, Fig. 3
shows the HV hardness values of the specimens aged at different
temperatures. Clearly, the hardness is almost the same for differ-
ent specimens, indicating that the precipitation of FeTiP could occur
during aging at different temperatures but it is limited since it is
not strong enough to cause a noticeable change in hardness.
To evaluate the concentration of phosphorus at the grain
boundary, a PHI595 Auger electron spectrometer (AES) was
employed. Rectangular AES specimens with sharp notches
(2.5 mm × 2.5 mm × 31.7 mm in size) were maintained in liquid
nitrogen in the AES chamber for approximately 30 min and then
immediately fractured by impact to obtain intergranular fracture
surfaces for subsequent AES measurements. Twenty grain bound-
aries were measured for each condition and the mean value of
the data points obtained along with the 95% confidence inter-
val was taken as the measured result. Typical parameters for the
Auger measurements were: primary energy = 3 keV, emission volt-
age = 170 V, filament current = 1.45 A, and vacuum = 1 × 10−10 Torr.
The primary beam size was about 0.8 ␮m in diameter. All spectra
were recorded in the differential mode dN(E)/dE. Assuming that the
Auger peak height of an element is proportional to its concentra-
tion, the concentration of an element (atomic fraction), Ci , could be
approximately evaluated by [17,18]
Hi /Si
Ci =  (1)
k
Hk /Sk

2.0
Heating

1.6
DSC/(mW/mg)

Fig. 2. Typical optical microstructures of the samples aged at different temperatures

1.2 ((a) 850 ◦ C; (b) 750 ◦ C and (c) 650 ◦ C).

0.8 where Hi (or Hk ) and Si (or Sk ) denote the Auger peak height and
sensitivity factor of element i (or k), respectively. In the calculation,
Cooling the Fe 703 eV and P 120 eV peaks were considered with their Auger
0.4 sensitivity factors of 0.21 and 0.53, respectively.
880 890 900 910 920 930 940 It is suggested [18] that the use of Eq. (1) is only a rough esti-
o mate of the concentration since the depth distribution is not taken
Temperature ( C)
into consideration. With the assumption that there is not a con-
Fig. 1. DSC curve of the experimental IF steel during continuous heating and cooling centration gradient within the boundary and the concentration of
at a rate of 1 K/min. an element in the matrix is equal to its bulk concentration (Cg ), its
 X.-M. Chen et al. / Materials Science and Engineering A 528 (2011) 8299–8304 8301

100

80
HV hardness

dN(E)/dE
60 Fe
P
40

20

0 Fe
600 650 700 750 850
200 400 600 800
o
Aging temperature ( C) Kinetic Energy (eV)
Fig. 3. HV hardness values of the specimens aged at different temperatures (error
Fig. 5. A typical AES spectrum for the specimen aged at 850 ◦ C.
bars represent the standard deviation).

A typical AES spectrum for the specimen aged for 30 min at

true boundary concentration (CiB ) could be approximately given by
[18–20]
CiB = 2Ci − Cg
The DBTT was measured by means of impact tests at differ-
ent temperatures. The rectangular specimens with a sharp V-notch
(1 mm deep) were used and their dimension is 50 mm long, 2.5 mm
wide and 2.5 mm thick. The specimen was soaked in the ethanol,
which could be cooled to different temperatures by liquid nitrogen
for subsequent impact testing. In the test, the specimen was soaked
for 10 min at each test temperature and then fractured by impact.
An S-4700 scanning electron microscope (SEM) was employed for
the analysis of fracture surfaces, and the DBTT was represented
by the fracture appearance transition temperature (FATT), i.e., the
temperature corresponding to 50% brittle fracture and 50% ductile
fracture. An HV-5 Vickers hardness testing machine with a load
of 9.8 N was chosen to measure the hardness values of different
specimens.
3. Results and discussion
A typical SEM fractograph is shown in Fig. 4 for the speci-
men aged for 30 min at 850 ◦ C and fractured by impact at −196 ◦ C
in the AES chamber. Apparently, the specimen exhibits partially
intergranular fracture. The intergranular facets are quite flat and
smooth, and thus they are suitable for AES grain boundary mea-
surements.
850 ◦ C is shown in Fig. 5. Obviously, there is considerable grain
boundary segregation of phosphorus, while no peaks of other
(2) elements, such as C, N, Si and Mn, are observed. In Ti-bearing inter-
stitial free steels, C and N are stabilized by Ti via forming carbide,
nitride and carbosulphide or carbonitride [1]. As a result, there is no
grain boundary segregation of C and N. Also, the low grain boundary
segregation energies of Mn and Si, 0.08 eV and 0.176 eV, could be
the main reason for no visible segregation of these two elements
[21]. Accordingly, we only deal with phosphorus grain boundary
segregation.
Fig. 6 shows the equilibrium segregation levels of phosphorus
in the specimens aged at different temperatures, determined by
AES analysis and corrected by Eq. (2). Obviously, the equilibrium
segregation levels of phosphorus increases with decreasing tem-
perature. Langmuir–McLean isotherm equation is the well-known
expression describing the temperature dependence of equilibrium
grain boundary segregation, given by [16]
Cg exp(G/RT )
Ceq = (3)
1 + Cg exp(G/RT )
where G is the free energy of segregation of solute, Ceq is the
equilibrium grain boundary concentration of solute at a given tem-
perature (T), R is the gas constant, and Cg is the solute concentration
in the matrix. The concentration of P in the matrix is related to the
precipitation of FeTiP. As described in the introduction, the precip-
itation of FeTiP may occur during annealing, reducing the matrix
concentration of P and in turn leading to a lower strength and
P boundary concentration (at.%)

25

20

15

10

5
600 650 700 750 800 850
o
Temperature ( C)

Fig. 4. A typical SEM fractograph for the specimen aged at 850 ◦ C and fractured by Fig. 6. Equilibrium grain boundary concentrations of phosphorus for the specimens
impact at −196 ◦ C in the AES chamber. aged at different temperatures (error bars represent the 95% confidence interval).
8302 X.-M. Chen et al. / Materials Science and Engineering A 528 (2011) 8299–8304
50
Segregation free energy (kJ/mol)
40
30
20
10
0 600
600 650 700 750
o o
Temperature ( C)
Fig. 7. Free energies of segregation of phosphorus at different temperatures (error
bars represent the 95% confidence interval).
hardness [1,10]. In the present work, there may be some FeTiP com-
pound precipitated during the isothermal holding process, but the
results show no visible changes in hardness for different specimens
(see Fig. 3). Also, as reviewed by Ray et al. [7], the strengthening
increment of the interstitial free high strength steels is derived
mainly from the solid solution hardening of the ferrite matrix by the
addition of P, although the precipitation of FeTiP has been observed
during batch annealing, which leads to impairment of both strength
and deep drawability. Thus, the phosphorus atoms should mainly
remain in solid solution. Consequently, it is assumed for simplicity
that the concentration of P in the matrix is constant and equals its
bulk concentration.
According to the AES measurements shown in Fig. 6 in conjunc-
tion with Eq. (3), one can obtain the free energies of segregation
of phosphorus at different temperatures. The results are plotted
in Fig. 7. As seen, the free energy of segregation of phosphorus
is almost a constant of ∼44.8 kJ/mol in the temperature range of
600–850 ◦ C. Normally, the free energy of segregation is expressed
as
G = H − TS
where H is the segregation enthalpy and S is the segregation
entropy. In terms of the results shown in Fig. 7, the segregation
entropy should be very small, being negligible in the temperature
range considered, and the free energy of segregation of phospho-
rus is equal to the segregation enthalpy, i.e., G = H = 44.8 kJ/mol.
Until now, there have been many experimental studies on the
thermodynamics of phosphorus segregation to ferrite grain bound-
aries [21,22]. It is demonstrated that the free energy of segregation
Fig. 8. SEM fractographs of the specimens aged at 850 ◦ C and fractured at (a) −5 ◦ C and (b) −3 ◦ C.
25
20
15
DBTT ( C)
o
10
5
0
-5
650 700 750 800 850
850
Aging temperautre ( C)
Fig. 9. DBTTs of the specimens aged at different temperatures.
of phosphorus depends on the boundary orientation and the
steel composition, being between 33.5 kJ/mol and 55.5 kJ/mol [21].
Clearly, the present result is well consistent with previous studies.
Phosphorus is a strong embrittling element in ␣-Fe and fer-
ritic steels, and grain boundary segregation of phosphorus has a
considerable effect on the DBTT [14]. In order to establish the rela-
tion of DBTT to phosphorus boundary concentration, The DBTTs
of the specimens aged at different temperatures were evaluated.
After fractured by impact, the fractographs of the specimens aged
at 850 ◦ C are shown in Fig. 8. As seen, the specimen exhibits fully
ductile fracture when it is impacted at −3 ◦ C, while it presents
completely brittle fracture with a mixture of intergranular fracture
and cleavage fracture when it is impacted at −5 ◦ C. Obviously, the
ductile-to-brittle transition of the experimental IF steel occurred in
a very narrow temperature range (−5 ◦ C to −3 ◦ C). With a reason-
able approximation, the DBTT of the 850 ◦ C -aged specimens could
be obtained as a midpoint of this temperature range, i.e., −4 ◦ C.
With the same method, one can obtain all the DBTTs corresponding
to all the aging temperatures. The measured results are plotted in
Fig. 9. Obviously, the DBTT increases with decreasing aging temper-
(4) ature, and when aged at 600 ◦ C the DBTT could be 24 ◦ C. This means
that, at room temperature or below, the cold work embrittlement
could occur at this condition.
Embrittlement of an alloy is classified into hardening embrittle-
ment and non-hardening embrittlement. Hardening embrittlement
is caused by alloy strengthening, such as strain hardening
and precipitation strengthening. And the brittleness of the
alloy increases with increasing strengthening. Nevertheless, non-
hardening embrittlement is mainly caused by grain boundary
segregation of some impurity elements, such as P, Sn, Sb and As
 X.-M. Chen et al. / Materials Science and Engineering A 528 (2011) 8299–8304
25
DBTT=1.60CP-14.14
20 2
R =0.962
15
DBTT ( C)
10
o
5 0.01wt.%
0
-5
8 12 16 20
P boundary concentration, CP (at.%)
Fig. 10. Dependence of DBTT on phosphorus grain boundary concentration.
[23–25]. Therefore, the DBTT of the present IF steel may be affected
by hardness, grain size and phosphorus grain boundary segregation
[26–28]. As shown in Figs. 2 and 3, there is no visible difference
in both grain size and hardness for different specimens. Thus,
the changes in the DBTT of the experimental Ti-stabilized IF steel
should mainly be caused by P grain boundary segregation. Accord-
ing to the data in Figs. 6 and 9, the dependence of DBTT (◦ C) on
phosphorus grain boundary concentration (CP in at.%) is plotted in
Fig. 10, indicating that there is a linear relationship between them
with a R-square value of 0.96, which could be expressed as
DBTT = 1.60CP − 14.14
Previous studies have indicated that there is a linear relation-
ship between DBTT and segregation of impurities in low carbon
low-alloy steels [29–31]. Takayama et al. [26] studied the relation-
ship among the phosphorus grain boundary segregation, hardness
and prior austenite grain size for P-doped 3.5Ni–1.7Cr low-alloy
steels by experiments and Taylor series expansion, obtaining the
following expression:
DBTT (◦ C) = −120 + 4.8PP + 2(H − 20) + 0.15(7 − G)PP
+ 0.23(H − 20)PP + 0.036(7 − G)(H − 20)PP
where PP is the Auger P120 /Fe703 peak height ratio (%), H is the
Rockwell hardness of the steel (HRC), and G is the American Soci-
ety for Testing and Materials (ASTM) grain size number. As seen,
if the hardness and grain size are fixed, the DBTT may present a
linear relationship with the phosphorus boundary concentration.
Song et al. [14] investigated temper embrittlement of a P-doped
2.25Cr1Mo steel by measurements of DBTT and phosphorus bound-
ary concentration, indicating that a linear relationship between
them can be expressed as
DBTT (◦ C) = 3.38CP − 91.95
where CP is the boundary concentration of phosphorus in at.%. The
coefficients in Eqs. (5)–(7) are related to hardness, grain size and
chemistry composition, which may be the main reason for the dif-
ferences. Consequently, it may be claimed that the present results
are consistent with the previous studies. It is worth mentioning
that the previous studies are concerned with prior austenite grain
boundaries while the present one with ferrite grain boundaries.
In the light of Eq. (5), if the grain boundary concentration of
phosphorus is known, the DBTT may be determined without exper-
iment. Undoubtedly, this empirical relation could be very useful to
engineering practitioners. Eq. (3) is the thermodynamics of equi-
librium grain boundary segregation. It can be used to evaluate the
equilibrium grain boundary concentration of solute attained at a
8303
30 0.037wt.% 0.1wt.%
20
DBTT ( C)
o
10
0
-10
24
600 650 700 750 800 850
o
Aging temperauture ( C)
Fig. 11. Predicted DBTTs as a function of aging temperature for different phosphorus
concentrations in the matrix.
given temperature (T) and solute concentration in the matrix (Cg ).
Using Eqs. (3) and (5), one can obtain the DBTT of the present
Ti-stabilized IF steel as a function of aging temperature through pre-
dicting the equilibrium grain boundary segregation of phosphorus.
Fig. 11 shows the predicted DBTTs as a function of aging temper-
ature for different phosphorus concentrations in the matrix. It is
obvious that the phosphorus concentration in the matrix and the
aging temperature both have a considerable effect on the DBTT.
For a low phosphorus concentration in the matrix (e.g., 0.01 wt.%
(0.018 at.%)), the DBTT is much lower than 0 ◦ C even when the spec-
(5) imens were aged at 600 ◦ C for a long period. In other words, there
would be no cold work embrittlement for the IF steel doped with
a small amount of phosphorus. For the specimens doped with a
medium phosphorus concentration in the matrix (e.g., 0.037 wt.%
(0.067 at.%)), the DBTT could be 24 ◦ C after 600 ◦ C aging. In this sce-
nario, the cold work embrittlement could occur if the deep drawing
operation is performed at room temperature, but it would not take
place after aging at temperatures above 650 ◦ C because in this case
the DBTT is lower than 15 ◦ C. If the matrix concentration of phos-
phorus is quite high, e.g., 0.1 wt.% (0.18 at.%), the curve is obviously
shifted to a much higher level and the DBTT would be above 20 ◦ C
(6)
even after aging around 800 ◦ C, which could lead to severe cold
work embrittlement at room temperature.
As shown in Fig. 11, cold work embrittlement of P-doped IF steel
could be severe when it is annealed at lower temperatures or the
matrix concentration of phosphorus is higher. In order to utilize
the beneficial effect of P, and meanwhile to suppress the cold work
embrittlement, the IF steel should be annealed at relatively higher
temperatures after cold rolling. In addition, refinement of grain
size could decrease both the boundary concentration of phospho-
rus [21,32] and the DBTT [26], which could also reduce the cold
work embrittlement.
(7)
In the present work, only a Ti-stabilized IF steel with a medium
phosphorus concentration was examined. And Eq. (5) is valid only
when there is little phosphide precipitated during heat treatment.
This is true when the bulk concentration of phosphorus is low. How-
ever, for an IF steel with a high concentration of phosphorus, there
may be quite a lot of phosphide precipitated in the matrix, which
could lead to a different expression. Further studies of ductile-to-
brittle transition in Ti-stabilized IF steel with different phosphorus
concentrations are needed in the future.
4. Conclusions
Equilibrium grain boundary segregation of phosphorus to fer-
rite grain boundaries in the experimental IF steel was examined
8304 X.-M. Chen et al. / Materials Science and Engineering A 528 (2011) 8299–8304

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